Analysis of Plastics (Rapra Review Reports)

Report 149

ISSN: 0889-3144

Analysis of Plastics

Martin J. Forrest

Volume 13, Number 5, 2002

Rapra Review Reports Expert overviews covering the science and technology of rubber and plastics

RAPRA REVIEW REPORTS A Rapra Review Report comprises three sections, as follows: 1. A commissioned expert review, discussing a key topic of current interest, and referring to the References and Abstracts section. Reference numbers in brackets refer to item numbers from the References and Abstracts section. Where it has been necessary for completeness to cite sources outside the scope of the Rapra Abstracts database, these are listed at the end of the review, and cited in the text as a.1, a.2, etc. 2. A comprehensive References and Abstracts section, resulting from a search of the Rapra Polymer Library database. The format of the abstracts is outlined in the sample record below. 3. An index to the References and Abstracts section, derived from the indexing terms which are added to the abstracts records on the database to aid retrieval.

Source of original article Title

Item 1 Macromolecules

33, No.6, 21st March 2000, p.2171-83 EFFECT OF THERMAL HISTORY ON THE RHEOLOGICAL BEHAVIOR OF THERMOPLASTIC POLYURETHANES Pil Joong Yoon; Chang Dae Han Akron,University The effect of thermal history on the rheological behaviour of ester- and ether-based commercial thermoplastic PUs (Estane 5701, 5707 and 5714 from B.F.Goodrich) was investigated. It was found that the injection moulding temp. used for specimen preparation had a marked effect on the variations of dynamic storage and loss moduli of specimens with time observed during isothermal annealing. Analysis of FTIR spectra indicated that variations in hydrogen bonding with time during isothermal annealing very much resembled variations of dynamic storage modulus with time during isothermal annealing. Isochronal dynamic temp. sweep experiments indicated that the thermoplastic PUs exhibited a hysteresis effect in the heating and cooling processes. It was concluded that the microphase separation transition or order-disorder transition in thermoplastic PUs could not be determined from the isochronal dynamic temp. sweep experiment. The plots of log dynamic storage modulus versus log loss modulus varied with temp. over the entire range of temps. (110-190C) investigated. 57 refs.

Location

GOODRICH B.F. USA

Authors and affiliation

Abstract

Companies or organisations mentioned

Accession no.771897

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RAPRA REVIEW REPORTS VOLUME 13 Series Editor Dr. S. Humphreys, Rapra Technology Limited Rapra Review Reports comprise a unique source of polymer-related information with useful overviews accompanied by abstracts from hundreds of relevant documents. A Rapra Review Report is an excellent starting point to improve subject knowledge in key areas. Subscribers to this series build up a bank of information over each year, forming a small library at a very reasonable price. This series would be an asset to corporate libraries, academic institutions and research associations with an interest in polymer science. Twelve reports are published in each volume and these can be purchased individually or on a subscription basis. Format: Soft-backed, 297 x 210 mm, ISSN: 0889-3144 Order individual published Rapra Review Reports (see the following pages for a list of available titles), or purchase a subscription to Volume 13 (12 issues).

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Previous Titles Still Available Volume 1

Volume 4

Report 3

Advanced Composites, D.K. Thomas, RAE, Farnborough.

Report 37

Report 4

Liquid Crystal Polymers, M.K. Cox, ICI, Wilton.

Polymers in Aerospace Applications, W.W. Wright, University of Surrey.

Report 5

CAD/CAM in the Polymer Industry, N.W. Sandland and M.J. Sebborn, Cambridge Applied Technology.

Report 39

Polymers in Chemically Resistant Applications, D. Cattell, Cattell Consultancy Services.

Report 8

Engineering Thermoplastics, I.T. Barrie, Consultant.

Report 41

Failure of Plastics, S. Turner, Queen Mary College.

Report 11

Communications Applications of Polymers, R. Spratling, British Telecom.

Report 42

Polycarbonates, R. Pakull, U. Grigo, D. Freitag, Bayer AG.

Report 12

Process Control in the Plastics Industry, R.F. Evans, Engelmann & Buckham Ancillaries.

Report 43

Polymeric Materials from Renewable Resources, J.M. Methven, UMIST.

Report 44

Flammability and Flame Retardants in Plastics, J. Green, FMC Corp.

Volume 2 Report 13

Injection Moulding of Engineering Thermoplastics, A.F. Whelan, London School of Polymer Technology.

Report 45

Composites - Tooling and Component Processing, N.G. Brain, Tooltex.

Report 14

Polymers and Their Uses in the Sports and Leisure Industries, A.L. Cox and R.P. Brown, Rapra Technology Ltd.

Report 46

Quality Today in Polymer Processing, S.H. Coulson, J.A. Cousans, Exxon Chemical International Marketing.

Report 47

Report 15

Polyurethane, Materials, Processing and Applications, G. Woods, Consultant.

Chemical Analysis of Polymers, G. Lawson, Leicester Polytechnic.

Report 16

Polyetheretherketone, D.J. Kemmish, ICI, Wilton.

Report 17

Extrusion, G.M. Gale, Rapra Technology Ltd.

Report 49

Report 18

Agricultural and Horticultural Applications of Polymers, J.C. Garnaud, International Committee for Plastics in Agriculture.

Blends and Alloys of Engineering Thermoplastics, H.T. van de Grampel, General Electric Plastics BV.

Report 50

Report 19

Recycling and Disposal of Plastics Packaging, R.C. Fox, Plas/Tech Ltd.

Automotive Applications of Polymers II, A.N.A. Elliott, Consultant.

Report 51

Report 20

Pultrusion, L. Hollaway, University of Surrey.

Biomedical Applications of Polymers, C.G. Gebelein, Youngstown State University / Florida Atlantic University.

Report 21

Materials Handling in the Polymer Industry, H. Hardy, Chronos Richardson Ltd.

Report 52

Polymer Supported Chemical Reactions, P. Hodge, University of Manchester.

Report 22

Electronics Applications of Polymers, M.T.Goosey, Plessey Research (Caswell) Ltd.

Report 53

Weathering of Polymers, S.M. Halliwell, Building Research Establishment.

Report 23

Offshore Applications of Polymers, J.W.Brockbank, Avon Industrial Polymers Ltd.

Report 54

Health and Safety in the Rubber Industry, A.R. Nutt, Arnold Nutt & Co. and J. Wade.

Report 24

Recent Developments in Materials for Food Packaging, R.A. Roberts, Pira Packaging Division.

Report 55

Computer Modelling of Polymer Processing, E. Andreassen, Å. Larsen and E.L. Hinrichsen, Senter for Industriforskning, Norway.

Volume 3

Report 56

Plastics in High Temperature Applications, J. Maxwell, Consultant.

Report 25

Report 57

Joining of Plastics, K.W. Allen, City University.

Report 58

Physical Testing of Rubber, R.P. Brown, Rapra Technology Ltd.

Report 59

Polyimides - Materials, Processing and Applications, A.J. Kirby, Du Pont (U.K.) Ltd. Physical Testing of Thermoplastics, S.W. Hawley, Rapra Technology Ltd.

Foams and Blowing Agents, J.M. Methven, Cellcom Technology Associates.

Volume 5

Report 26

Polymers and Structural Composites in Civil Engineering, L. Hollaway, University of Surrey.

Report 27

Injection Moulding of Rubber, M.A. Wheelans, Consultant.

Report 28

Adhesives for Structural and Engineering Applications, C. O’Reilly, Loctite (Ireland) Ltd.

Report 60

Report 29

Polymers in Marine Applications, C.F.Britton, Corrosion Monitoring Consultancy.

Volume 6

Report 30

Non-destructive Testing of Polymers, W.N. Reynolds, National NDT Centre, Harwell.

Report 61

Food Contact Polymeric Materials, J.A. Sidwell, Rapra Technology Ltd.

Report 31

Silicone Rubbers, B.R. Trego and H.W.Winnan, Dow Corning Ltd.

Report 62

Coextrusion, D. Djordjevic, Klöckner ER-WE-PA GmbH.

Report 63

Conductive Polymers II, R.H. Friend, University of Cambridge, Cavendish Laboratory.

Report 64

Designing with Plastics, P.R. Lewis, The Open University. Decorating and Coating of Plastics, P.J. Robinson, International Automotive Design.

Report 32

Fluoroelastomers - Properties and Applications, D. Cook and M. Lynn, 3M United Kingdom Plc and 3M Belgium SA.

Report 33

Polyamides, R.S. Williams and T. Daniels, T & N Technology Ltd. and BIP Chemicals Ltd.

Report 65

Report 34

Extrusion of Rubber, J.G.A. Lovegrove, Nova Petrochemicals Inc.

Report 66

Report 35

Polymers in Household Electrical Goods, D.Alvey, Hotpoint Ltd.

Reinforced Thermoplastics - Composition, Processing and Applications, P.G. Kelleher, New Jersey Polymer Extension Center at Stevens Institute of Technology.

Report 67

Report 36

Developments in Additives to Meet Health and Environmental Concerns, M.J. Forrest, Rapra Technology Ltd.

Plastics in Thermal and Acoustic Building Insulation, V.L. Kefford, MRM Engineering Consultancy.

Report 68

Cure Assessment by Physical and Chemical Techniques, B.G. Willoughby, Rapra Technology Ltd.

Report 69

Toxicity of Plastics and Rubber in Fire, P.J. Fardell, Building Research Establishment, Fire Research Station.

Report 70

Acrylonitrile-Butadiene-Styrene Polymers, M.E. Adams, D.J. Buckley, R.E. Colborn, W.P. England and D.N. Schissel, General Electric Corporate Research and Development Center.

Report 71

Rotational Moulding, R.J. Crawford, The Queen’s University of Belfast.

Report 72

Advances in Injection Moulding, C.A. Maier, Econology Ltd.

Report 94

Compressive Behaviour of Composites, C. Soutis, Imperial College of Science, Technology and Medicine.

Report 95

Thermal Analysis of Polymers, M. P. Sepe, Dickten & Masch Manufacturing Co.

Report 96

Polymeric Seals and Sealing Technology, J.A. Hickman, St Clair (Polymers) Ltd.

Volume 9 Report 97

Rubber Compounding Ingredients - Need, Theory and Innovation, Part II: Processing, Bonding, Fire Retardants, C. Hepburn, University of Ulster.

Report 98

Advances in Biodegradable Polymers, G.F. Moore & S.M. Saunders, Rapra Technology Ltd.

Report 99

Recycling of Rubber, H.J. Manuel and W. Dierkes, Vredestein Rubber Recycling B.V.

Volume 7 Report 73

Reactive Processing of Polymers, M.W.R. Brown, P.D. Coates and A.F. Johnson, IRC in Polymer Science and Technology, University of Bradford.

Report 74

Speciality Rubbers, J.A. Brydson.

Report 75

Plastics and the Environment, I. Boustead, Boustead Consulting Ltd.

Report 100 Photoinitiated Polymerisation - Theory and Applications, J.P. Fouassier, Ecole Nationale Supérieure de Chimie, Mulhouse.

Report 76

Polymeric Precursors for Ceramic Materials, R.C.P. Cubbon.

Report 101 Solvent-Free Adhesives, T.E. Rolando, H.B. Fuller Company.

Report 77

Advances in Tyre Mechanics, R.A. Ridha, M. Theves, Goodyear Technical Center.

Report 102 Plastics in Pressure Pipes, T. Stafford, Rapra Technology Ltd.

Report 78

PVC - Compounds, Processing and Applications, J.Leadbitter, J.A. Day, J.L. Ryan, Hydro Polymers Ltd.

Report 103

Report 79

Rubber Compounding Ingredients - Need, Theory and Innovation, Part I: Vulcanising Systems, Antidegradants and Particulate Fillers for General Purpose Rubbers, C. Hepburn, University of Ulster.

Report 80

Anti-Corrosion Polymers: PEEK, PEKK and Other Polyaryls, G. Pritchard, Kingston University.

Report 81

Thermoplastic Elastomers - Properties and Applications, J.A. Brydson.

Report 82

Advances in Blow Moulding Process Optimization, Andres Garcia-Rejon,Industrial Materials Institute, National Research Council Canada.

Report 83

Molecular Weight Characterisation of Synthetic Polymers, S.R. Holding and E. Meehan, Rapra Technology Ltd. and Polymer Laboratories Ltd.

Report 84

Rheology and its Role in Plastics Processing, P. Prentice, The Nottingham Trent University.

Gas Assisted Moulding, T.C. Pearson, Gas Injection Ltd.

Report 104 Plastics Profile Extrusion, R.J. Kent, Tangram Technology Ltd. Report 105 Rubber Extrusion Theory and Development, B.G. Crowther. Report 106 Properties and Applications of Elastomeric Polysulfides, T.C.P. Lee, Oxford Brookes University. Report 107 High Performance Polymer Fibres, P.R. Lewis, The Open University. Report 108 Chemical Characterisation of Polyurethanes, M.J. Forrest, Rapra Technology Ltd.

Volume 10 Report 109 Rubber Injection Moulding - A Practical Guide, J.A. Lindsay. Report 110 Long-Term and Accelerated Ageing Tests on Rubbers, R.P. Brown, M.J. Forrest and G. Soulagnet, Rapra Technology Ltd.

Volume 8

Report 111

Polymer Product Failure, P.R. Lewis, The Open University.

Report 85

Ring Opening Polymerisation, N. Spassky, Université Pierre et Marie Curie.

Report 112 Polystyrene - Synthesis, Production and Applications, J.R. Wünsch, BASF AG.

Report 86

High Performance Engineering Plastics, D.J. Kemmish, Victrex Ltd.

Report 113 Rubber-Modified Thermoplastics, H. Keskkula, University of Texas at Austin.

Report 87

Rubber to Metal Bonding, B.G. Crowther, Rapra Technology Ltd.

Report 114 Developments in Polyacetylene - Nanopolyacetylene, V.M. Kobryanskii, Russian Academy of Sciences.

Report 88

Plasticisers - Selection, Applications and Implications, A.S. Wilson.

Report 115 Metallocene-Catalysed Polymerisation, W. Kaminsky, University of Hamburg.

Report 89

Polymer Membranes - Materials, Structures and Separation Performance, T. deV. Naylor, The Smart Chemical Company.

Report 116 Compounding in Co-rotating Twin-Screw Extruders, Y. Wang, Tunghai University.

Report 90

Rubber Mixing, P.R. Wood.

Report 117 Rapid Prototyping, Tooling and Manufacturing, R.J.M. Hague and P.E. Reeves, Edward Mackenzie Consulting.

Report 91

Recent Developments in Epoxy Resins, I. Hamerton, University of Surrey.

Report 118 Liquid Crystal Polymers - Synthesis, Properties and Applications, D. Coates, CRL Ltd.

Report 92

Continuous Vulcanisation of Elastomer Profiles, A. Hill, Meteor Gummiwerke.

Report 119 Rubbers in Contact with Food, M.J. Forrest and J.A. Sidwell, Rapra Technology Ltd.

Report 93

Advances in Thermoforming, J.L. Throne, Sherwood Technologies Inc.

Report 120 Electronics Applications of Polymers II, M.T. Goosey, Shipley Ronal.

Volume 11 Report 121 Polyamides as Engineering Thermoplastic Materials, I.B. Page, BIP Ltd. Report 122 Flexible Packaging - Adhesives, Coatings and Processes, T.E. Rolando, H.B. Fuller Company. Report 123 Polymer Blends, L.A. Utracki, National Research Council Canada. Report 124 Sorting of Waste Plastics for Recycling, R.D. Pascoe, University of Exeter. Report 125 Structural Studies of Polymers by Solution NMR, H.N. Cheng, Hercules Incorporated. Report 126 Composites for Automotive Applications, C.D. Rudd, University of Nottingham. Report 127 Polymers in Medical Applications, B.J. Lambert and F.-W. Tang, Guidant Corp., and W.J. Rogers, Consultant. Report 128 Solid State NMR of Polymers, P.A. Mirau, Lucent Technologies. Report 129 Failure of Polymer Products Due to Photo-oxidation, D.C. Wright. Report 130 Failure of Polymer Products Due to Chemical Attack, D.C. Wright. Report 131 Failure of Polymer Products Due to Thermo-oxidation, D.C. Wright. Report 132 Stabilisers for Polyolefins, C. Kröhnke and F. Werner, Clariant Huningue SA.

Volume 12 Report 133 Advances in Automation for Plastics Injection Moulding, J. Mallon, Yushin Inc. Report 134 Infrared and Raman Spectroscopy of Polymers, J.L. Koenig, Case Western Reserve University. Report 135 Polymers in Sport and Leisure, R.P. Brown. Report 136 Radiation Curing, R.S. Davidson, DavRad Services. Report 137 Silicone Elastomers, P. Jerschow, Wacker-Chemie GmbH. Report 138 Health and Safety in the Rubber Industry, N. Chaiear, Khon Kaen University. Report 139 Rubber Analysis - Polymers, Compounds and Products, M.J. Forrest, Rapra Technology Ltd. Report 140 Tyre Compounding for Improved Performance, M.S. Evans, Kumho European Technical Centre. Report 141 Particulate Fillers for Polymers, Professor R.N. Rothon, Rothon Consultants and Manchester Metropolitan University. Report 142 Blowing Agents for Polyurethane Foams, S.N. Singh, Huntsman Polyurethanes. Report 143 Adhesion and Bonding to Polyolefins, D.M. Brewis and I. Mathieson, Institute of Surface Science & Technology, Loughborough University. Report 144 Rubber Curing Systems, R.N. Datta, Flexsys BV.

Volume 13 Report 145 Multi-Material Injection Moulding, V. Goodship and J.C. Love, The University of Warwick. Report 146 In-Mould Decoration of Plastics, J.C. Love and V. Goodship, The University of Warwick Report 147 Rubber Product Failure, Roger P. Brown Report 148 Plastics Waste – Feedstock Recycling, Chemical Recycling and Incineration, A. Tukker, TNO

Analysis of Plastics

Martin J. Forrest (Rapra Technology Limited)

ISBN 1-85957-333-9

Analysis of Plastics

Contents 1.

Introduction .............................................................................................................................................. 3

2.

Analytical Techniques ............................................................................................................................. 3 2.1

Wet Chemistry Techniques ............................................................................................................. 3

2.2

2.5

Spectroscopic Techniques ............................................................................................................... 4 2.2.1 Infrared Spectroscopy (IR) ................................................................................................. 4 2.2.2 Ultraviolet Light Spectroscopy (UV) ................................................................................. 4 2.2.3 Nuclear Magnetic Resonance Spectroscopy (NMR) ......................................................... 4 2.2.4 Atomic Absorption Spectroscopy (AAS) ........................................................................... 4 2.2.5 X-Ray Fluorescence Spectroscopy (XRF) ......................................................................... 5 2.2.6 Raman Spectroscopy .......................................................................................................... 5 Chromatographic Techniques ......................................................................................................... 5 2.3.1 Gas Chromatography-Mass Spectrometry (GC-MS) ......................................................... 5 2.3.2 Gas Chromatography (GC) ................................................................................................ 6 2.3.3 High Performance Liquid Chromatography (HPLC) ......................................................... 6 2.3.4 Liquid Chromatography-Mass Spectroscopy (LC-MS) ..................................................... 6 2.3.5 Gel Permeation Chromatography (GPC) ........................................................................... 6 2.3.6 Thin Layer Chromatography (TLC) ................................................................................... 7 Thermal Techniques ........................................................................................................................ 7 2.4.1 Differential Scanning Calorimetry (DSC) ......................................................................... 7 2.4.2 Dynamic Mechnanical Thermal Analysis (DMTA) ........................................................... 8 2.4.3 Thermogravimetric Analysis (TGA) .................................................................................. 9 Elemental Techniques ................................................................................................................... 12

2.6

Microscopy Techniques ................................................................................................................ 12

2.7

Miscellaneous Techniques ............................................................................................................ 12

2.3

2.4

3.

Determination of Molecular Weight and Microstructure of Plastic Polymers ................................ 12 3.1

3.2

Determination of Molecular Weight ............................................................................................. 12 3.1.1 Gel Permeation Chromatography (GPC) ......................................................................... 13 3.1.2 Viscosity ........................................................................................................................... 14 3.1.3 Osmometry ....................................................................................................................... 14 3.1.4 Light Scattering ................................................................................................................ 14 3.1.5 Other Methods .................................................................................................................. 15 Monomer Types and Microstructure ............................................................................................ 15

4.

Determination of Polymer Type ........................................................................................................... 15

5.

Determination of the Plasticiser and Filler in a Plastic Compound ................................................. 19

6.

5.1

Determination of Plasticiser ......................................................................................................... 19

5.2

Determination of Fillers ................................................................................................................ 19 5.2.1 Particulate Fillers .............................................................................................................. 19 5.2.2 Fibrous Fillers ................................................................................................................... 20

Determination of Stabilisers in a Plastics Compound ....................................................................... 21 6.1

UV Stabilisers ............................................................................................................................... 21

6.2

Antioxidants .................................................................................................................................. 22

1

Analysis of Plastics

7.

8.

9.

Determination of Functional Additives ............................................................................................... 24 7.1

Process Aids and Lubricants ......................................................................................................... 24

7.2

Slip Additives ................................................................................................................................ 25

7.3

Pigments ........................................................................................................................................ 25

7.4

Antistatic Agents ........................................................................................................................... 25

7.5

Crosslinking Agents and Co-Agents............................................................................................. 26

7.6

Blowing Agents............................................................................................................................. 27

7.7

Flame Retardants .......................................................................................................................... 28

7.8

Impact Modifiers........................................................................................................................... 28

Analysis of Plastics for Food Contact Use ........................................................................................... 28 8.1

Global Migration Tests ................................................................................................................. 29

8.2

Specific migration and residual monomer tests............................................................................ 30

Determination of Stabilisers in PVC ................................................................................................... 31

10. Analysis of Plastic Laminates and Fibres ............................................................................................ 32 11. Surface Analysis of Plastics ................................................................................................................... 34 11.1 X-Ray Photoelectron Spectroscopy (XPS) ................................................................................... 34 11.2 Laser Induced Mass Analysis (LIMA) ......................................................................................... 34 11.3 Secondary Ion Mass Spectroscopy (SIMS) .................................................................................. 36 12. Failure Diagnosis ................................................................................................................................... 36 12.1 Common Compositional Problems ............................................................................................... 36 12.2 Environmental Stress Cracking .................................................................................................... 37 12.3 Contamination Problems .............................................................................................................. 37 12.4 Odour and Emissions Problems .................................................................................................... 37 13. Conclusions ............................................................................................................................................. 38 Additional References ................................................................................................................................... 39 Appendix 1. Solubility Parameters of Plastics, Plasticisers and Typical Solvents .................................. 41 Appendix 2. Specific Gravities of Plastics and Compound Ingredients .................................................. 43 Abbreviations and Acronyms ....................................................................................................................... 45 Abstracts from the Polymer Library Database .......................................................................................... 47 Subject Index ............................................................................................................................................... 133

The views and opinions expressed by authors in Rapra Review Reports do not necessarily reflect those of Rapra Technology Limited or the editor. The series is published on the basis that no responsibility or liability of any nature shall attach to Rapra Technology Limited arising out of or in connection with any utilisation in any form of any material contained therein.

2

Analysis of Plastics

1 Introduction Plastics present chemical analysts with one of their most difficult, but satisfying, challenges. In order to obtain useful products that perform under a variety of demanding conditions, the plastic matrix can be tailor made by the bringing together of a wide range of polymers and additives. There is a very wide range of polymer types available and in some cases they are blended together. The technology of plastics is therefore a mature one, allowing fine tuning of a compound to fit a number of design criteria and product requirements. The choice of materials available means that plastics can be used in many applications, ranging from replacement windows to packaging materials, and from mundane products such as disposable cutlery to highly specialised components in electrical and aerospace products. The plastics analyst has therefore to bear in mind the possible complexity of the system that confronts him and the potential interferences that may be brought into play. When reverse engineering a plastic compound a considerable number of elemental, spectroscopic, chromatographic and thermal techniques have to be used in an integrated and structured approach in order to accumulate and cross check the data necessary for an accurate result. With sufficient experience and access to the necessary instrumental techniques, it should be possible for the analyst to successfully elucidate a formulation. The determination of the particular ‘grade’ of plastic, although a consistent request, is however rarely possible. This is mainly due to the fact that a number of manufacturers produce very similar, if not identical, products or that the material has been specially compounded for a particular purpose. Commercial confidentiality can also restrict the ability to use the analytical data to identify a particular manufacturer’s product as a significant amount of compositional information may not be disclosed. The objective of this review is to present, as fully as is possible within this format, an introduction to the techniques and methods that are used to characterise and carry out quality control work on plastics; to investigate the failure of plastic products; and to deformulate plastic compounds. With respect to the last category, the analyst’s job when characterising ‘unknowns’ is always made much easier if at least some information is available on the sample and the types of species that may be present in it. Armed with this knowledge they can work much more

efficiently and obtain better results. To assist in the acquisition of this knowledge opportunities have been taken within the text to not only detail the analytical methods, but provide examples of the species that they may be used to detect and quantify. In other words, in order to have a full understanding of the principles behind and surrounding the analytical methods and approaches it is vital to have an understanding of plastic technology itself. Relevant books and academic papers are cited throughout the review, but there are also a number of general texts which will provide useful further reading (79, 199, 315, 377, 387, 398, a.1-a7). The appendices provide useful additional information. Appendix 1 gives solubility parameters of a range of materials. Appendix 2 lists the specific gravities of a range of plastics and compounding ingredients.

2 Analytical Techniques 2.1 Wet Chemistry Techniques Before the advent of modern instrumental techniques, plastic analysis relied on a sequence of wet chemistry reactions to determine information such as the generic polymer type of a material. The amount of wet chemistry carried out in the modern polymer analysis laboratory in the 21st Century is minimal. There are some tests which can still be grouped under this heading, although even some of these can employ an instrumental technique to provide the final answer. One such method is the oxygen flask combustion method, which can be used on PVC products to determine the amount of PVC in the formulation by quantifying the chlorine present. The oxygen flask method (ISO 6528.1-1992 and BS 7164 Section 23.1- 1993) uses an initial burn in oxygen (although the sample is trapped between two platinum gauge ‘flags’) and trapping of the volatile products in an absorbing solution comprising 1-5 ml of 0.05M potassium hydroxide, 0.2 ml of 30% hydrogen peroxide and 10 ml of distilled water. Once the volatiles have been trapped there is a choice of analytical method. A titration can be performed, or ion chromatography can be used to quantify the chloride ion.

3

Analysis of Plastics

2.2 Spectroscopic Techniques 2.2.1 Infrared Spectroscopy (IR) Infrared spectroscopy (IR) is used extensively in the analysis of plastics. It is a very good, relatively quick technique for the determination of the polymer present in a plastic product. Unlike rubbers, where the majority of compounds contain additives such as carbon black and plasticisers that can interfere with the infrared data obtained, it is normally possible to record infrared spectra directly from the plastic sample using either a surface technique (e.g., attenuated total reflectance (ATR) spectroscopy) or in transmission through the sample from a film produced by pressing a specimen above its glass transition or melting point. Some plasticised plastics products (e.g., PVC or nylon 11) will need to be extracted with a solvent (e.g., methanol) first to remove the plasticiser. Products that are filled (e.g., polypropylene/talc kettle bodies) will require a pyrolysis technique where a pyrolysis condensates infrared library, such as the one published by Rapra Technology, needs to be available. It is also possible with amorphous plastics that are soluble in conventional solvents (e.g., chloroform) at room temperature to record infrared spectra from films cast from solution. This approach has the drawback that all the solvent needs to be removed from the film if interference bands are to be avoided. Analysis of the solvent extract obtained to prepare the plastic sample for an IR technique can be used to identify the plasticiser present in a compound. IR analysis of an ash of the compound obtained by heating at 550 °C can help to identify inorganic fillers. IR can also be used to identify specialist additives such as fire retardants.

2.2.2 Ultraviolet Light Spectroscopy (UV) Although not as universally used as IR, UV is another spectroscopic technique which has a role to play in the

analysis of plastics. It is used in the qualitative and quantitative analysis of additives, particularly antioxidants and UV stabilisers.

2.2.3 Nuclear Magnetic Resonance Spectroscopy (NMR) NMR is a powerful tool for the determination of polymer structure. It is at its most sensitive when used on analytes in solution. Table 1 gives examples of solvents used for NMR. Amorphous plastics, such as polystyrene can be dissolved in deuterated chloroform, whereas for the less soluble semi-crystalline plastics (e.g., PET) solvents such as trichloroacetic acid have to be used. Of the conventional instruments, both proton and carbon 13 instruments have been used in plastics analysis. Combinations of two solvents can be used to achieve a good degree of solubility and elevated temperatures (e.g., 70 °C) are also common. The proton NMR solvents can be used for carbon 13 experiments, but the reverse is rarely the case. Techniques are available for work on a specific plastic type, e.g., in the analysis of polyvinylidene fluoride, fluorine 19 NMR can be used. In this case a solvent such as dimethylformamide is employed. The 13 C NMR spectrum for a polypropylenepolyethylene copolymer is shown in Figure 1. The spectrum was obtained at 90 °C in a solution of orthodichlorobenzene. The major peaks at 21, 27 and 46 ppm are due to the polypropylene, with the other, minor peaks being due to polyethylene.

2.2.4 Atomic Absorption Spectroscopy (AAS) This technique, and the related inductively coupled plasma (ICP), are used where it is necessary to quantify metals in a plastic compound. Although not often required it can be of use in the analysis of flame retardant systems, where additives such as antimony trioxide and zinc borate have been used.

Table 1 Examples of solvents used in NMR work on plastics Proton NMR Deuterated chloroform

Carbon 13 NMR Orthodichlorobenzene

Trifluoroacetic acid

Trichlorobenzene

Deuterated benzene

Aliphatic hydrocarbons, e.g., heptane

1,1,2,2-Tetrachloro-deuterated ethane

4

Analysis of Plastics

Figure 1 13C

NMR spectrum of polypropylene-polyethylene copolymer

2.2.5 X-Ray Fluorescence Spectroscopy (XRF) This technique is very useful for obtaining semiquantitative elemental data from plastic compounds and their ashes. Among other things, it helps to identify inorganic fillers and pigments in samples. The technique is usually used in conjunction with IR. When it comes to analysing small samples, sample surfaces or contaminants in samples, the scanning electron microscope (SEM)/XRF combination (sometimes referred to as energy dispersive analysis (Edax)) can be a very valuable tool.

2.2.6 Raman Spectroscopy Until 1986 Raman spectrometers were either dispersive long focal length double monochromators or shorter focal length triple monochromators and required highly trained scientists to obtain good quality data. The advent of the Fourier Transform (FT)-Raman technique in 1986 significantly reduced data acquisition times and also brought the technical advantage of suppressing any laser induced fluorescence within the sample. Further developments have enabled smaller, low cost, high performance, quality instruments to be produced and

have led to the development of the Raman microscope an instrument analogous to the IR microscope. This has enabled Raman spectroscopy to be used routinely for the identification of polymer types and the analysis of contaminants within polymer samples.

2.3 Chromatographic Techniques 2.3.1 Gas Chromatography-Mass Spectrometry (GC-MS) This powerful, versatile technique can be used to obtain a significant amount of compositional information on plastic samples. It is particularly useful in identifying minor components of the sample such as the stabiliser, antistatic agent and, where appropriate, the crosslinking system. It can also be used to investigate the polymer fraction within a sample when the instrument is fitted with a pyrolysis unit set at around 600 °C. The technique also plays a role in failure diagnosis by being able to provide information on odours, and

5

Analysis of Plastics

organic contaminants that may have degraded the plastic matrix. There are a variety of ways that the sample or fractions of the sample (e.g., an extract) can be analysed by GCMS. These include static headspace, dynamic headspace, solution injection and pyrolysis.

2.3.2 Gas Chromatography (GC) This technique can also be used to obtain polymer type information by use of a pyrolysis approach, although the technique is less powerful because of the absence of a mass spectrometer, and a pyrogram ‘fingerprint’ has to be used and a comparison made against a library of known standards. This technique is also used for the identification and quantification of additives such as antioxidants and, where sufficient volatility exists, plasticisers and organic flame retardants.

2.3.3 High Performance Liquid Chromatography (HPLC) HPLC can be used to identify and quantify additives that are either too involatile or insufficiently stable to be determined by GC/GC-MS. This is particularly the case with antioxidants such as Irganox 1010 and 1036. HPLC also comes into its own in the quantification of plasticisers such as dioctyl phthalate (DOP).

2.3.4 Liquid Chromatography-Mass Spectroscopy (LC-MS) This instrument is essentially a coupling of an HPLC with a mass selective detector and as such offers a significant enhancement in performance to the polymer chemist. Although such combinations have been around for many years, they were complex and expensive (i.e., effectively research tools only), and it is only within the last five years or so that single quadrupole benchtop LC-MS systems have become reasonably common place due to their relative ease of use and cost. A mass spectrometer can be the ideal detector for liquid chromatography because it offers both universality and the required selectivity for complex analytical problems. For many years development work has concentrated particular on the design of

6

the interface between the chromatograph and the detector. Today, the two most popular types of interface for the benchtop single quadrupole LC-MS are the particle beam interface and the atmospheric pressure ionisation (API) interface. The particle beam interface is used to generate electron ionisation (EI) spectra and the API interface is used to generate either electrospray (ESI) or atmospheric pressure chemical ionisation (APCI) spectra. A further complexity is that the API interface can generate either positive (i.e., molecular ion plus one hydrogen) spectra or negative (i.e., molecular ion minus one hydrogen) spectra. The particle beam interface is very good for qualitative work because the 70 eV spectra contain a significant amount of structural information and can be searched against conventional mass spectra libraries. However, in the full scan mode the sensitivity is restricted to the low nanogram levels. In the case of the API interface, both the electrospray and APCI modes are soft ionisation techniques which leave the molecular ion (or pseudomolecular ion) intact without much fragmentation. The interface therefore offers more sensitivity and is ideal for quantitative work at low levels (e.g., contamination of drug and food matrices by polymer additives/ breakdown products).

2.3.5 Gel Permeation Chromatography (GPC) For this technique to be successful the sample must be readily soluble in an organic solvent. It has a wide application in the analysis of plastic samples. It is possible to obtain molecular weight data on both amorphous plastics and semi-crystalline plastics. In the amorphous case (e.g., polystyrene), the system used is set around ambient temperature (30 °C) and solvents such as THF, chloroform and toluene are used. With semi-crystalline plastics (e.g., polyolefins), more aggressive solvents such as orthodichlorobenzene and meta-cresol are used at elevated (140 °C) temperatures. In the case of some complex plastic systems (e.g., blends), the development of interfaces such as the Lab Connections LC Transform, have proved very useful in increasing the amount of information that can be obtained in a GPC analysis by enabling IR data to be recorded on the resultant chromatogram. Hence, with the correct choice of separating column, polymer blends can be separated and identified as well as plasticisers.

Analysis of Plastics

2.3.6 Thin Layer Chromatography (TLC) TLC is a relatively simple technique that can be used for both the separation and identification of additives such as antioxidants and UV stabilisers. A number of approaches are possible using different developing solvents and spraying agents. It is also the case that TLC can be used in a preparative way for the isolation of sample fractions for subsequent chromatographic or spectroscopic analysis. TLC does have the image of being somewhat old fashioned and it is to be expected that the market penetration of LC-MS systems will further erode the standing of this technique in the modern analytical laboratory.

2.4 Thermal Techniques 2.4.1 Differential Scanning Calorimetry (DSC) DSC is used extensively in the analysis of plastics, particularly those that are semi-crystalline - polyolefins, nylons, polyesters, etc. It is sensitive enough to

differentiate between different polyethylenes (i.e., LDPE, LLDPE, HDPE, etc.) from their melting points and the appearance of their melting endotherms as well as being able to detect and, with appropriate standard materials, quantify plastic blends, e.g., PP/PE and nylon 6/nylon 6,6. The DSC trace for a quenched sample of PET is shown in Figure 2. This trace shows the Tg (around 75 °C) of the material, the exothermic formation of the crystalline phase (at 156.9 °C) and the endotherm due to the melting of this phase (at 255 °C). The DSC trace of a plastic blend is shown in Figure 3. The data obtained has been compared to standards and the material has been shown to be a blend of ethylenevinyl acetate copolymer (EVA) and LDPE. The approximate proportions of each is EVA 15-20%/LDPE 20-25%. In addition the EVA copolymer is thought to contain around 20-25% of vinyl acetate (VA). Although not as sensitive as dynamic mechanical thermal analysis (DMTA) to glass transitions, DSC can be used to identify a plastic from the glass transition in its thermogram. The glass transition (Tg) and crystalline melting temperatures (Tm) of a range of plastics are given in Table 2.

Figure 2 DSC trace for a quenched sample of PET

7

Analysis of Plastics

Figure 3 DSC trace of a blend of EVA and LDPE

It is also possible to use DSC to provide quality control fingerprint thermograms from which deviations in the composition of a plastic compound can be detected. One reason for this is that although the technique is not capable of determining the molecular weight of a plastic, differences in molecular weight will be apparent in the melting endotherm region. Using appropriate standard materials it is also possible to use DSC to quantify the level of certain additives, e.g., peroxides, in a sample. DSC can also be used in thermal stability studies of the plastic compound, and to investigate the effectiveness of antidegradants and fire retardants.

2.4.2 Dynamic Mechnanical Thermal Analysis (DMTA) DMTA is very useful for generating modulus versus temperature data on plastic compounds. The effects

8

of temperature on this important material property can be obtained over a wide temperature range (typically –150 °C to +200 °C), along with the glass transition temperature and information on thermal stability. The use of DMTA to differentiate between plastic samples that have a similar chemical composition, but very different physical properties is shown in Figure 4. Both of these samples are polymethylmethacrylate (PMMA), but the top one is crosslinked having been prepared with a small amount of difunctional monomer and the bottom sample is the standard thermoplastic material. It can be seen that the crosslinked sample does not melt and the modulus does not fall away significantly until thermal degradation occurs. The sensitivity of DMTA to glass transition temperatures (approximately 1,000 times greater than DSC which measures heat capacity changes rather than modulus) is very useful in the analysis of plastics and their blends.

Analysis of Plastics

Table 2 Glass transition (Tg) and crystalline melting temperatures (Tm) of a range of plastics Plastics Type

Tg (°C)

Tm (°C) 105 (LDPE)

Polyethylene

–20

115 (MDPE) 135 (HDPE)

Polypropylene

5

160

Polybut-1-ene

–20

12 0

Polypent-1-ene

24

70

PTFE

115

32 7

Polychlorotrifluoroethylene (PCTFE)

52

22 1

Polyvinyl alcohol

70

Decomposes below Tg

Polyvinyl chloride

80

-

Polyvinylidene chloride

–18

19 0

80 to 140

-

Atactic polystyrene

95

-

Isotactic polystyrene

100

23 0

PET

67

25 6

Methyl methacrylate

100

-

Polycarbonate of bisphenol A

150

22 5

Polysulfone of bisphenol A

195

-

Nylon 6

50

21 5

Nylon 6,6

60

26 6

Polyethylene oxide

–55

66

Polypropylene oxide

–62

65

Polyvinyl methyl ether

–31

14 4

Polyvinyl ethyl ether

-

86

Polyvinyl t-butyl ether

-

250

Polyacrylonitrile

2.4.3 Thermogravimetric Analysis (TGA) This technique is useful in the analysis of compounded plastic samples. It is possible to obtain accurate quantifications of the principal compound constituents such as plasticiser, polymer and inorganic species. This data can be obtained on small (e.g., 10 mg) samples in a relatively short time (around 45 minutes). By the use of the temperature maxima at which weight events occur it is also possible to use the technique to obtain some qualitative assignments for the plasticiser and polymer.

A typical TGA programme would be: Heat from ambient to 550 °C in a nitrogen atmosphere at 20 °C/min until no further weight loss occurs. Then, reduce the heat to 300 °C, change the atmosphere to air and heat at 20 °C/min to 1,000 °C. It is common to plot the weight loss derivative in conjunction with the weight loss, and this can be used to detect the presence of a polymer blend of two or more components. Thermal decomposition temperatures of a range of plastics are shown in Table 3.

9

Analysis of Plastics

Figure 4 DMTA results for (a) crosslinked and (b) standard grades of PMMA

10

Analysis of Plastics

Table 3 Thermal decomposition temperatures of a range of plastics Temperature to achieve 50% decomposition* (°C)

Plastic Type Polyvinyl chloride

260

Polymethyl methacrylate

327

Polypropylene

387

Polyethylene

414

Poly-p-xylene

432

PTFE

509

*The temperature at which the polymer loses half its weight in vacuo at 30 minutes preceded by 5 minutes preheating at that temperature

Other uses for the technique include the production of compositional fingerprints for quality control purposes and the investigation of thermal stability and the effects that additives such as flame retardants and antioxidants have on it. It is possible to interface modern TGA instruments directly to IR instruments or mass spectrometers, thus obtaining both quantitative and qualitative data in one analytical step.

The introduction of high resolution TGA instruments has enabled more accurate quantifications of minor weight loss events to be made. For example, the use of high resolution TGA to quantify the amount of residual monomer in a sample of polymethylmethacrylate is shown in Figure 5. The residual monomer weight loss event peaks at 297.5 °C.

Figure 5 High resolution TGA of polymethylmethacrylate

11

Analysis of Plastics

2.5 Elemental Techniques The determination of the concentration of certain elements can be very useful in plastic analysis work. In particular, it is often necessary to determine the amount of nitrogen or a halogen such as chlorine or fluorine in the calculation of polymer content or polymer blend proportions. Also, the targeting of specific elements can enable the quantity of a particular additive (e.g., phosphate flame retardant or titanium dioxide pigment) to be calculated. The determination of nitrogen is usually done using carbon/hydrogen/nitrogen analysers and the technique is relatively simple and uses small amounts (e.g., 2050 mg) of sample. With the other elements, the technique will vary according to the element being quantified. Sulfur and chlorine, for example, can be determined using oxygen combustion followed by ion chromatography analysis of the products.

2.6 Microscopy Techniques High magnification (e.g., 150x) optical microscopy can be used to examine the dispersion of fillers within the plastic matrix. The success of this operation is usually dependent on the generation of high quality microtome sections of the sample. The technique of scanning electron microscopy has already been briefly mentioned in Section 2.2.5 in relation to the elemental analysis of surfaces in conjunction with XRF. It can also be used in its own right, where its high magnification powers can be employed to determine the particle size of fillers and in the detailed examination of fracture surfaces. Transmission electron microscopy (TEM) can be used to investigate the phase morphology of polymer blends and the dispersion of fillers.

of inorganic additives (e.g., rutile and anatase forms of titanium dioxide) and direct probe mass spectroscopy (for the determination of high molecular weight antioxidants). Surface analysis techniques such as secondary ion mass spectrometry (SIMS), laser induced mass analysis (LIMA) and X-ray photoelectron spectroscopy (XPS) are used for failure diagnosis work associated with such things as poor bonding to substrates and for surface characterisation work. A chromatography technique that achieved prominence in the research literature around ten to fifteen years ago for the determination of relative high molecular weight additives (e.g., antioxidants) and the study of plastic oligomers is supercritical fluid chromatography (SFC). This is essentially a liquid chromatography technique that uses similar analytical columns to HPLC but where the mobile phase is a substance (e.g., carbon dioxide) that is kept in a supercritical state by a suitable combination of temperature and pressure. One of the benefits of the technique is that the analytes can be easily separated from the mobile phase once the chromatography has taken place so, for example, they can be deposited on infrared transparent substrates for analysis using an infrared microscope. The relatively expensive nature of the instrumentation and the development of other techniques (e.g., LC-MS) have restricted its market penetration.

3 Determination of Molecular Weight and Microstructure of Plastic Polymers This section covers analytical techniques that can be applied both to uncompounded plastic resins and compounded materials.

3.1 Determination of Molecular Weight For other spectroscopic techniques see Section 2.2.

2.7 Miscellaneous Techniques There are a number of other analytical techniques that can be used to characterise plastic samples and many of these feature in the abstracts at the back of this Review Report. These include X-ray diffraction (XRD) to identify between different crystalline forms

12

In common with other polymers, plastics have a distribution of molecular weights. This distribution will be widest for polymers produced by free radical polymerisation (e.g., polystyrene) and narrowest for plastics produced using specialised catalyst systems such as metallocenes. There are a number of ways in which the molecular weight distribution of a plastic can be expressed:

Analysis of Plastics

3.1.1 Gel Permeation Chromatography (GPC)

Mn = Number average molecular weight = Sum nM Sum n Mw = Weight average molecular weight = Sum nM2 Sum nM Mz = Z average molecular weight

= Sum nM3 Sum nM2

where n = the number of molecules of molar mass M. The Z average is very sensitive to high molecular weight molecules within the polymer. The weight average is always of greater value than the number average. A measure of the breadth of the molecular distribution of the polymer can be obtained by dividing the weight average by the number average: Polydispersity = Mw Mn As the polymer tends to monodispersity the polydispersity approaches unity. There are a wide variety of methods that can be used to obtain molecular weights. The principal ones are as follows.

This is the pre-eminent technique and has been refined and developed extensively over the past 30 years. It is possible to use it on both uncompounded resins and plastic compounds and Mn, Mw and Mz values can be obtained. GPC is essentially a liquid chromatography technique where the sample is dissolved in a suitable solvent (e.g., THF for polystyrene) and injected into a system where the molecules are separated according to their molecular size by a column that contains a swollen, particulate, porous gel packing. Figure 6 shows the GPC chromatograms for two polymers that have different molecular weight distributions but similar calculated molecular weight averages. The standard detector for GPC systems is the refractive index (RI) detector, but a feature of developments over the past 10 years is the development of double (RI and viscosity) or triple detector systems (RI, viscosity and light scattering). These multiple detection systems provide measures of ‘true’ molecular weight by obtaining the actual Mark-Houwink parameters (in the case of the viscosity detector) for the polymer being

Figure 6 GPC chromatograms for two polymers with different molecular weight distributions but similar molecular weight averages

13

Analysis of Plastics

analysed, as opposed to the polystyrene equivalent molecular weight from the use of monodisperse polystyrene calibrants alone. An inherent property of the light scattering detector is that it provides ‘true’ molecular weight data. It is also possible to use spectroscopic detectors such as infrared and ultraviolet. One practical use of the latter is to determine if chemical modifiers (e.g., silane coupling agents) are bound to polymer molecules. This is done by measuring the molecular weight distribution of the modified plastic at a UV wavelength where the polymer itself does not contribute to the absorbance and comparing this to the distribution of the unmodified plastic. The use of the LC transform module with GPC has extended its capabilities by allowing IR data to be generated on the species during the course of an analysis. This is done by impinging the species onto a germanium disc which is then placed into a module fitted into the sample compartment of an IR bench. IR data is collected on the entire chromatogram using continuous collection software, which enables the IR spectrum of any particular section to be viewed. This technique is very useful for plastic blends and highly compounded plastics such at PVC, as it allows the polymers in the blend to be identified, as well as relatively high molecular weight additives such as plasticisers.

3.1.2 Viscosity This is a standard procedure for molecular weight determinations and involves the use of specially designed viscometers to accurately measure the viscosity of a polymer solution. From this the intrinsic viscosity is determined and hence the molecular weight. The time taken for the polymer solution to pass between two marks on the viscometer is compared to that of pure solvent and the ratio is the viscosity of the solution. Successive dilutions give a range of concentrations and times from which the intrinsic viscosity can be calculated. The value for this is then entered into the Mark-Houwink equation:

3.1.3 Osmometry There are two principal osmometry techniques: vapour pressure osmometry and membrane osmometry. Vapour pressure osmometry involves the indirect measuring of the lowering of the vapour pressure of a solvent due to the presence of a solute. It is based on the measurement of the temperature difference between droplets of pure solvent and of polymer solution maintained in an isothermal atmosphere saturated with the solvent vapour. Calibration is by the analysis of standards of known molecular weight and should be over the entire range of molecular weights of interest to ensure the best results. The technique is useful for polymers that have molecular weights in the 500-50,000 range. Membrane osmometry involves the use of a membrane between the solvent and the polymer solution that is permeable to the solvent molecules but not to the solvated polymer molecules. This is the major restriction on the technique and means that it cannot be used for low molecular weight polymers (< approximately 50,000).

3.1.4 Light Scattering Recent developments in instrumentation have led to a resurgence of this technique where the weight average molecular weight is obtained from the light scattering behaviour of polymer solutions. These developments have centred around low angle laser light scattering (LALLS), multi-angle laser light scattering (MALLS) and evaporative light scattering (ELS). As well as being stand alone instruments, light scattering detectors have been developed for GPC systems. MALLS detectors can provide direct information on the branching ratio of a polymer (a.8). Care has to be taken to ensure that the polymer solution is clear (to reduce variability) and low cell volumes (0.1 μl) and dilute solutions help this. Solvent choice is also critical, with the best results being with solvents that have a very different refractive index to the polymer, and that are low-scattering themselves.

Intrinsic viscosity = KMX where K and X are constants for the particular solvent being used and are referred to as the Mark-Houwink parameters.

Evaporative light scattering involves the removal of the solvent from the solvated polymer as it elutes down a drift tube and the isolated polymer particles then scatter light from the light source.

Depending on the source of the Mark-Houwink parameters the molecular weight can be expressed as either the number or weight average.

Light scattering can produce precise data and has been used successfully on polymers with molecular weights ranging from 10,000 to 10,000,000.

14

Analysis of Plastics

3.1.5 Other Methods Other methods include end group analysis (Mn), ultracentrifugation (Mw) and, indirectly by determining glass transition temperatures, DSC/DTA. A review of the determination of the molecular weight of polymers has been produced by Holding and Meehan (396).

3.2 Monomer Types and Microstructure The use of transmission IR, pyrolysis IR and pyrolysis GC to determine the polymer type of a plastic is covered in Section 2.1. Where appropriate standards are available, it is also possible to use IR to quantify the amounts of monomers in copolymers and terpolymers. Another technique that is very effective at identifying the monomers present in a plastic materials is NMR. The NMR technique will also provide information on the proportions of the various monomers in copolymers and tripolymers. In contrast to IR this information can be obtained without having to analyse standards of known monomer composition; the areas under the diagnostic chemical shifts being used. NMR instruments can also be used to obtain fundamental structural information on polymers such as end group chemistry, branch points and structural isomerism. It is also possible to use IR for the latter, although some of the isomeric structures have relatively weak absorptions which makes detection difficult when they are at a low concentration.

4 Determination of Polymer Type One of the most basic and useful tests to carry out on a plastic sample is to determine its polymer type. Due to their relative simplicity, it is usually possible to carry out an infrared analysis of the plastic material in the as received state and identify the plastic by reference to a standards database. The advent of the single bounce attenuated total reflectance (ATR) accessories for Fourier transform infrared spectroscopy (FTIR) instruments enables this operation to be carried out in a matter of minutes on a sample a few millimetres in size. Some care should be taken as the relative intensities of the bands present in ATR spectra can vary

compared to conventional transmission spectra (historically used to compile databases) and there is a slight shifting in the absorption wavenumber value of the bands. If more traditional spectra are required, the usual approach is to press a thin film of the samples using a temperature which is above the Tg or Tm and to record a transmission spectrum. A transmission infrared spectrum of polypropylene produced from a film pressed at 170 °C is shown in Figure 7. Another technique that can be used to obtain transmission spectra is to dissolve the sample up using a suitable solvent and to cast a film. Care has to be taken to remove all of the solvent by drying in an oven otherwise it can influence the data obtained. A transmission infrared spectrum of PVC produced from a film cast from a solution in THF is shown in Figure 8. For those plastic compounds that contain a plasticiser and/or organic flame retardant, a certain amount of preparation work is required to effectively remove the interference of these constituents. After milling or comminuting the sample to increase surface area, a solvent extraction is performed to remove these organic species. It is then usually possible to record the infrared spectrum using either an ATR technique or by transmission through a hot pressed film. One of the most comprehensive databases available of plastic infrared spectra has been produced by Hummel (a.9). Where the plastic sample contains both a major organic additive and a filler, it is necessary to pyrolyse the extracted portion of the sample and then record an infrared spectrum of the collected pyrolysis condensates. Providing that an extensive database of pyrolysate spectra is available (234), this method is very successful in identifying generic polymer types and polymer blends. In the case of blends, it is also possible to express the results semi-quantitatively if the appropriate standards are available. If the plastic only contains a filler, the pyrolysis approach can be employed without using the initial solvent extraction step. The pyrolysate infrared spectra of nylon 6 and low density polyethylene are shown in Figures 9 and 10, respectively. Another method which enables the polymer type within a plastic sample to be identified is pyrolysis gas chromatography. This method can be applied to either

15

Analysis of Plastics

Figure 7 Transmission infrared spectrum of polypropylene produced from a film pressed at 170 °C

Figure 8 Transmission infrared spectrum of unplasticised PVC produced from a film cast from a THF solution

16

Analysis of Plastics

Figure 9 Pyrolysate infrared spectrum of nylon 6

Figure 10 Pyrolysate infrared spectrum of low density polyethylene

17

Analysis of Plastics

the extracted portion of the sample or the sample as received. In the former case any relatively low molecular weight plasticiser elutes early on and does not have a significant influence on the pyrogram as a whole. As with pyrolysis IR, a database of standards needs to be put together and then the pyrogram fingerprints of unknowns can be matched. The temperature that the pyrolysis unit is set at, and the design of the unit (e.g., Curie point or microfurnace), will affect the pyrograms produced from a particular sample. Again, it is possible to identify and quantify blends and blend ratios. Typical experimental conditions for pyrolysis GC experiments are as follows: Sample weights

0.1-5.0 mg

Pyrolysis temperatures

400-800 °C (microfurnace and Curie point) 800-1200 °C (platinum filament)

Microfurnace type pyrolyser - specific example using an SGE Pyrojector Weight of sample

0.4 mg

Pyrolysis temperature

600 °C

Pyrolysis gas

Helium at 0.10 MPa

GC column

5% Diphenyl siloxane 30 m x 0.25 mm, 1.0 μm film

GC column temperature program

2 min at 50 °C followed by 10 °C/min to 280 °C and then 10 min at 280 °C

GC carrier gas

Helium at 0.06 MPa

GC injector temperature 320 °C Detector

Flame ionisation detector (FID) at 350 °C

Adding a mass spectrometer into the system, so that the technique becomes pyrolysis GC-MS, further increases the usefulness of the method and the information that can be obtained. The principal diagnostic pyrolysis species which can be detected in pyrograms of plastics are shown in Table 4. It can be seen from the above list that certain plastics ‘unzip’ to regenerate their monomers whereas other undergo decomposition reactions to generate characteristic breakdown products. In reality, a certain amount of both types of reaction take place for the majority of polymers and it is the one that predominates that determines what the major pyrolysis products will be. With respect to the quantification of the polymer component within a plastic compound, the easiest technique to use is TGA. It is also possible to detect a blend of polymers with TGA and to often obtain a semi-quantification of the blend ratio by reference to the splitting of the weight loss derivative. Unfortunately, some plastic types (e.g., PVC) undergo two stage weight loss processes when heated and the first stage (loss of hydrogen chloride) will overlap with the volatilisation of organics (e.g., plasticiser) stage. It is therefore not possible to use TGA alone to determine the polymer content of these samples. Another complicating factor is that a number of plastics (e.g., halogenated, polyamides, polyurethanes, polyesters, other heteroatom containing systems) do not completely pyrolyse during the nitrogen atmosphere region and leave a carbonaceous residue which essentially oxidises to carbon dioxide in the air region. This carbonaceous residue, which may to an extent overlap with any weight loss due to a carbon black pigment, has to be included in order to obtain an accurate polymer content.

Table 4 Diagnostic pyrolysis species in pyrograms of plastics Plastic type

Species

Polystyrene

benzene, toluene, ethylbenzene and styrene

Polymethylmethacrylate

methylmethacrylate, methyl isobutyrate

Polyethylene

n-hexane, n-pentane, other straight chain hydrocarbons

Polypropylene

branched hydrocarbons such as 2,4-dimethyl heptane

PVC

hydrogen chloride, benzene, chlorobenzenes

18

Analysis of Plastics

5 Determination of the Plasticiser and Filler in a Plastic Compound

conventional carbon black; the former having a maximum oxidation weight loss around 700 °C and the latter around 550 °C.

5.1 Determination of Plasticiser

The TGA trace for an EVA cable covering filled with a conducting black is shown in Figure 11.

Mention has already been made in Section 4 of the isolation of plasticisers from a plastic matrix by solvent extraction. Careful choice of solvent is required to ensure that the polymer itself doesn’t undergo dissolution and that the plasticiser is selectively isolated. A solvent which has been found to be useful for polymers such as PVC is methanol. The extraction is carried out under Soxhlet conditions with the weight of extract being obtained from the weight gain of the conditioned solvent reservoir flask once the solvent has been dried off at 105 °C. Having quantified the plasticiser present by extraction it is then possible to obtain an identification by the use of transmission IR. There is an excellent database available (399) which enables an identification to be made. Where the plasticisers have distinct IR spectra (e.g., phthalates and sulfonamides) it is possible to detect the presence of a blend of plasticisers. If a quantification of the blend composition is required, though, this is usually easier to achieve by HPLC then IR. The TGA technique can usually provide a good quantification of plasticiser content. Plasticisers that have higher molecular weights (e.g., so called polymerised plasticisers) can give problems as the weight loss event due to their volatilisation can merge with the pyrolysis weight loss event of the polymer. As mentioned in the above section, polymers that lose small molecules by heat degradation (e.g., HCl lost by PVC) give more complicated TGA traces and will require a solvent extraction step to determine their plasticiser level.

5.2 Determination of Fillers 5.2.1 Particulate Fillers On some occasions, carbonaceous fillers such as a conducting black (acetylene black) or graphite are added to a plastic to enable it to meet certain conductivity requirements. It is possible to use TGA to quantify these types of fillers. It is also a useful way of differentiating between these materials and

The fact that a number of rubbers (e.g., halogenated, nitrile and polyurethane) produce carbonaceous residues during the nitrogen atmosphere region has already been mentioned in Section 4.1, and care must be taken to ensure that these do not affect the quantification of the carbonaceous filler in the air atmosphere region. Use of a high resolution TGA instrument will assist in this as it will improve the separation of the two weight loss events. TGA is also convenient for the quantification of inorganic fillers such as barytes, silica and silicates. The limitation of the technique is that the total inorganic content of the plastic is obtained, with no indication of the relative proportion if a blend of inorganic fillers is present. It is therefore common practice to complement the TGA data with a least a semi-quantitative elemental technique such as XRF in order to obtain qualitative as well as quantitative data. A useful exception to this rule is where the compound contains calcium carbonate (a relatively common diluent filler), in which case the carbonate will undergo quantitative degradation at around 680700 °C into carbon dioxide and calcium oxide (which remains as a residue). It is therefore possible to quantity the amount of calcium carbonate in the sample from the carbon dioxide weight loss (which will represent 44% of the carbonate by mass) and the remaining quantity of residue will indicate if any other inorganics are present. The other technique commonly used for the quantification and isolation of inorganic materials (both fillers and additives such as glass fibres) is furnace ashing. This method is described in ISO 345-1 (1997) and a temperature of 500-600 °C is usually used. Once the ash has been obtained, qualitative information on the inorganic species present can be obtained by IR (liquid paraffin mull technique), XRF or, where the quantification of specific species is required, ICP. Some of the principal diagnostic IR absorption bands for inorganic fillers are given in Table 5.

19

Analysis of Plastics

Figure 11 TGA trace for an EVA cable cover compound showing weight loss and derivative weight loss curves

Table 5 Diagnostic IR absorption bands for inorganic fillers Filler

Band

Silica

Broad band at 950-1330 cm which peaks at 1050-1100 cm

Silicates

Broad band at 850-1300 cm which peaks at 950-1100 cm

Calcium carbonate

1420, 870 and 710 cm

Barium sulfate

1080 and 610 cm

5.2.2 Fibrous Fillers In certain applications it is necessary to impart the strength required to a plastic part by the use of a fibrous fillers. The following types are among those used: (1) Glass fibres (2) Carbon fibres (3) Synthetic polymer fibres (e.g., nylon) (4) Wood flour

20

It is usually obvious whether a plastic contains a fibrous filler from either a visual inspection or the use of a relatively low powered optical microscope. Glass fibres can be isolated and gravimetrically determined by ashing at 600 °C in a muffle furnace. Higher temperatures (above 700 °C) can cause problems as the glass will eventually reach its melting point. Confirmation that the fibres are glass can be carried out using an infrared microscope. The IR microscope will also give the cellulose spectrum which is expected for

Analysis of Plastics

the wood flour filler type, and be able to detect the type of synthetic fibre (e.g., nylon or polypropylene) used from its characteristic transmission spectrum. TGA will enable the amount of carbon fibres in a composite to be quantified. The oxidation temperature of around 700 °C (instead of the 500-600 °C experienced with carbon blacks) will also provide a confirmation of their presence. As mentioned above, synthetic polymeric fibres can be identified by the IR microscope once sufficiently isolated or, by use of their melting point, by the hot stage microscope or DSC. In the case of DSC, some quantification data can be obtained from the size of the melting endotherm providing standards are available.

antidegradant identified by reference to its molecular ion and a database. The direct probe mass spectroscopy technique can be carried out on samples in the as received state as well as sample extracts, whereas LCMS is only used for extracts.

6.1 UV Stabilisers There is a large range of commercial UV stabilisers for plastic materials and a number of analytical approaches can be used for their detection and quantification. The UV stabilisers can be divided into five different groups: (a) Benzophenone derivatives

6 Determination of Stabilisers in a Plastics Compound

(b) Salicyclic acid esters

In common with other polymer systems, to maintain the physical properties of a plastic compound stabilisers need to be added to stop, or at least retard, degradation by a number of agencies (e.g., heat and UV light).

(e) Coumarin drivatives

The use of an initial solvent extraction/dissolution step is common in the analysis of a plastic matrix for antidegradants, as these species may not be volatile enough to be removed by heating the sample. In some cases (e.g., butylated hydroxytoluene) heating a sample liberates enough of the species to enable an identification to be made using GC-MS; however quantification will usually require removal by a solvent (to as near 100% efficiency as possible). Analysis of the extract can then be carried out by HPLC, UV spectroscopy, or GC if the species is heat stable and sufficiently volatile. Relatively non-specific solvents (i.e., having mid-range solubility parameters) such as chloroform are good extracting solvents. Another common approach is to dissolve up the sample in a suitable solvent and then add a nonsolvent to precipitate the polymer. The stabiliser will remain in the solvent phase. If the type of organic antidegradant in a compound is completely unknown, analysis of the solvent extract by GC-MS or LC-MS is an excellent method for identification. Once the identification has been achieved, a quantification can be carried out using a preferred method and a validated procedure if available. Where the antidegradant is not volatile enough to be identified using a GC based technique, direct probe mass spectrometry or LC-MS can be used and the

(c) Resorcinol esters (d) Benzotriazole compounds

In a number of cases specific methods have been developed to determine a particular stabiliser within a particular polymer. Some representative methods are outlined next. In some cases (e.g., the determination of 2-hydroxy-4n-octoxybenzophenone in polyethylene) the stabiliser has distinctive diagnostic bands and the relative simplicity of the infrared characteristics of the polymer matrix enables it to be quantified using transmission infrared spectroscopy. A thin film of the sample is produced by hot pressing at 120 °C, along with films of virgin polyethylene containing known amounts of the stabiliser. The absorbance maxima of the diagnostic band between 15.8 and 16.2 microns in the standard films is used to produce a calibration curve from which the amount of stabiliser in the unknown is calculated. The method is capable of detecting the stabiliser down to 0.02% w/w with an accuracy of +/- 5%. A number of methods use the UV absorbing properties of the UV stabiliser. For example, Tinuvin 326 can be detected in polypropylene down to 0.02% w/w by using an extraction with chloroform under reflux followed by analysis of the extract using a UV/Vis spectrometer. The ultraviolet absorption peak at 355 nm is used and a calibration curve produced by dissolving known amounts of Tinuvin 326 in chloroform. Another technique uses the fluorescence of these compounds. Uvitex OB can be detected in a chloroform

21

Analysis of Plastics

solution (0.8% w/v of polymer) of polystyrene by excitation at 370 nm and recording the fluorescence at 435 nm. Standard solutions at the 0.8 w/v level of virgin polystyrene and known amounts of Uvitex OB are used as calibrants. It is also possible to use gas chromatography (e.g., Tinuvin P, Tinuvin 326, Tinuvin 327 and Cyasorb UV531 in toluene extracts of polyethylenes), thin layer chromatography (e.g., benzophenone and salicylic acid types in polyethylenes) and HPLC. This latter method has been used extensively for the determination of antioxidants but has not received as much attention in the literature for UV stabilisers. It is also the case that the white pigment titanium dioxide provides protection against UV light and so this can be added at reasonable high loadings (e.g., 10% or greater) to products such as window frames. The amount of titanium dioxide in a plastic can be determined after acid digestion of the matrix by the use of an elemental technique such as AAS/ICP.

6.2 Antioxidants HPLC based techniques have been widely used by analysts for the determination of antioxidants in plastics and a review has been provided by Sidwell (400).

The chromatogram obtained for the determination of Irganox 1076 in an HDPE compound is shown in Figure 12. An extract of the polymer was analysed using a C18 reverse phase column with UV detection at 230 nm and a mobile phase of 70:30 methanol/water changing to 100% methanol. There is a useful HPLC method which can be used on plastics for the detection and quantification of a wide range (20 species) of antidegradants. The sample is dissolved up using a suitable solvent at an elevated temperature if necessary. A non-solvent (e.g., methanol) is then added and the extract analysed by HPLC using the following conditions: Injection volume

25 μl

HPLC column

Aqua 5 C18 ODS reverse phase column 150 mm x 3.0 mm (or similar)

Mobile phase

A= 75:25 Methanol/Water B= 50:50 Ethyl Acetate/Acetonitrile

Gradient

Time Initial After 25 min

Flow rate

2.0 ml/min

Figure 12 HPLC chromatogram of HDPE for determining Irganox 1076

22

%A 90 0

%B 10 100

Analysis of Plastics

Detection

UV detector set at 270 nm

Temperature

40 °C

The chromatogram obtained using this method to separate a complex cocktail of antidegradants is shown in Figure 13.

The following antioxidants are examples of those that can be determined using this technique:

The wide applicability of this method is due to the mobile phase mixture.

(1) Irganox 1010

The capability of HPLC has been greatly extended by the commercialisation of affordable liquid chromatography-mass spectroscopy (LC-MS) instruments. The mass selective detector enables unknown samples to be analysed and the antioxidants present to be identified. The LC-MS technique therefore compliments GC-MS and, with it, enables the complete molecular weight/volatility/polarity range to be covered.

(2) Irganox 1098 (3) Irganox 1076 (4) Irganox 1330 (5) Butylated hydroxytoluene (6) Irgafos 168 (7) Triclosan

TLC is comparatively easy and cheap to use and it is both quick and accurate for the identification of

Figure 13 HPLC chromatogram of a complex mixture of antidegradants

23

Analysis of Plastics

antioxidants in plastic extracts. Irrespective of the complexity of the extract composition and the amount used, this method can be used to give a sharp separation for identification purposes. Distinctive Rf values and colours can be seen for each antioxidant depending on the stationary phase, the developing solvent used and the detection agent. TLC, in addition to being used for identification purposes, can be used in a semi quantitative way; the logarithm of the spot area being proportional to the quantity of the analyte in the spot, and this value being compared to spots containing standard amounts of the analyte. Gas chromatography has been used for the analysis of phenolic and amine type antioxidants. Antioxidants which have high boiling points cannot be directly by GC but they can be analysed as derivatives such as acetates, trifluoroacetates, trimethyl silyl-ethers, methyl ethers, etc. Trimethyl silane based antioxidants, for example, give good separations on standard silicone based columns (a.10). Benchtop LC-MS instruments are proving to be excellent tools in the analysis of plastics of unknown composition to identify and, once this is achieved, quantify the antioxidant present. Prior to the advent of LC-MS it was very difficult to use conventional HPLC for this task because of the large range of possible compounds. Using the general analysis conditions shown below a number of antioxidants can be detected in toluene or chloroform extracts of plastics: Sample preparation: Around 5 mg of extract is diluted 1/20 with 80% acetonitrile/water Instrument:

Agilant 1100 series LC-MS

Column:

Zorbac SB-C18, 5 um, 2.1 mm x 150 mm

Mobile phase: A=water, B=acetonitrile Gradient

Time

A

B

Initially after 10 min

15% 1%

85% 99%

or

Initially after 10 min

35% 10%

65% 90%

Flow rate:

0.7 ml/min

24

Injection volume: 5 μl MS conditions:

Atmospheric Pressure Chemical Ionisation (APCI)

Ion mode:

Positive or negative

Vapouriser:

300 °C

Scan range:

200-1600 amu

Fragmentor:

70 or 120 volts (The fragmentor voltage is chosen to modify the degree of fragmentation and hence sensitivity)

Antioxidants which have been identified in polyolefins using the above conditions include: •

Irgafos 168

•

Irganox 1076

•

Irganox B225 (50:50 mixture of Irganox 1010 and Irgafos 168)

7 Determination of Functional Additives 7.1 Process Aids and Lubricants In PVC technology certain polymeric additives can be considered as process aids. These polymers have a similar composition to those used as impact modifiers in PVC formulations but are more compatible and so are primarily included to ensure more uniform flow and hence improve surface finish. Such process aids include ABS, chlorinated polyethylene, MBS, EVAPVC graft polymers and acrylate-methacrylate copolymers. As these are usually found in unplasticised PVC, direct analysis of the product by IR will usually indicate the presence of those that have a distinctive spectrum as no masking by plasticiser will take place. However, even rigid PVC can contain a small amount of phthalate and so it is advisable to carry out a solvent extraction to clean up the matrix first. Where the process aid (e.g., chlorinated polyethylene) has a relatively bland spectrum, a technique such as NMR will be required to both detect and quantify it. NMR will usually be required to quantify the other types as well, unless the spectrum is very distinctive and standards of known composition are available.

Analysis of Plastics

In the case where a relatively large quantity of filler (talc) has to be incorporated into a polymer (e.g., polypropylene) it is often necessary to use a process aid/lubricant such as a zinc or calcium stearate. A quantification of the process aid can be achieved by the analysis of the sample for the metal by acid digestion-AAS. The stearate can be qualitatively detected by solvent extraction GC-MS.

7.2 Slip Additives It is common for aliphatic amides to be incorporated into plastics, particularly polyethylenes, to act as slip additives. It is possible to use LC-MS to detect these types of slip additives in plastic samples. Using the LC-MS conditions described in Section 6.2, it is possible to detect Behenamide (mixture of two aliphatic amides of molecular weight 331 and 339) and erucamide (molecular weight 337) in solvent extracts of polyethylene and polypropylene. It is also possible to use GC and GC-MS to analyse these and another common slip additive oleamide in extracts from plastics as they have sufficient volatility to elute from the GC column.

7.3 Pigments Pigments are used extensively in plastic compounds and can be of one of four main types:

available, they have relatively high molecular weights and so cannot be easily removed from the matrix by solvent extraction and can be thermally labile. One technique which has been used to identify both these types of pigment and inorganic ones is vapour phase ultraviolet absorption spectrometry at 200 nm (a.11). In this method the samples are powdered and then directly vapourised in the heated graphite atomiser. Thermal ultraviolet profiles of organic pigments show absorption bands between 300 °C and 900 °C, while profiles of inorganic pigments are characterised by absorption bands at temperatures above 900 °C. Specific assignments are made with respect to temperature, relative intensity and width of the absorption bands. A relatively unknown technique (laser desorption fourier transform ion cyclotron resonance mass spectroscopy) has been used (397) to identify dyes in plastics such as polymethylmethacrylate. A detection limit of 0.1% was obtained, which compared with a limit of 1-2% using an ATR infrared spectroscopy technique. Infrared spectroscopy techniques can be useful, particularly if the plastic matrix itself (e.g., polyethylene) has a relatively simple infrared spectrum and if standard infrared spectra of a wide range of pigments is available. Carbon black is used extensively as a black pigment in products such as cable sheaths. The amount present is usually less than 2% and so its quantification by TGA can be difficult due to the small sample size (10 mg) used. The standard method to quantify the amount of carbon black in such a product is therefore the tube furnace as much larger sample sizes can be used (e.g., 2 g) and hence more accurate quantifications obtained.

(1) Inorganic compounds (2) Organo-metallic compounds

7.4 Antistatic Agents

(3) Organic compounds (4) Carbon black Pigments such as titanium dioxide and iron oxide belong to the first group and the analysis of these is relatively easy as they are thermally stable (so can be determined in both the sample ash or in the sample in the as received state) and have a diagnostic metal atom together with a simple chemical structure. Analysis techniques used are therefore elemental methods such as AAS and ICP. Groups 2 and 3 present the analyst with a greater challenge as there is a very wide number commercially

Antistatic agents are usually hygroscopic compounds which readily attract moisture and so inhibit the build up of a static charge on the surface of a plastic product. They are used in many applications from the body of the humble plastic pen to numerous packaging applications. The selection of an antistatic agent depends greatly on the polymer matrix since a degree of incompatibility is vital to ensure that migration to the surface of the product occurs at a fast rate after manufacture. Exact chemical composition information can be difficult to obtain from suppliers and so analysis for these additives can be difficult.

25

Analysis of Plastics

In the case of polystyrene, quaternary ammonium compounds are widely used and for polyethylene, polyethylene glycol alkyl esters can be used. In the case of the glycol esters, these can of sufficiently low molecular weight to be extractable by solvents such as diethyl ether and then identified by a chromatographic technique such as GC-MS. As in a number of cases it is to be expected that LC-MS will play a role in the analysis of these additives in the future.

7.5 Crosslinking Agents and Co-Agents For some plastic products (e.g., cable sheathing) it can be necessary to impart a degree of crosslinking into the product to achieve the requisite physical properties. This can be achieved by irradiation using gamma rays. However, some polymers degrade when subjected to high energy radiation as illustrated in Table 6. Chemical agents such as peroxides are also used. These species produce diagnostic breakdown products the identification of which will reveal the type of peroxide used. The most useful technique for this type of work is GCMS. There are two possible modes of sample introduction: solution injection and dynamic headspace. In the case of the former a useful method of sample preparation involves cryogenic grinding of 0.3 g of the sample, followed by extraction using 2 ml of diethyl ether in an ultrasonic bath for 30 minutes. The resulting extract is then analysed under the following conditions: Instrument:

Hewlett Packard 6890/5973 GC-MSD

Carrier:

Helium @ 2.0 ml/min constant flow

Column type:

RTX5-MS 30 m x 0.25 mm, 0.25 μm film thickness

Column temperature:

40 °C for 5 min, 20 °C/min up to 300 °C held for 12 min

MS settings:

20 to 620 Daltons scanned every 0.33 s

In the case of the dynamic headspace approach a relatively small amount of sample (e.g., 3 mg) is heated in the oven of a dynamic desorption unit and the volatiles produced collected in a cryogenically cooled Tenax filled trap. The experimental conditions are as follows: Dynamic Headspace Instrument:

Perkin Elmer ATD 400

Desorption temperature:

150 °C for 10 min

Desorption flow:

Helium @ 20 ml/min

Trap collection temperature: –30 °C Trap injection temperature:

250 °C

Trap outlet split flow:

9 ml/min

Trap inlet split flow:

off

Split:

10:1

GC-MS The conditions used are the same as for the diethyl ether method with the exception of the following:

Injection mode: 1 μl splitless (0.75 min; 50 ml/min)

GC Column temperature: –30 °C to 50 °C at 5 °C/min, following by 20 °C/min to 300 °C and then held at 300 °C for 12 min

Injection temperature: 320 °C

Carrier

Helium @ 0.07 MPa

Table 6 Behaviour of polymers subjected to high energy radiation Polymers that crosslink

Polymers that degrade

Polyethylene Polyacrylic acid Polymethyl acrylate Polyacrylamide Styrene-acrylonitrile copolymers

Poly(α-methylstyrene) Polymethyl methacrylate Polymethacylic acid Polyvinylidene chloride PCTFE PTFE Polypropylene

26

Analysis of Plastics

Table 7 Diagnostic species associated with different cure systems Peroxide curative

Diagnostic species

Perkadox 14/40

Tertiary butanol 1,3 Di-(1,1-Dimethylmethanol) benzene methanol)

Tert-butyl cumyl peroxide

1,1-Dimethyl benzene methanol Acetophenone Tertiary butanol

Dicumyl peroxide

1,1-Dimethyl benzene methanol Acetophenone

For either analytical approach, identification of the diagnostic cure system breakdown species is by reference to mass spectral libraries such as those produced by the National Institute of Standards and Technology (USA) (NIST), the Royal Society of Chemistry, Wiley/NBS (a.12) and the US Environmental Protection Agency (EPA)/National Institute of Health (NIH). The mass spectra of the majority of species of interest are in these libraries and so, providing the knowledge to reconstruct cure systems is available, successful attempts can be made. One problem associated with this task is that a number of peroxide curing agents breakdown to give more that one product and a number of these are common to more than one peroxide species. This is demonstrated in Table 7. In addition to identifying the type of peroxide used, these GC-MS techniques will also identify the type of co-agent (e.g., triallyl cyanurate (TAC) or triallyl isocyanurate (TAIC)) used.

7.6 Blowing Agents There are two main types of blowing agent used with polymer systems in general: (1) Chemical Chemical compounds (principally organic) that undergo chemical decomposition at the processing temperature to form a gaseous species (e.g., nitrogen) which will create the cellular structure. Examples include azo compounds, nitroso compounds, sulfonyl hydrazide compounds and sodium bicarbonate.

(2) Physical

Low boiling point organic compounds (e.g., dichloromethane or pentane) which volatilise at the processing temperature to create a cellular structure.

With plastics, the most widely used type are the physical blowing agents. Where it is suspected that a physical type blowing agent has been used to produce a foam, is it possible to use headspace GC-MS to identify it. Even in the blown state, the high sensitivity of the technique enables an assignment to be made from the small amount of residual blowing agent that will be present. It is usual to use this type of blowing agent in amorphous plastics that have glass transition temperatures around 100 °C, e.g., styrenics. This enable the expansion of the plastic to be well controlled. The reactivity of the chemical blowing agent type can make analysis difficult (e.g., they will decompose in the injection port of a GC-MS instrument), and the approach that is used is to indirectly identify them by the determination of breakdown fragments. The GCMS instrument is the best choice for this and a library of typical breakdown fragments is required. Quantification of the chemical blowing agent in an unblown product is very difficult as the polarity and reactivity (e.g., hydrogen bonding reactions and thermal instability) can cause problems during isolation from the compound and subsequent analysis. In terms of reverse engineering, this is unlikely to be required since the product will invariably be already blown. For laboratories that are carrying out quality control work, other properties such density and expansion ration can be used to determine compound loadings.

27

Analysis of Plastics

7.7 Flame Retardants As with blowing agents, there are two main categories of flame retardant: organic and inorganic. The amount and type of organic flame retardant present in a plastic compound can be determined in an analogous way to the plasticiser, since this type of flame retardant is usually similar in molecular weight and polarity and, hence, extractability. Once the type of organic flame retardant has been determined by IR, an accurate quantification can be obtained by carrying out an elemental analysis for the halogen (or other relevant element, e.g., phosphorus) on the unextracted sample. The extract value itself will rarely provide a meaningful quantification as other species, particularly any process aid/plasticiser, will contribute to it as well. In some instances (e.g., organophosphates) it may be possible to use an HPLC analysis of the extract to quantify the flame retardant. GC based techniques can also be used in some cases, but bromide types present problems for these techniques because of their relatively high molecular weights (> 900). Care must be taken over the quantification of inorganic flame retardants, since some of them (e.g., antimony trioxide) can react with the organic flame retardant present, or break down to produce volatile products, under quantitative ashing conditions, and during analysis by thermal techniques such as TGA. A good initial approach is a semi-quantitative elemental analysis by XRF, to see which types are present. Accurate quantifications can then be obtained by precise elemental determinations. If it is known that hydrated alumina is present in the sample, it is possible to quantify this reasonably well using TGA, by making use of the water loss data. Hydrated alumina loses close to 35% of its weight when it is heated to 550 °C in a TGA experiment.

distribution within the matrix of the domains that contain it. Actual impact performance is determined by physical tests such as the Charpy and Izod impact tests, and the size and distribution of domains is investigated by transmission electron microscopy (TEM), but there are a number of chemical tests that can be carried out to determine the level of modifier. (1) IR analysis - this is performed on a pressed film and the relative size of the absorption bands due to styrene (700 cm) and butadiene (966 cm) are taken and compared to standards of known styrenebutadiene levels. (2) NMR - the plastic is dissolved and the level of the two polymers determined by specific shift areas. (3) Classical wet chemistry - the butadiene level is determined in solution by reaction of a reagent with the double bonds. There are some instances (e.g., rubber impact modification of nylon) where the chemical properties of the two polymers are so dissimilar that solubility differences can be used to isolate and, in this case, quantify the rubber modifier. The test is carried out by taking an accurately weighed sample and refluxing it in formic acid until the plastic is digested and only the rubber phase remains. The rubber is then washed, dried and weighed. Other plastics which can contain rubber modifiers (or at least modifiers that have lower glass transition temperatures than the plastic phase) include PET and PVC. In the case of PVC, acrylates and methacrylates are common and the normal approach is to use IR to detect the modifier and then NMR to quantify it.

8 Analysis of Plastics for Food Contact Use 7.8 Impact Modifiers The most commonly encountered impact modified plastic is high impact polystyrene (HIPS). The impact modification is achieved by incorporating discreet domains of a rubber (butadiene) within the polystyrene matrix. The level of butadiene can be varied according to the requirements of the end use. A high level can convert a glassy brittle material into a ductile, tough product. The efficiency of the butadiene to improve impact resistance alone is not solely related to concentration, but is also dependent on the size and

28

For more than 30 years work has been going on involving food contact plastics and the effect that migrants from plastics products have on food. The first European Directive (78/142/EEC), which was on the vinyl chloride monomer content of food contact PVC, was published in the late 1970s and this was followed ultimately by the more comprehensive Plastics Directive (90/128/EEC) in 1990. Since 1990, there has been a gradual harmonisation of European testing requirements through amendments to 90/128/EEC. The seventh amendment (2002/17/EC) has recently been

Analysis of Plastics

published and the initial requirements for testing overall and specific monomer migration have now grown to include additive (e.g., antioxidant) migration. In general, there are two types of analytical test that are carried out on food contact plastics: (1) Global migration tests - In these, the plastic is put into contact with an appropriate food simulant under representative end use conditions and the total amount of material that has migrated into the simulant determined gravimetrically or, in the case of involatile food simulants such as olive oil, by gas chromatography. (2) Specific migration tests - Again, the plastic is contacted with a food simulant but any analytical work in targeted on a specific additive and its concentration determined using an appropriate chromatographic technique. In the case of certain plastics materials, e.g., ABS, grades that are intended for food use have to meet certain residual monomer targets. Direct analysis of these polymers is undertaken to determine the concentration of these monomers.

8.1 Global Migration Tests The following food simulants are used for food contact plastics: Distilled water - Aqueous food use Distilled water 95%:Ethanol 5% - Alcoholic beverages such as beers and lagers Distilled water 85%:Ethanol 15% - Wines Distilled water 60%:Ethanol 40% - Spirits A solution of 3% w/v acetic acid in distilled water Acidic aqueous foods Olive oil* - Fatty foods (also isopropanol or hexane) (*Isopropanol and Hexane have been introduced as fatty food simulants to circumvent the analytical problems that can occur with olive oil due to its potential variability as a natural product and involatility.) As mentioned, the global migration figure for a particular plastics material is determined gravimetrically. One

Table 8 Contact time and temperature for food contact testing (EC Directive 82/711/EC) Conditions of contact in actual use

Test conditions

1. Contact time > 24 hours T < 5 °C

10 days at 5 °C

5 °C < T < 40 °C

10 days at 40 °C

2. Contact time between 2 hours and 24 hours T < 5 °C

24 hours at 5 °C

5 °C < T < 40 °C

24 hours at 40 °C

T > 40 °C

In accordance with National Laws

3. Contact time less than 2 hours T<5

2 hours at 5 °C

5 °C < T < 40 °C

2 hours at 40 °C

40 °C < T < 70 °C

2 hours at 70 °C

70 °C < T < 100 °C

1 hour at 100 °C

100 °C < T < 121 °C

30 min at 121 °C

T >121 °C

In accordance with National Laws

29

Analysis of Plastics

approach is to use conditioned glass crucibles and to dry off the simulant on a hot plate after the contact experiment has been performed under the appropriate conditions (time and temperature). Once the appropriate simulant has been chosen the contact time and temperature to use are given in EC Directive 82/711/EEC (Table 8). In addition, for plastics in contact with food for which a preservation temperature of less than 20 °C is required the test condition will be 10 days at 20 °C. The overall global migration limit for plastics is stated in the EC Directive 90/128/EEC as being 10 mg/dm2 (surface area of plastic). This limit can be expressed as 60 mg/kg of foodstuff in certain situations. To be used for food contact a plastics product must meet this requirement. In a number of packaging types, only one side of a plastic film or laminate may contact the food. Specific single side migration cells have been developed (e.g., by PIRA) to enable the migration from a material under these conditions to be investigated.

8.2 Specific migration and residual monomer tests In addition to the global migration limit 90/128/EEC also provides a number of specific migration limits (SMLs) for plastic monomers (Table 9). There are also SMLs for plastic additives, some examples are shown in Table 10. In the case of some monomers, 90/128/EEC gives limits (called quantification limit-monomer (Qm)) relating to the plastic material itself. For example, vinylidene chloride has a QM of 5 mg/kg of plastic. Over the years, the detection of species migrating from food contact materials has advanced hand in hand with the gradual lowering of analytical detection limits brought about by the refinement of the techniques. For example, the SML for acrylonitrile is set at not detectable above 0.02 mg/kg (i.e., 20 parts per billion) and this would not be obtainable on a routine basis without the benefits of modern instrumentation. The development of suitable methods for the detection of the wide range of monomers and additives used in

Table 9 SMLs for plastic monomers (90/128/EEC) Monomer

SM L

Vinyl acetate

12 mg/kg foodstuff

Acrylonitrile

Not detectable above 0.02 mg/kg foodstuff

Caprolactam

15 mg/kg foodstuff

Formaldehyde

15 mg/kg foodstuff

Terephthalic acid

7.5 mg/kg foodstuff

Vinylidene chloride

Not detectable above 0.05 mg/kg foodstuff

Table 10 SMLs for some plastic additives (90/128/EEC) Additive

SM L

Adipate and phthalate esters

1.5 mg/kg foodstuff

Antimony trioxide

0.01 mg/kg foodstuff

BHT

3.0 mg/kg foodstuff

Hydrogenated hydrocarbons

3.0 mg/kg foodstuff

Conventional hydrocarbons

0.3 mg/kg foodstuff

Oleamide/stearamide

Cannot be used for fatty food use

30

Analysis of Plastics

food contact materials requires the application of state of the art analytical techniques. Normally, headspace methods are preferred for volatile monomers as such methods overcome a lot of the problems of sample matrix clean-up. In principle the food contact simulant, foodstuff or plastic material is heated in a sealed vial fitted with an inert septum (usually PTFE coated rubber). The vial is heated to an accurate set temperature normally in the range 80-100 °C, for an equilibrium time of at least one hour. The headspace above the sample is then analysed for the presence of the analyte. The quantity of analyte in the headspace will always be in equilibrium with the amount present in the sample. Standard addition methods are used to obtain calibration curves, with the calibrant vials being analysed under the same conditions (i.e., time, temperature and ratio of headspace to bulk material (polymer if necessary)) as the samples. To acquire sufficiently low detection limits it is sometimes necessary to use specific detectors (e.g., a nitrogen/ phosphorus detector (NPD)) or, in the case of mass selective detectors, a single ion monitoring approach. For species that are too involatile for headspace based methods, other chromatographic and spectroscopic methods are employed. A summary of the analytical techniques used in food migration work is shown in Table 11. In the cases where HPLC has been assigned, LC-MS would also be applicable.

9 Determination of Stabilisers in PVC Although it is one of the bulk thermoplastics, PVC suffers from relatively poor stability to ageing agencies such as heat and UV light. In order to achieve its status as an important plastic it was therefore necessary to develop a specific additive group: PVC stabilisers. These technological developments have resulted in a range of stabilisers being available that are appropriate for different grades of PVC, products and end uses. Some of the main types are: (a) Lead stabilisers (e.g., lead carbonate, lead stearate, lead phthalate) (b) Metallic soaps (e.g., stearates, palmitates, ricinoleates and octoates of cadmium, barium, calcium and zinc) (c) Organo-tin compounds (e.g., dibutyltin di-isooctylthioglycollate) (d) Epoxide stabilisers (e.g., epoxidised oils and bisphenol A epoxide resins). The analyst has to bear in mind that it is common for a number of different stabilisers to be used in a PVC compound in order achieve the optimum ageing resistance.

Table 11 Analytical techniques used in migration testing Analyte

Technique

Vinyl chloride

Headspace GC

Styrene

Headspace GC and HPLC

Terephthalic acid

HPLC

Ethylene glycol

Headspace GC

Acrylonitrile

Headspace GC with NPD

Butadiene

Headspace GC with mass selective detector (MSD)

Isocyanates

Derivatisation HPLC

Formaldehyde

Derivatisation colorimetry

Organic acids

Ion pair HPLC or IC

Plasticisers

HPLC

Antioxidants

HPLC, GC or SFC

Inorganics

AAS or ICP

Polar organics

HPLC and capillary electrophoresis

31

Analysis of Plastics

It is obvious that a large number of these stabilisers contain metal atoms and so a cost effective way of achieving an initial evaluation of the type of stabiliser present is to use a semi-quantitative XRF technique on the sample in the as received state. Care should be taken with this as some inorganic pigments/fillers (e.g., titanium dioxide) can mask certain key elements (e.g., cadmium). If it is a case of quantifying a known stabiliser, then AAS or ICP can be used to quantify the metal and, with knowledge of the compound formula, the result obtained. The organo-tin compounds are widely used and for analytical considerations it is convenient to divide them into those that contain sulfur and those that do not. To the first group belong compounds like dialkyltin mercaptides, mercaptoesters and mercapto carboxylates, to the second, dialkyltin carboxylates and their esters. The identification of acids and alcohols present in tin stabilisers containing no sulfur and the identification of alcohols from stabilisers containing mercaptoesters presents little or no difficulty. However, the identification of the thioacid and of the alkyl groups attached directly to tin can prove more difficult, especially if long chain acids form part of the compound or if the stabiliser is not pure, e.g., if it contains plasticiser. The thioacid may also tend to decompose during hydrolysis procedures. The application of a number of analytical methods (e.g., NMR, IR and GC) to determine these types of stabiliser in PVC extracts have been described by Udris (a.13). Some classic methods based on titration and TLC to determine organo-tin compounds in solvent extracts of PVC include: •

Potentiometric titration of organo-tin in the extract with standard sodium methoxide in pyridine using antimony and calomel electrodes (a.14).

•

Titration of dialkyltin thiol compounds in benzene/ methanol extract with standard silver nitrate (in IPA medium) using sulfide coated wire electrode (a.13).

•

TLC of organo-tin thioacids and thiols using Kielselgel G plates with development with glacial acetic acid and detection with catechol violet (a.15).

•

32

TLC of organo-tins using Kieselgel GF 254 with development using butanol/glacial acetic acid and detection with catechol violet and UV irradiation (a.16).

Of the other types of organo-metallic stabilisers, Mal’kova and co-workers (a.17) have described an alternating current polarographic method for the determination of cadmium, zinc and barium stearates or laurates in PVC. Other techniques used on PVC extracts include, column chromatography for barium, cadmium and zinc salts of fatty acids, paper chromatography for cadmium, lead and zinc salts of fatty acids (a.18) and polarography for cadmium, lead and zinc salts (a.19). The advent of bench top LC-MS instruments has enabled the analysis of stabilisers such as the organotin type to be re-examined and laboratories such as the Analysis Division at Rapra Technology Limited are investigating the capability of this technique in this area. This could be another area of plastics analysis where LC-MS replaces the more traditional techniques.

10 Analysis of Plastic Laminates and Fibres Plastic laminates are used extensively from the ordinary crisp packet to high specification products for medical and pharmaceutical use. In all these cases, laminates are used since the application demands a number of properties which no single polymer exhibits. Taking the example of the crisp packet, the innermost layer must be inert to the product and provide a barrier to air, the outside layer has to be capable of being printed onto and the middle layer (or tie layer) has to be able to stick both of the other two together. One of the principle analytical techniques for the analysis of laminates is the infrared microscope. This instrument is capable of recording transmission infrared spectra from sample down to 10 square microns in size. The approach is usually to prepare a section of the laminate by microtoming a section and then recording a spectrum of each layer aided by the masking off of the other layers. The sectioning is often undertaken obliquely in order to maximise the apparent layer thickness. The microscope also allows the thickness of each layer to be determined. It is also possible to use an ATR technique to record infrared spectra of the outside layers and reserve the IR microscope for the central layers. This is possible because the ATR technique only penetrates a few microns into the surface of the layers. It is also possible by choosing the appropriate crystal (e.g., germanium,

Analysis of Plastics

zinc selenide, etc) to control the depth of penetration. This can be useful if the layers are particularly thin. Using the knowledge gained by infrared spectroscopy of the generic polymer types present, the assignments can be refined by the use of DSC. Due to the fact that laminates by their nature are often constructed of completely different plastic types, the complete structure can be analysed in one operation and the melting endotherm transitions obtained used to differentiate between various grades. For example in the case of a laminate which had been shown to be comprised of a polyethylene and a nylon, it would be possible to differentiate between LLDPE, LDPE and HDPE, and nylon 6 from nylon 6,6. It is also possible to use a Raman microscope to analyse the different layers that are present within a laminate. As with the IR microscope, it has the ability to isolate individual layers and, given a satisfactory database, the spectra obtained can be used for identification purposes. The Raman spectra for four common polymer types are shown in Figure 14. Examination of the cross section of laminate samples under an optical microscope enables the individual layers to be viewed. Phase contrast microscopes can aid the differentiation of layers of similar refractive index. The use of a polarising microscope can also assist in characterising individual layers and is particularly useful when heating laminates under a microscope on a hot stage to recognize the characteristic melting temperature of the individual layers. There are a number of synthetic fibres that can be used to produce both woven and non-woven fabrics. The most popular include polyamide, polyester and acrylics and they can be used in products as varied as clothing and life rafts. Once again, the infrared microscope is ideal at recording generic polymer identification spectra from individual fibres. Once the generic type has been established, further refinement of the assignment can be obtained by DSC (e.g., specific polyamide type) and, where a number of fibres are available GPC (molecular weight). Other microscopic techniques, such as optical (aspect ratio), SEM (surface morphology) and EDAX (elemental analysis), Raman microscopy and atomic force microscopy can be used to further characterise the product.

Figure 14 Raman spectra of (a) polyethylene, (b) PVC, (c) polystyrene and (d) polyethylene terephthalate

33

Analysis of Plastics

11 Surface Analysis of Plastics There are a number of analytical techniques that can be used to obtain data on the surface of plastics materials or products. Three of the techniques, IR and Raman microscopy and Edax are covered in Sections 2.2.1, 2.2.6 and 2.6. It can be argued that these techniques have come into being as the logical development of the original, general purpose techniques. There are however a number of analytical instruments that have been developed with the specific intention of analysing surfaces. Three of the principal ones will be mentioned in this section.

11.1 X-Ray Photoelectron Spectroscopy (XPS) In this case the surface of the sample is irradiated with soft X-rays. These X-rays are sufficiently energetic to cause photoemission of electrons from the core levels of atoms present on the sample surface. The photoelectrons generated are collected and passed to an electron energy analyser and detector. The measured kinetic energy (KE) of an electron is given by : KE = hv - BE - sigma where: hv = energy of the X-ray photon BE = Binding energy sigma = work function of the spectrometer The binding energy of a given core electron is characteristic of the element and it is this which enables the elements on the surface of a sample to be identified. It is also possible to carry out quantitative work by measuring the relative intensities of the photoemission from each of the elements present. The binding energy of a core level depends principally on the charge on the nucleus of the atom concerned and smaller changes are induced as a result of chemical bonding. Although small, such charges are measurable and provide a means of studying the chemistry of the sample surface (a.20, a.21). Because only electrons from the top few atomic layers will have sufficient energy to escape, the technique is very surface specific and results are normally obtained from between 5 and 10 nm depth at a detection limit of around 0.1 atom percent. The analysis area is typically 3-10 mm2 and all the elements with the only exception of hydrogen can be detected.

34

Because of its ability to determine surface chemistry, XPS can be particularly useful in the analysis of polymer surfaces to see if oxidation has taken place and, if so, what functional groups (e.g., ester, acid, aldehyde) the oxygen is present in. This ability of XPS to detect oxygen containing functional groups is shown in the narrow and broad scan spectra of PET presented in Figure 15. Another application is the analysis of polymers to determine if certain surface treatments (e.g., corona discharge) have been carried out satisfactorily. In common with the other surface analysis techniques, it can also be used to investigate surface contamination problems and to determine the composition of the fracture surfaces in adhesion failures.

11.2 Laser Induced Mass Analysis (LIMA) In the LIMA technique, the surface of the sample is subjected to a pulsed UV laser which is sufficiently energetic to volatilise a small volume (about 1 μm cube) of material. The ionised fragments in this volume are then separated and identified by means of a time of flight mass spectrometer. Both negative and positive fragment data can be obtained. The analysis area in a LIMA experiment is typically 1-2 μm, the analysis depth 0.25-0.5 μm and the detection limit 10-100 ppm. The technique has the ability to detect all of the elements in a qualitative way. The technique is very useful for determining compounds on the surface by means of these elements and molecule fragments, but it is very sensitive, and care must be taken to ensure that the surface is not contaminated (e.g., by handling without gloves) and that the representative control samples are available to assist in the interpretation of the data. Its sensitivity and surface specificity make it ideal in the detection of very low levels of contamination/ modification. For example, the detection of a monolayer of silicone contamination of a plastic part that was hampering the wetting of a paint. It can also be used to analyse particulate impurities, fibres and defects in surface coatings. LIMA is also referred to as laser microprobe mass spectroscopy (LAMMS).

Analysis of Plastics

(a)

(b)

Figure 15 XPS spectra of PET (a) narrow spectrum (b) broad spectrum

35

Analysis of Plastics

11.3 Secondary Ion Mass Spectroscopy (SIMS) In this technique the sample surface is bombarded by a primary ion beam (positive ions of argon, caesium, oxygen or gallium). These primary ions impart energy to the surface and, as a consequence of the collisions produced, ions, atoms and molecular fragments (called sputtered particles) are ejected. The primary ions may penetrate several atom layers into the surface, but the sputtered particles only come from the outer 2-3 atom layers. In common with the other two techniques, therefore, SIMS is very surface specific and it is possible to restrict it to a single monolayer. The analysis area is typically 150 μm, the detection limit is 1 ppm and all the elements are detectable. Two types of SIMS experiment can be carried out: static SIMS and dynamic SIMS. In the former case, the surface is bombarded with low energy ions and molecular and atomic fragments are produced without the experiment changing the nature of the surface appreciably; the surface chemistry can therefore be investigated. Dynamic SIMS uses high energy ions to obtain highly sensitive elemental data down to ppb levels, but the structural information is lost. In the case of static SIMS, dedicated libraries are required to enable the mass spectra of the fragments to be identified (a.22). Another application of SIMS is in the study of the migration of additives (e.g., slip additives and antistats) onto the surface of plastics. It is often the case that complementary surface analysis techniques such as SIMS and XPS can be used together in order to successfully solve a failure or characterisation problem. In such cases, XPS would be used to generate quantitative information, whilst SIMS would provide qualitative clues with respect to the chemistry. An example of this is where XPS has successfully detected and quantified silicon on a surface which is not responding well to bonding with an adhesive, but the chemical form that the silicon is in is not readily apparent, i.e., it could be silica, silicate or silicone. Analysis of the same surface by static SIMS enables the mass spectrum of the sputtered top layer fragments to be determined and the presence of m/e ions at 43, 73 and 147 confirm that a polydimethyl siloxane is present.

12 Failure Diagnosis It is an unfortunate fact that plastic products fail in service. One of the major reasons for this is an incorrect

36

formulation of the product initially, which is a technological failing, the other is where the formulation is correct for the application, but where there has been a problem in the mixing/processing side, leading to a product that does not meet the specification. Analysing the plastic component can be useful in failure diagnosis.

12.1 Common Compositional Problems If it is suspected that the composition of the product is not correct, for example that the antioxidant or correct cure system has not been incorporated into the compound, then the appropriate species specific tests that have been discussed earlier can be carried out. If possible, it is advisable to conduct the analysis alongside that of a sample known to be of the correct composition. This ensures that no product specific matrix effects/interference reactions affect the data obtained and hence the conclusions reached. A surprisingly large number of failure problems can be solved by carrying out a simple series of tests including a polymer identification check by IR, a bulk compositional analysis by TGA and a molecular weight determination. Molecular weight determination is very important in the case of plastics because of the wide use (sometimes unauthorised) of regrind material. Unfortunately, the quality of regrind plastic can vary greatly due to the degradation, and hence reduction in molecular weight and associated physical properties, that a plastic undergoes when it is reground. This depends greatly on the conditions (e.g., heat and time of heating) that it is subjected to during the regrinding process. Also, if a material already contains a proportion of reground material the onset of degradation can be accelerated by structural anomalies already present in the polymer. The widespread applicability of GPC to determine the molecular weight distribution of the majority of common plastics makes it the perfect technique to investigate if regrind is in a sample. Although small amounts (e.g., 5%) of reasonably high quality regrind can be hard to spot, any significant amount will reveal itself by a shift in the distribution towards the low molecular weight end. As usual with GPC, the availability of reference samples is important as the technique is mainly comparative. Most of the failures that are associated with the use of either some or too much regrind are related to a reduction in the strength properties of the plastic, but another reasonably common type of failure is odour, especially in packaging applications. This odour is invariably due to oxygenated degradation products of the plastic and can be detected and analysed by headspace GC-MS.

Analysis of Plastics

12.2 Environmental Stress Cracking Environmental stress cracking (ESC) is the premature initiation of cracking and embrittlement of a plastic due to the simultaneous action of stress and strain and contact with specific fluids. It is estimated that 15% of all plastic component failures are due to ESC. The source of stress is often that which is unavoidably processed in during moulding and so an applied stress is not a pre-requisite. The fluid is sometimes that for which the component was designed to contain or conduct, but it is often supplied by such agencies as adhesives, paints, cleaning agents and inks. Because this type of failure is associated with relatively mobile (i.e., low molecular weight) liquids which are normally present in small concentrations the technique of GC-MS is very well suitable to its investigation. A particularly effective approach is dynamic headspace GC where any stress cracking fluid can be removed from the plastic matrix without the use of another solvent and long heating times enable it to be concentrated up to aid detection. An area of plastic that has not stress cracked can be used as a control. There are cases where stress cracking can occur due to the migration of a less volatile liquid (e.g., a plasticiser). An example of such a case is the stress cracking of ABS due to the migration of plasticiser from PVC, and this can be approached by the detection of phthalate in the ABS matrix by solvent extraction and then analysis of the extract using HPLC. Where the liquid is relatively non-volatile and complex in composition (such as silicone oil which causes cracking of polyethylene) again a solvent extraction technique has to be performed with either infrared microscopy analysis of a cast micro-film or a liquid chromatography method (i.e., LC-MS or HPLC) as the analysis technique. A review of the environmental stress cracking of plastics has been produced by Wright (315).

manufacturing stage (e.g., mixing, extruding or moulding). More often than not this contamination is in the form of solid, discreet entities which makes their removal from the product relatively easy. Once removed the microscopic techniques IR and Edax are excellent at obtaining assignment data in a cost effective way. Where enough of the contaminant is obtainable (e.g., 1 mg), and if a mixture of chemicals is suspected, a bulk composition by TGA can be obtained. If identification problems are still occurring, more sophisticated techniques such as GC-MS, SIMS and LIMA can be employed. Where the contamination is in a liquid form, a similar analytical regime can be used. A number of plastic products can suffer from solid inclusions, but it is probably most common in extruded products such as car door seals. It is also possible to use a Raman microscope system for the analysis of contaminants in plastic materials (293). One situation where the technique is particularly useful is in the identification of very small (e.g., a few micrometers in diameter) polymer gel inclusions within the same polymer matrix. Often these gels have a higher degree of crystallinity and Raman spectroscopy with its high spatial resolution and ability to differentiate between difference degrees of crystallinity is the ideal technique to differentiate between these and contamination by a foreign material. Contamination of plastics products by a species at a low level (i.e., less than 1% or at ppm levels) can sometimes be important, for example if a product is to be used in the pharmaceutical industry. If it is suspected that the contaminant is, or contains, a metal, then AAS can be employed. If the presence of an organic molecule is suspected, then headspace GC-MS can be used to identify and quantify the species. The high sensitivity of this technique normally makes the use of a control sample extremely important for a quick interpretation of the output, which is often complex.

12.4 Odour and Emissions Problems 12.3 Contamination Problems Plastic products can fail, both aesthetically and physically, because of contaminants. Chemical resistance and electrical failure are less likely causes of failure as this type of contaminant is not usually present at a high enough concentration.

The continuing drive to improve customer care and the high profile of health and safety issues, has led to pressure on the suppliers of plastics components to certain industries to minimise odours, and volatiles in general, from their products. This is particular true of the automotive industry.

Contamination can enter the product stream either in the ingredients used in the production, or during the

There are a number of specific tests that automotive companies insist that plastics components manufactured

37

Analysis of Plastics

by suppliers have to pass. An example of such a test is the VW emissions test which involves placing the component in a cell of given dimensions and heating the cell for a given time and a specified temperature. Rather than carry out a detailed analysis of the components liberated from the component, the result is expressed in terms of ppm of total organic compounds as determined by an organic vapour analyser (OVA). Limits are given as to the permissible concentrations. For quality control purposes it is the case at present that human smell panels will be used in preference to instrumental analytical techniques which do not yet adequately mimic the human response. There are practical drawbacks to this approach, leading to a lot of research going into ‘electronic noses’ utilising a number (e.g., 32) of sensors based on organic conducting polymers. These devices enable fingerprints of satisfactory products to be recorded which are used as references for quality checks. Work has been carried out to determine the additives which contribute the most to the overall odour of plastic products. One of the most useful techniques is headspace GC-MS. It is advisable to use the dynamic form of headspace sampling as this enables the volatiles from the sample to be concentrated. This benefit is important as some chemical species can cause an odour problem at very low levels due to the specific sensitivity of the human nose. For this type of work the dynamic headspace sampler (e.g., the Perkin Elmer ATD 400) is operated in a diffusion mode where the sample is heated at a relatively low temperature (e.g., 50 °C), which helps to ensure that additional volatile species are not generated due to degradation of the sample, for a relatively long period of time (e.g., in excess of 30 minutes). The odour species collected in the trap of the dynamic headspace sampler can then be analysed under the following conditions: Headspace trap injection temperature: 200 °C GC column type:

SGE RTX5 MS 30 m x 0.25 mm, 0.25 μm film

GC column temperature

–30 °C to 50 °C at 5 °C/ min and then 20 °C/min

(cryogenic cooling)

to 320 °C.

MS conditions

20 to 450 atomic mass units scanned every 0.33 s

38

13 Conclusion This review describes the analysis of plastics, plastic compounds and plastic products in as comprehensive a way as is possible within the format of a Rapra Review Report. The abstracts from the Rapra Polymer Library and the additional reading references provided should greatly assist the analyst who requires more information on recent developments. For the future, the reduction in cost of LC-MS systems will increase their accessibility and, in combination with GC-MS, will greatly improve the efficiency and accuracy with which the analysis of antidegradants, cure systems, plasticisers and other additives can be carried out. The combination of these two instruments will enable the full spectrum of polarity and molecular weight to be covered and enable a quantum leap in capability to be achievable by all analytical laboratories. Experiments which for years have had to be carried out by TLC because of the limitations of conventional HPLC instruments will now be carried out by LC-MS. The specific analysis techniques SIMS, XPS and LIMA are becoming increasing routine and, as a result, cost effective for consultants to use in characterisation and failure diagnosis work and therefore an expansion of their use is guaranteed. In the thermal analysis field, a number of developments have occurred in recent years, with modulated temperature forms of TGA, DSC and TMA being brought out by manufacturers. Modulating the temperature enables these techniques to deliver better, more informative data on samples. Another development within the thermal analysis group is the micro-thermal analysis (micro-TA) instrument. This technique combines the topographical mapping capabilities of a scanning probe microscope with the ability to perform localised thermal analysis (DTA and TMA) on a micron scale. The instrument is also capable of being connected to a GC-MS via a heated interface for the chemical identification of specific features. It is clear that, even with the development of new and more advanced techniques, the analysis of plastic compounds and products will continue to present the polymer analyst with complex and difficult challenges.

Analysis of Plastics

Additional References a.1

Surface Characterisation of Advanced Polymers, Eds., L. Sabbatini and P.G. Zambonin, Wiley-VCH, 1993.

a.2

G. Lawson and J. Sidwell, Plastics and Rubber International, 1983, 8, 6, 15.

a.3

J.L. Koenig, Spectroscopy of Polymers, Elsevier, 1999.

a.4

T.R Crompton, Manual of Plastics Analysis, Plenum, 1998.

a.5

T.R. Crompton, Practical Polymer Analysis, Plenum Press, 1993.

a.6

Polymer Spectroscopy, Ed., A.H. Fawcett, Wiley, 1996.

a.7

J. Haslam, H.A. Willis and D.C.M. Squirrell, Identification and Analysis of Plastics, 2nd Edition, Butterworth, 1972.

a.8

P.J. Wyatt, Analytica Chimica Acta, 1992, 272, 1.

a.9

D.O. Hummel, Atlas of Polymer and Plastics Analysis, Volume 2, Carl Hanser Verlag, 1984.

a.10

H.B.S Conacher and B.D. Page, Journal of Chromatographic Science, 1979, 17, 188.

a.11

P. Tittareli, T. Zerlia, A. Colli and G. Ferrari, Analytical Chemistry, 1983, 55, 220.

a.12

F. Lafferty and D.B. Stauffer, Wiley/NBS Registry of Mass Spectral Data, John Wiley & Sons, 1989.

a.13

J. Udris, Analyst, 1971, 96, 130.

a.14

A. Groagova and M.A. Pribyl, Analytical Chemistry, 1968, 234, 423.

a.15

F. Belpaire, Revue Belge des Matieres Plastiques, 1965, 6, 201.

a.16

D. Simpson and B.R. Currell, Analyst, 1971, 96, 515.

a.17

L.N. Mal’kova, A.I. Kalanin and E.M. Derepletchikova, Zhurnal Analiticheskoi Khimii, 1972, 27, 1924.

a.18

E. Schroeder and K. Thinius, Deutsche Farben Zeitschrift, 1960, 14, 146.

a.19

E. Schroeder and S. Malz, Deutsche Farben Zeitschrift, 1958, 5, 417.

a.20

Practical Surface Analysis, Eds., D. Briggs and M.P. Seah, John Wiley and Sons, 1988.

a.21

Handbook of X-Ray Photoelectron Spectroscopy, Ed., G.E. Muilenberg, Perkin Elmer Corporation, Eden Prarie, MN, 1979 (update 1992-95).

a.22

D. Brigg, A. Brown and J.C. Vickerman, A Library of Standard Static SIMS Spectra, Wiley, 1989.

39

Analysis of Plastics

40

Analysis of Plastics

Appendix 1 Solubility Parameters of Plastics, Plasticisers and Typical Solvents Solubility parameters of plastics Plastic Type

Solubility Parameter

PTFE

6.2

PCTFE

7.2

Polyethylene

8.0

Polypropylene

8.0

Poly t-butyl methacrylate

8.3

Poly n-hexyl methacrylate

8.6

Poly n-butyl methacrylate

8.7

Poly butyl acrylate

8.8

Poly ethyl methacrylate

9.0

Polystyrene

9.2

Poly methyl methacrylate

9.2

PVC

9.5

Bisphenol A polycarbonate

9.5

Polyvinylidene chloride

9.8-12.2

Ethyl cellulose

8.5-10.3

Cellulose di-nitrate

10.55

PET

10.7

Acetal polymers

11.1

Cellulose di-acetate

11.35

Nylon 6,6

13.6

Polymethyl α-cyanoacrylate

14.1

Polyacrylonitrile

14.1

Solubility parameters of plasticisers Plasticiser

Solubility Parameter

Paraffinic oils

7.5

Aromatic oils

8.0

Dioctyl adipate

8.7

Dioctyl sebacate

8.7

Didecyl phthalate

8.8

Di butyl sebacate

8.9

Dioctyl phthalate

8.9

Di 2-butoxyethyl phthalate

9.3

Dibutyl phthalate

9.4

Triphenyl phosphate

9.8

Tritolyl phosphate

9.8

Trixylyl phosphate

9.9

Dibenzyl ether

10.0

Dimethyl phthalate

10.5

41

Analysis of Plastics

Solubility parameters of solvents Solvent

Solubility Parameter

Neo-pentane

6.3

n-Hexane

6.6

Diethyl ether

7.4

Di-isopropyl ketone

8.0

Cycohexane

8.2

sec-Amyl acetate

8.3

Carbon tetrachloride

8.6

Piperidine

8.7

Xylene

8.8

Dimethyl ether

8.8

Toluene

8.9

1,2-Dichloropropane

9.0

THF

9.1

Ethyl acetate

9.1

Benzene

9.2

Chloroform

9.3

Methyl ethyl ketone (MEK)

9.3

Trichloroethylene

9.3

Tetrachloroethylene

9.4

Trichloroethane

9.6

Dichloromethane (DCM)

9.7

Cyclohexanone

9.7

Ethylene dichloride

9.8

N,N-Diethyl acetamide

9.9

Acetone

9.9

o-Dichlorobenzene

10.0

Carbon disulfide

10.0

N,N-Diethyl formamide

10.6

n-Butanol

11.4

Cycohexanol

11.4

Acetonitrile

11.9

N,N-Dimethylformamide

12.1

Acetic acid

12.6

Ethanol

12.7

Dimethylsulfoxide

12.9

Formic acid

13.5

Methanol

14.5

Phenol

14.5

Ethylene glycol

14.6

Glycerol

16.5

Water

23.4

42

Analysis of Plastics

Appendix 2 Specific Gravities of Plastics and Compound Ingredients Specific gravities of polymers Polymer

Specific Gravity

Low density polyethylene

0.92

High density polyethylene

0.96

Polypropylene

0.90

Polyvinyl chloride

1.41

PTFE

2.2

PCTFE

2.1

Polyvinylidene fluoride

1.5

Polyvinylidene chloride

1.7

Crystal polystyrene

1.05

Medium impact polystyrene

1.05

Very high impact polystyrene

1.02

SAN

1.06

Medium impact ABS

1.04-1.07

High impact ABS

1.01-1.04

MBS

1.07-1.10

Polybutylene terephthalate

1.31

Polyethylene terephthalate

1.37

General purpose phenolic resin

1.35

Melamine-phenolic resin

1.5-1.6

Urea-formaldehyde

1.5-1.6

Polysulfone

1.24

Polycarbonate

1.2

Polyphenylene oxide

1.06

Acetal homopolymer

1.43

Acetal copolymer

1.41

Polyimide

1.42

Nylon 4,6

1.18

Nylon 6,6

1.14

Nylon 6

1.13

Nylon 6,10

1.09

Nylon 6,12

1.07

Nylon 11

1.04

Nylon 12

1.02

43

Analysis of Plastics

Specific gravities of plastic compounding ingredients Ingredient

Specific Gravity

Aluminium silicate

2.10

Antimony trioxide

5.40

Bitumen

1.04

Barium sulfate

4.30

Calcium silicate

2.10

Carbon black

1.80

Carnauba wax

0.99

Calcined china clay

2.50

China clay (kaolin)

2.60

Cotton fibre

1.05

Diethylene glycol

1.12

Graphite

2.04

Iron oxide

4.5-5.1

Lanolin

1.08

Calcium oxide (lime)

2.19

Litharge

9.30

Magnesium oxide

3.60

Magnesium carbonate

2.21

Mica

2.80

Mineral oil

0.91

Oleic acid

0.90

Paraffin oil

0.80

Paraffin wax

0.90

Rosin

1.07

Silica

1.95

Stearic acid

0.85

Sulfur

2.05

Talc (magnesium silicate)

2.80

Titanium dioxide (anatase)

3.90

Titanium dioxide (rutile)

4.20

Calcium carbonate

2.65

Zinc oxide

5.55

Zinc stearate

1.10

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Analysis of Plastics

Abbreviations and Acronyms AAS

atomic absorption spectroscopy

ABS

acrylonitrile-butadiene-styrene

amu

atomic mass units

APCI

atmospheric pressure chemical ionisation

API

atmospheric pressure ionisation

ATR

attenuated total reflectance

BS

British standard

DCM

dichloromethane

DMTA

dynamic mechanical thermal analysis

DOP

dioctyl phthalate

DSC

differential scanning calorimetry

Edax

energy dispersive analysis

EI

electron ionisation

ELS

evaporative light scattering

EPA

Environmental Protection Agency (US)

ESC

environmental stress cracking

ESI

electrospray ionisation

EVA

ethylene-vinyl acetate copolymer

FID

flame ionisation detector

FT

Fourier transform

FTIR

Fourier transform infrared spectroscopy

GC

gas chromatography

GC-MS

gas chromatography-mass spectrometry

GPC

gel permeation chromatography

HDPE

high density polyethylene

HIPS

high impact polystyrene

HPLC

high performance liquid chromatography

ICP

inductively coupled plasma

IR

infrared spectroscopy

ISO

International Standards Organisation

KE

kinetic energy

LALLS

low angle laser light scattering

LAMMS

laser microprobe mass spectroscopy

LC-MS

liquid chromatography-mass spectroscopy

LDPE

low density polyethylene

LIMA

laser induced mass analysis

LLDPE

linear low density polyethylene

MALLS

multi-angle laser light scattering

MBS

methylmethacrylate-butadiene-styrene

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Analysis of Plastics

MEK

methyl ethyl ketone

micro-TA

micro-thermal analysis

Mn

number average molecular weight

MSD

mass selective detector

Mw

weight average molecular weight

Mz

Z average molecular weight

NIH

National Institute of Health (US)

NIST

National Institute of Standards and Technology (US)

NMR

nuclear magnetic resonance

NPD

nitrogen/phosphorus detector

OVA

organic vapour analyser

PE

polyethylene

PET

polyethylene terephthalate

PMMA

polymethylmethacrylate

PP

polypropylene

PTFE

polytetrafluoroethylene

PVC

polyvinyl chloride

Rf

Rf value is defined as ‘the distance from the start line on the plate to the analyte spot after development, divided by the distance from the start line to the solvent front’ and is reasonably constant for a given TLC plate type and developing solvent

RI

refractive index

SAN

styrene-acrylonitrile copolymer

SEM

scanning electron microscope

SFC

supercritical-fluid chromatography

SIMS

secondary ion mass spectrometry

SML

specific migration limits

TAC

triallyl cyanurate

TAIC

triallyl isocyanurate

TEM

transmission electron microscopy

Tg

glass transition temperature

TGA

thermogravimetric analysis

THF

tetrahydrofuran

TLC

thin layer chromatography

Tm

melting temperature

TMA

thermomechanical analysis

UV

ultraviolet

VA

vinyl acetate

Vis

visible light

XPS

X-ray photoelectron spectroscopy

XRD

X-ray diffraction

XRF

X-ray fluorescence

46

References and Abstracts

Abstracts from the Polymer Library Database Item 1 Polymer Testing 21, No.5, 2002, p.591-5 SPECTROSCOPIC BEHAVIOUR OF POLYVINYL ALCOHOL FILMS WITH DIFFERENT MOLECULAR WEIGHTS Abd El-Kader K M; Orabi A S Suez Canal,University Details are given of the preparation of PVAL films by a casting technique. Optical absorption and transmission measurements were performed. The identification of molecular structures and assignments of energy bands were also studied using FTIR and NMR. Correlations between refractive index and molecular weight were investigated. 17 refs. EGYPT

Accession no.856878 Item 2 International Journal of Polymeric Materials 51, No.4, 2002, p.315-23 EFFECTS OF CURING TEMPERATURE ON POLY(ETHYLENE TEREPHTHALATE) Al-Raheil I A Mu’tah,University The effect of cure temperature over the range from 280 to 350C on PETP was investigated and changes in polymer structure analysed by various techniques, including DSC, TGA, scanning electron microscopy and hot-stage microscopy. Changes in the crystallisation behaviour of PETP at the different cure temperatures and the morphology of the PETP spherulites are discussed and melting data of the melt crystallised PETP at 215C are presented. 16 refs. JORDAN

Accession no.856733 Item 3 Journal of Applied Polymer Science 84, No.8, 23rd May 2002, p.1524-32 KINETIC STUDY OF HINDERED AMINE LIGHT STABILIZER UNDER NATURAL WEATHERING CONDITIONS Kaci M; Hebal G; Benhamida A; Boukerrou A; Djidjelli H; Sadoun T Bejaia,University The photografting kinetics of a hindered amine light stabiliser (HALS) containing a polymerisable double bond in low density polyethylene (LDPE) films was studied under natural weathering conditions. The HALS (PBH3, chemical structure shown) was added to the polymer at a concentration of 0.3 wt.%. The photografting kinetics

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were determined by spectroscopic measurement of the absorption band area of the stabiliser around 308 nm in the UV spectra and 1605 cm -1 in the FTIR spectra, corresponding to benzylidene malonate and benzylidene malonic groups respectively. Parallel measurements on the free PBH-3 content after chloroform extraction of the photostabiliser from the polymer matrix by UV and gas chromatography showed that in natural weathering grafting took place in the LDPE film after very short exposure times of 127 and 168 hours as indicated by UV and FTIR respectively. The curves for the photografting and the free HALS kinetics were similar. The photografting mechanism was thought to involve a quick photoreaction between the methylene double bond of the stabiliser and the polymer macroalkyl radicals, with consequent formation of polymer-bonded aminyl stabiliser derivatives. 24 refs. ALGERIA

Accession no.853710 Item 4 Polymer Bulletin 48, No.1, March 2002, p.43-51 PYROLYSIS OF GAMMA-IRRADIATED BISPHENOL-A POLYCARBONATE Navarro-Gonzalez R; Coll P; Aliev R CNRS; Mexico,Universidad Nacional Autonoma This work shows the application of quantitative pyrolysisgas chromatography coupled with infrared spectroscopy and electron impact mass spectrometry in the study of radiation-induced scission of bisphenol-A polycarbonate (PC). PC under vacuum was gamma-irradiated using a 60Co source in the dose range from 0.125 to 1.0 MGy. This was followed by flash pyrolysis under an inert atmosphere observed by GC-FTIR-MS. Pyrolysis of the irradiated PC gave different products depending on the dose. Yields of carbon dioxide and methane decreased with dose whereas those of phenol and 4-methylphenol increased. The yields of benzene and toluene were unaffected by irradiation. Analysis of the products in this study helped to infer two main pathways for the radiationinduced scission of PC that involve carbonate bond rupture or aliphatic-aromatic bond rupture. 30 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; MEXICO; WESTERN EUROPE

Accession no.853698 Item 5 Journal of Polymers and the Environment 8, No.4, Oct. 2000, p.167-74 SENSITIVE ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY METHOD FOR DETECTION OF POLYIMIDE DEGRADATION BY

47

References and Abstracts

MICROORGANISMS Gu J-G; Cheng S-P; Liu J; Gu J-D Shenyang,Agricultural University; Nanjing,University; Beijing,University of Aeronautics & Astronautics; Hong Kong,University An electrochemical impedance spectroscopy method was evaluated for monitoring the microbial degradation of polyimides for electronic packaging. A mixed culture of fungi isolated from degraded polyimides was used as the microbial inoculum and scanning electron microscopy was employed to examine fungi growing on the surface of the inoculated polyimides. The data from the microscopic analysis was utilised to further support the relationship between changes in the impedance spectra and microbial degradation of the polyimide. 30 refs. CHINA; HONG KONG

Accession no.853552 Item 6 PVC 2002: Towards a Sustainable Future. Proceedings of a conference held Brighton, 23rd-25th April 2002. London, IOM Communications Ltd., 2002. Paper 14, p.157-65, 21cm, 012 PLATE-OUT IN PVC EXTRUSION Gilbert M; Varshney N; Van Soom K; Schiller M Loughborough,University; Honeywell; Chemson (Institute of Materials) The results are reported of a study of plate-out in PVC extrusion carried out using several analytical techniques, including DSC, SEM-EDX, FTIR spectroscopy and laser ionisation mass spectrometry. A special die and calibrator unit developed to investigate plate-out are illustrated and the reproducibility of the method evaluated. The effects of water content and anti-plate-out additives, such as alumina and silica, on plate-out are discussed and mechanisms explaining the formation of plate-out are proposed. 11 refs. AUSTRIA; BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.852750 Item 7 PVC 2002: Towards a Sustainable Future. Proceedings of a conference held Brighton, 23rd-25th April 2002. London, IOM Communications Ltd., 2002. Paper 9, p.116-23, 21cm, 012 DETERMINING THE LEVEL OF GELATION BY ODSC ON PVC WINDOW PROFILES Klingenfuss H; Zahn A Sueddeutsches Kunststoff-Zentrum (Institute of Materials) The degree of gelation of PVC window profiles and of weld beads was investigated using oscillating differential calorimetry (ODSC). Tests carried out on a PVC dry blend revealed that this analytical technique was capable of determining the degree of gelation of very small samples

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and permitted the determination of gelation at every point of the profile and weld without the need for calibration samples. 7 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; UK; WESTERN EUROPE

Accession no.852745 Item 8 Polymer International 51, No.5, May 2002, p.379-85 STUDIES OF CURE KINETICS OF POLYISOIMIDE BY DIFFERENTIAL SCANNING CALORIMETRY IN THE SOLID STATE Kim Y J; Son G I; Kim J-H Sung Kyun Kwan,University Detailed kinetic studies of the thermal imidisation of polyisoimide by DSC are described. Both isothermal and dynamic methods were used to obtain kinetic parameters and a phenomenological rate equation for estimating the degree of imidisation as a function of time. 15 refs. KOREA

Accession no.851649 Item 9 Journal of Adhesion 76, No.1, 2001, p.55-74 EVALUATING CURE OF A PMDI-WOOD BONDLINE USING SPECTROSCOPIC, CALORIMETRIC AND MECHANICAL METHODS Harper D P; Wolcott M P; Rials T G Washington State,University; US,Dept.of Agriculture,Forest Service The cure of polymeric diphenylmethane diisocyanate(pMDI)/wood bondline in a controlled saturated steam environment was monitored using micro-dielectric analysis(micro-DEA). Saturated steam environments were produced between 110 and 140C. The degree of cure calculated from micro-DEA was a basis for further spectroscopic, calorimetric and mechanical evaluation. Interpretation of calorimetric and spectroscopic analysis revealed a high consumption of isocyanate early in cure. Mechanical strength, however, as revealed by lap shear tests, did not develop until late in cure. Low lap shear strengths and a plateau in conversion rates were detected for samples pressed at 110 and 120C. Several components of the analysis suggested that low temperature cure could result in crystal formation, leading to diffusion controlled cure. 24 refs. USA

Accession no.851472 Item 10 Journal of Advanced Materials 34, No.2, April 2002, p.33-7

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References and Abstracts

DEGREE OF CURE, HEAT OF REACTION AND VISCOSITY OF 8552 AND 977-3 HM EPOXY RESINS Ng S J; Boswell R; Claus S J; Arnold F; Vizzini A US,Naval Air Warfare Center; Maryland,University The heat of cure, degree of cure and viscosity of two epoxy resins (Hexcel 8552 and Cytec Fiberite 977-3 HM) were investigated using a modulated differential scanning calorimeter and a rheometric digital analyser. Mathematical models were developed to correlate the rate of the degree of cure and the viscosity with the degree of cure and used to predict the kinetic behaviour of the epoxy resins, which was then compared with that of Hercules 3501-6. A comparison was also made of cure models developed based on neat and prepreg forms of the viscosity data. 6 refs. USA

Accession no.850900 Item 11 Polymers & Polymer Composites 10, No.3, 2002, p.237-48 CURE BEHAVIOUR AND STRUCTURE OF DICYANATE-EPOXY NOVOLAC BLENDS Guo B; Fu W; Jia D; Qiu Q; Wang L South China,University of Technology The objectives of this work are to investigate the cure behaviour and structure of bisphenol A dicyanate-novolac epoxy blends. The cure characteristics were investigated by gel time determination and dynamic DSC. To disclose the structural differences between cured cyanate-novolac epoxy blends and more traditional cyanate-diglycidyl ether systems, FTIR investigations were performed on the two kinds of blends, and in situ FTIR was used to examine the Bauer mechanism. The effects of epoxy concentration in the blend on the cure kinetics was investigated using two blends with different molar ratios, and in situ FTIR. 33 refs. CHINA

Accession no.850546 Item 12 Macromolecular Chemistry & Physics 203, No.4, 15th March 2002, p.653-62 MISCIBILITY AND CRYSTALLIZATION BEHAVIOUR OF POLYETHYLENE TEREPHTHALATE/POLYVINYLIDENE FLUORIDE BLENDS Rahman M H; Nandi A K Indian Association for the Cultivation of Science The miscibility of PETP and PVDF was studied. The Tg, melting point, the crystallisation temperature and the crystallinity values of the blends of different compositions, prepared at different conditions were measured. The polymer-polymer interaction parameter

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was measured from equilibrium melting point depression data. 50 refs. INDIA

Accession no.850061 Item 13 Chichester, John Wiley & Sons, 1999, pp.xiv,409. 23cm. 911 MICROSTRUCTURAL CHARACTERISATION OF MATERIALS Brandon D; Kaplan W D Haifa,Technion Institute This unreferenced book describes the technical and theoretical aspects of a wide range of techniques for studying the microstructure of materials, including X-ray and electron diffraction; optical microscopy, including polarised optical microscopy and interference microscopy; transmission and scanning electron microscopy; X-ray microanalysis; electron energy loss spectroscopy; and surface analysis by photoelectron spectroscopy, Auger electron spectroscopy, and secondary ion mass spectrometry. The techniques are described from sample preparation through information acquisition to interpretation of results. A final chapter describes the derivation of quantitative structural data from the results of these techniques. Examples used in the book mainly involve highly ordered materials such as metals and inorganic crystalline materials, but many of the techniques used are applicable to polymers. Problems for the reader are included. ISRAEL

Accession no.849739 Item 14 Polimeros: Ciencia e Tecnologia 11, No.4, Oct./Dec.2001, p.213-21 Portuguese NEAR-INFRARED SPECTRA OF POLYSTYRENE, POLY(METHYL METHACRYLATE) AND POLYCARBONATE De Araujo S C; Kawano Y Sao Paulo,Instituto de Quimica The near-infrared (NIR) spectra of amorphous polymers PS, PMMA and polycarbonate (PC) are studied. The tentative assignment of the overtone and combination frequencies is made using the curve fitting calculations and the local mode theory. Anharmonicity correction and mechanical frequency are determined from a Birge-Sponer plot. A tentative assignment of stretch overtone frequency of CH2 and CH functional groups of PS; CH3 and CO functional groups of PMMA; and CH, CH3 and CO functional groups of PC is made. An anharmonicity correction of 57 and 58 cm-1 is obtained for CH2 and CH stretch modes of PS; 59 and 9 cm-1 for CH3 and CO stretch modes of PMMA; and 53, 59 and 10 cm-1 for CH, CH3 and CO stretch modes of PC, respectively. 21 refs. BRAZIL

Accession no.849333

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References and Abstracts

Item 15 Macromolecules 35, No.7, 26th March 2002, p.2667-75 THERMAL PROPERTIES OF CROSS-LINKED POLYISOPROPYLACRYLAMIDE, POLYMETHACRYLIC ACID, THEIR RANDOM COPOLYMERS, AND SEQUENTIAL INTERPENETRATING POLYMER NETWORKS Diez-Pena E; Quijada-Garrido I; Frutos P; BarralesRienda J M CSIC The thermal properties of polyisopropyl acrylamide, polymethacrylic acid, isopropyl acrylamide-methacrylic acid copolymers and their blends were investigated by DSC and TGA. The state of the water was studied on the basis of DSC traces of swollen samples. The Tg of the same series of materials was also measured. 64 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.849122 Item 16 Applied Spectroscopy 56, No.2, Feb.2002, p.187-91 RAMAN MICROSCOPY AND MAPPING AS A PROBE FOR PHOTODEGRADATION IN SURFACE RELIEF GRATINGS RECORDED ON LAYER-BY-LAYER FILMS OF CONGO RED/ POLYELECTROLYTE Constantino C J L; Aroco R F; He J A; Zucolotto Z; Li L; Olveira O N; Kumar J; Tripathy S K Windsor,University; Lowell,Massachusetts University

Item 17 Injection Molding 10, No.1, Jan. 2002, p.40-4 THE MATERIALS ANALYST: PART 50. THE CASE OF THE DISAPPEARING CONTAMINANT Sepe M Dickten & Masch Mfg. A report is presented on the diagnosis of the failure of a component made from a 33% glass-reinforced nylon 66 on the assembly line with the aid of DSC, thermal gravimetric analysis, which was utilised to determine filler content and type, X-ray fluorescence and IR spectroscopy. The analytical procedures employed indicated that failure of the component could be attributed to the presence of chlorine probably arising from contamination of the process by PVC. USA

Accession no.848744 Item 18 Journal of Polymer Science: Polymer Physics Edition 40, No.5, 1st March 2002, p.434-53 FREE VOLUME, GLASS TRANSITION, AND DEGREE OF BRANCHING IN METALLOCENEBASED PROPYLENE/ALPHA-OLEFIN COPOLYMERS: POSITRON LIFETIME, DENSITY, AND DIFFERENTIAL SCANNING CALORIMETRIC STUDIES Dlubek G; Bamford D; Rodriguez-Gonzalez A; Bornemann S; Stejny J; Schade B; Alam M A; Arnold M Bristol,University; ITA Institut fuer Innovative Technologien GmbH; Martin-Luther-Universitat Halle

Raman microscopy, mapping and surface-enhanced Raman scattering techniques are applied to investigate the degradation of Congo Red (CR) in a surface relief grating (SRG) recorded on electrostatically assembled layer-by-layer film of CR alternated with polydimethyl diallylammonium chloride (PDAC). Photoinduced degradation is suggested by a decrease in the Raman bands assigned to CR with a concomitant increase in the background signal. More degradation is observed in the valleys of the SRG, which correspond to the most illuminated areas. In a line mapping across the SRG, the Raman intensity of CR bands follows the modulation of the grating, which indicates that photodegradation of CR contributes at least partially to the SRG formation. Surface-enhanced resonance Raman scattering (SERRS) indicates that the phenyl ring groups are located at the film surface. Mapping of the Raman signal over many periods of SRG shows that, within the limits of detection, the chromophores appear to be oriented in much the same way throughout the film. They have no preferred orientation in the peaks and valleys of the SRG after the recording process is completed. 23 refs.

Results of the above studies are presented and are discussed with particular reference to Tg and degree of branching, local free volume and degree of branching, local free volume and Tg, specific volume and degree of branching, and number density of holes and degree of branching. 56 refs.

CANADA; USA

Positron annihilation spectroscopy (PAS) is a special nondestructive evaluation (NDE) technique for materials

Accession no.848921

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EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; UK; WESTERN EUROPE

Accession no.848572 Item 19 Polymer Preprints. Volume 42. Number 2. Fall 2001. Proceedings of a conference held Chicago, Il., 7th-11th April 2002. Washington, D.C., ACS,Div.of Polymer Chemistry, 2001, p.13-4 POSITRON ANNIHILATION SPECTROSCOPY AS A NOVEL SURFACE PROBE OF POLYMERS Jean Y C; Zhang R; Mallon P; Chen H; Huang C-M; Li Y; Zhang J; Huang Y Y; Sandreczki T C; Wu Y Missouri-Kansas City,University (ACS,Div.of Polymer Chemistry)

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References and Abstracts

characterisation, which uses the positron (anti-electron). Positron-electron annihilation gamma-rays reveal useful information about the electronic and defect properties of materials under study. The unique repulsive force between the positron and the ion cores of materials makes the positron ideal for probing defects at the atomic and molecular levels. In recent years, PAS was developed as a useful tool to probe the microscopic properties of polymeric materials. One of the great successes in this line of research is the direct determination of polymer free volume and hole properties at an atomic scale (0.2-2 nm). Most existing PAS studies emphasise the bulk of polymers in measuring positron annihilation lifetime. Recently, another method of positron annihilation radiation, Doppler broadening of energy spectra, coupled with a slow positron beam, has been developed to examine the defect profile near the surface. The results of experiments on the photodegradation of polymer-based coatings induced by 313 nm UV irradiation as studied by slow positron annihilation spectroscopy are reported and correlated with gloss measurements. The sub-nanometer defect S parameter is found to decrease with exposure time. Current results suggest that the slow positron technique is a sensitive tool for detecting degradation of polymers in a time much earlier than for any existing testing methods. It is particularly sensitive to the surface defect properties. Applications of PAS to systems of polymers and fillers appear to be interesting to investigate in the near future. 6 refs. USA

Accession no.847946 Item 20 Adhesives & Sealants Industry 9, No.1, Feb. 2002, p.38-40 ENHANCED DSC INSTRUMENTATION IMPROVES DESIGN AND CHARACTERIZATION OF ADHESIVES Cassel R B TA Instruments The use of differential scanning calorimetry (DSC) for the characterisation and development of adhesive products is discussed. The Q Series DSC with Advanced Tzero Technology from TA Instruments is described, with reference to the advantages it affords as a new and enhanced tool for improved design and characterisation of adhesives. The development incorporates a new measurement principle with an additional sensor that together provide compensation for intrinsic instrument distortion of the DSC signal. With distortion virtually eliminated, it is possible to measure specific-heat capacity directly in a single scan, and to achieve greater sensitivity and accuracy. Analysis time is also reduced, especially for modulated temperature differential scanning calorimetry. It’s use in curing analysis of a two-part epoxy, and of pressure-sensitive adhesives is demonstrated. 3 refs. USA

Accession no.847415

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Item 21 Macromolecules 35, No.5, 26th Feb. 2002, p.1797-804 LIQUID CHROMATOGRAPHY OF SYNTHETIC POLYMERS UNDER CRITICAL CONDITIONS. THE CASE OF SINGLE ELUENTS AND THE ROLE OF THETA CONDITIONS Macko T; Hunkeler D; Berek D Swiss Federal Institute of Technology; Slovak Academy of Sciences PMMA, polybutyl methacrylates and polystyrenes in various solvents were investigated with bare silica gel and silica C18 bonded phases. The effect of variations in eluent nature on polymer retention is discussed. Critical conditions were identified in some single eluents which are thermodynamically poor solvents for the polymers. 37 refs. SLOVAK REPUBLIC; SLOVAKIA; SWITZERLAND; WESTERN EUROPE

Accession no.847047 Item 22 Macromolecules 35, No.5, 26th Feb. 2002, p.1677-84 LOW-TEMPERATURE CRYSTALLIZATION OF ETHYLENE-RAN-PROPYLENE COPOLYMERS. CONFORMATIONAL REARRANGEMENT OF SEQUENCES DURING THE FORMATION OF THE AGGREGATES Bracco S; Comotti A; Simionutti R; Camurati I; Sozzani P Milan,University; Basell Spa Low-temperature crystallisation of ethylene-propylene copolymers was followed by DSC and solid-state NMR. The trans conformation fraction identifying the aggregates was detected for all temperatures independent of thermal history. 41 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.847031 Item 23 Macromolecular Materials and Engineering 286, No.7, 27th July 2001, p421-8 THERMOGRAVIMETRY OF THERMOPLASTIC POLYIMIDE POWDERS UNDER FOUR DIFFERENT ATMOSPHERES Xin-Gui Li; Mei-Rong Huang; He Bai; Yu-Liang Yang Tongji,University; Tianjin Customs Central Laboratory; Fudan,University The high resolution thermogravimetry technique uses a variable heating rate response to changes in the weight loss rate to both reduce test times and improve definition. The thermal degradation of a thermoplastic polyimide polymer in nitrogen, helium, argon and air was analysed using both conventional and high resolution

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References and Abstracts

thermogravimetric analysis techniques. It was concluded that the thermal degradation results varied with both atmosphere and test technique with the high resolution technique providing more precise data in the inert atmosphere tests but less resolution in air. Thermogravimetric analysis data for a number of polyimide polymers is tabulated. The thermoplastic polyimide polymer evaluated was more thermally stable than many other polyimides. Complete details of the test techniques are given with full discussion of the results. 40 refs. CHINA

Accession no.846773 Item 24 Journal of Applied Polymer Science 83, No.12, 2002, p.2522-7 CRYSTALLIZATION AND CROSSLINKING OF POLYAMIDE-1010 UNDER ELEVATED PRESSURE Jun Yang; Wenfei Dong; Yucheng Luan; Jingjiang Liu; Shue Liu; Xingguan Guo; Xudong Zhao; Wenhui Su Changchun,Institute of Applied Chemistry; Jilin,University This study looked at the structural changes to polyamide1010 (PA1010) when it was treated at 250 degC for 30 min at a pressure of 0.7-2.5 GPa. Crystals grew when the pressure was below 1.0 GPa or above 1.2 GPa. Crosslinking occurred in the pressure range 1.0-1.2 GPa. DSC and wide angle x-ray diffraction showed that PA1010 lost its crystallisation ability after treatment at pressures of 1.0-1.2 GPa. Crystallised PA1010 had a greater thermal stability than crosslinked PA1010 at 400 degC. 20 refs. CHINA

Accession no.846587 Item 25 Kautchuk und Gummi Kunststoffe 55, No.1-2, 2002, p.9-14 German ANALYSIS OF TECHNICAL POLYMER BLENDS WITH COUPLING OF LIQUID CHROMATOGRAPHY WITH FTIR SPECTROSCOPY Pasch H; Rode K; Kloninger C; Esser E Deutsches Kunststoff-Institut The coupling of liquid chromatography with FTIR spectroscopy provides a new and interesting method for the detailed analysis of complex polymer systems. The application of this hyphenated technique to the analysis of polymer blends shows that it is possible to identify the different blend components by their spectral characteristics. Components of different chemical compositions are determined selectively and their chemical structure is analysed through well-resolved FTIR spectra. For structure elucidation, all facilities of

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state-of-the-art FTIR spectroscopy can be used. From the chromatographic and spectroscopic data, contour diagrams are generated that present the molecular heterogeneity of the sample in the coordinates molar mass and chemical composition. 17 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.846265 Item 26 Polymer 43,No.6,2002,p.1835-47 THERMAL DEGRADATION OF PET AND ANALOGOUS POLYESTERS MEASURED BY THERMAL ANALYSIS-FOURIER TRANSFORM INFRARED SPECTROSCOPY Holland B J; Hay J N Birmingham,University The thermal degradation of two commercial PET samples and two laboratory prepared polyesters, poly(ethylene isophthalate) and poly(diethylene glycol terephthalate), was studied using thermogravimetry and thermal analysisFTIR. The commercial PET samples were copolymerised with diethylene glycol and isophthalic acid groups in different proportions, and their thermal stabilities were found to differ. Through a study of the thermal degradation of poly(diethylene glycol terephthalate) and poly(ethylene isophthalate), it was found that diethylene glycol and isophthalate units promoted thermal degradation through increased chain flexibility and more favourable bond angles, respectively. The thermal degradation of all the polyesters tested led to the formation of non-volatile residue. IR spectroscopic analysis indicated that the residue consisted almost exclusively of interconnected aromatic rings. 21 refs. EU; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE; WESTERN EUROPE-GENERAL

Accession no.846155 Item 27 Progress in Organic Coatings 43, No.4, Dec.2001, p.226-32 SIMPLE RAMAN TECHNIQUE TO MEASURE THE DEGREE OF CURE IN UV CURABLE COATINGS Nichols M E; Seubert C M; Weber W H; Gerlock J L Ford Research Laboratory The curing of four UV-curable clearcoats was studied by confocal Raman microscopy. The disappearance of the C:C line near 1636/cm provided the signature for the curing of the samples, but quantification of the degree of cure by standard peak fitting and baseline subtraction methods did not work well because of sample fluorescence, baseline shifts and overlapping peaks. A smoothed second-derivative processing approach overcame all of these difficulties and provided a simple,

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References and Abstracts

rapid and objective quantification procedure. Steep cure gradients through the thickness of the clearcoat, due to screening of the bottom of the clearcoat by both the UVA and photoinitiator, were observed. Cure gradients at the top of the clearcoat due to oxygen inhibition were also observed. The most complete cure throughout the film thickness was obtained with a mixture of standard and red-shifted photoinitiators. 9 refs. USA

Accession no.846135 Item 28 Polymer 43, No.5, 2002, p.1587-97 FULL COPOLYMER CHARACTERIZATION BY SEC-NMR COMBINED WITH SEC-MALDI Montaudo M S CNR Random copolymers with units of methyl methacrylate, butyl acrylate, styrene and maleic anhydride were studied by fractionating the copolymer by size exclusion chromatography(SEC), collecting 30 to 40 fractions and then recording both the NMR and MALDI spectra of the fractions. In a successive step, bivariate distribution of chain sizes and composition maps were derived from knowledge of the molar mass, weight and composition of the copolymer fractions. The compositional distribution was obtained by summation of the sections of the bivariate distribution which belonged to a narrow compositional range. A model for SEC fractionation of copolymers was developed which allowed prediction of the composition and D(x) of the SEC fraction, D(x) being the ratio between the number-average and the weight-average molar mass, with x being the fraction number. Off-line SEC-MALDI measurements were performed in order to measure D(x) experimentally for the random copolymers. 31 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.846119 Item 29 Polymer Testing 21, No.2, 2002, p.155-61 BISPHENOL A-BASED POLYCARBONATES: CHARACTERIZATION OF COMMERCIAL SAMPLES Delpech M C; Coutinho F M B; Habibe M E S Rio de Janeiro,Universidade Federal; Rio de Janeiro,Universidade Estadual; Polialden Petroquimica SA Samples of bisphenol A polycarbonate were characterised by DSC, TGA, FTIR spectroscopy, size exclusion chromatography(SEC), vapour pressure osmometry (VPO) and viscometry. The samples exhibited the same FTIR spectrum profile and almost the same values of Tg and initial temp. of degradation. Slight differences were, however, observed in differential TGA curves, which could be due to the presence of additives. The number-

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average molec.wts. of the samples, as received and purified, were determined by VPO in two different solvents, trichloromethane and THF. Viscometric average molec.wts. were obtained in trichloromethane at 25C. Five different equations were used to calculate intrinsic viscosities and viscometric constant values. Relative molec.wts. and polydispersities were determined by SEC, in THF at 35C and in trichlorobenzene at 135C. It was confirmed that the results obtained in the latter solvent were in better agreement with those obtained by the other techniques. 25 refs. BRAZIL

Accession no.845967 Item 30 Plastics Engineering 58, No.2, Feb. 2002, p.40/55 PLASTICS ANALYSIS - THE ENGINEERS RESOURCE FOR TROUBLESHOOTING PRODUCT AND PROCESS PROBLEMS AND FOR COMPETITIVE ANALYSIS Ezrin M Connecticut,University Methods for competitive analysis, troubleshooting process and product problems, plastics analysis, analysis of failed products and analysis of polymeric formulations are discussed. Procedures covered include FTIR spectroscopy, Raman spectroscopy, NMR spectroscopy, surface analysis by spectroscopy, gas chromatography/mass spectrometry, atomic force microscopy and techniques for analysing unidentified formulations. 47 refs. USA

Accession no.845139 Item 31 Journal of Applied Medical Polymers 5, No.2, Autumn 2001, p.77-9 NOVEL TECHNIQUE FOR THE DETECTION OF A HINDERED AMINE LIGHT STABILIZER, BASED ON SILICON TECHNOLOGY Narayan S; Lee R E; Hallberg D; Malatesta V Great Lakes Chemical Corp.; Great Lakes Chemical Italia Details are given of the development of a novel method to detect the presence of a hindered amine light stabiliser in PP, based on silicon technology. The method consisted of extracting the stabiliser from the PP matrix followed by detection and quantification using proton NMR. 3 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; USA; WESTERN EUROPE

Accession no.844622 Item 32 Adhasion Kleben & Dichten 45, No.12, 2001, p.34-8 German

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NON-DESTRUCTIVE NUCLEAR MAGNETIC RESONANCE CONTACT TECHNIQUE EXAMPLES AND POSSIBILITIES Hartwig A; Wolter B Fraunhofer-Institut fuer Ang.Materialforschung; Bundesministerium fuer Wirtschaft; DECHEMA On page 25 of the November 2001 issue of Adhaesion, Kleben & Dichten, the nuclear magnetic resonance contact technique was introduced as a new sort of method for non-destructive characterisation of polymers. This article uses examples from the area of epoxy resins and thick-layer bondings to give an impression of typical, potential applications for this new non-destructive testing method. 2 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.844288 Item 33 Applied Spectroscopy 55, No.12, Dec.2001, p.1729-32 FORENSIC ANALYSIS OF SINGLE FIBRES BY RAMAN SPECTROSCOPY Miller J V; Bartick E G Washington G.,University; US,FBI Microscopical analysis by FT-IR spectroscopy has been the preferred method for obtaining additional information on the polymeric composition of a fibre. It allows unequivocal determination of the generic class and frequently permits sub-classification. FT-IR analysis cannot be conducted while the fibre is mounted due to the strong absorption of IR radiation by glass. The fibre must be removed from the slide and rinsed to clean off the mounting medium before preparing the fibre. This increases sample preparation time and the chance for sample loss. Glass produces little response to Raman spectroscopy. Therefore, Raman analysis of fibres can be conducted while the fibre remains mounted on a glass slide under coverslips. The theoretical beam width of the laser is 0.8 mu m; thus, Raman will potentially permit measurement of microfibres used in some fabrics in the current market. The samples do not need to be thinned or flattened, as with IR, because the photons are scattered from the surface and not transmitted through the sample. The current literature contains limited reports and citations on the use of Raman microprobe spectroscopy for forensic analysis of fibres. It has previously been shown that it is possible to scan fibres while they are taped onto a glass slide. By the same sample preparation method, it has been demonstrated that it is possible to differentiate between several generic and sub-generic classes of fibres. It is illustrated that it is possible to scan through a glass coverslip and mounting medium to obtain polymeric identification of non-dyed fibres. 14 refs.

Item 34 Journal of Applied Polymer Science 83, No.5, 31st Jan.2002, p.956-66 SAFETY ASSESSMENT OF POLYMERIC ADDITIVES FOR FOOD PACKAGING: HYDROLYSIS OF POLYMERIC PLASTICISERS BY DIGESTIVE FLUIDS Hamdani M; Thil L; Gans G; Feigenbaum A E Institut National de la Recherche Agronomique; BASF AG The safety of polymeric plasticisers capable of migrating into food was assessed by an in vitro study of the hydrolysis of poly(1,2-propylene adipate) (PPA) by digestive fluid liquids. Freshly prepared simulated intestinal fluid solutions produced a high degree of hydrolysis. As indicated by high performance size exclusion chromatography, the bulk plasticiser disappeared completely, and low molecular weight oligomers were produced within 4 hours. Gas-phase chromatography indicated no significant conversion to free monomers after hydrolysis, and NMR tests showed that the cleavage selectivity occurred selectively at primary ester linkages. Silica gel fractionation of the hydrolysate gave six oligomeric fractions, which were recovered and analysed. Proton NMR was used to evaluate the absolute molecular weight of the plasticisers and the hydrolysis products. Under simulated gastric and saliva conditions the degree of hydrolysis was less than 2%. 3 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; GERMANY; WESTERN EUROPE

Accession no.842741 Item 35 Journal of Applied Polymer Science 81, No.7, 15th Aug.2001, p.1588-94 CHARACTERIZATION OF BRANCHED POLYMERS BY SIZE EXCLUSION CHROMATOGRAPHY COUPLED WITH MULTIANGLE LIGHT SCATTERING DETECTOR. I. SIZE EXCLUSION CHROMATOGRAPHY ELUTION BEHAVIOR OF BRANCHED POLYMERS Podzimek S; Vlcek T; Johann C Wyatt Technology Corp.; Pardubice,University; Wyatt Technology Deutschland GmbH The elution behaviour of randomly branched PS and starbranched poly(benzyl methacrylate) with different levels of branching was studied by size exclusion chromatography (SEC) coupled with a multiangle light scattering detector. The highly branched polymers showed abnormal SEC elution behaviour. After normal elution at small elution volumes, the molar mass and root mean square radius of the eluting molecules increased with increasing elution volume. Reasons for this were explored and discussed. SEC separation was compared with separation by thermal field flow fractionation. 8 refs.

USA

CZECH REPUBLIC; EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; USA; WESTERN EUROPE

Accession no.843701

Accession no.842695

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References and Abstracts

Item 36 Revista de Plasticos Modernos 81, No.538, April 2001, p.461-6 Spanish APPLICATION OF INFRARED SPECTROSCOPY AND THERMAL ANALYSIS IN MONITORING THE CURE OF THERMOSETTING RESINS USED IN THE AIRCRAFT INDUSTRY Sanchez-Blazquez A CASA The amine cure of Hexcel 8552 epoxy resin, for use as the matrix in carbon fibre-reinforced composites for application in aircraft construction, was monitored by near-infrared spectroscopy. This technique was validated by comparison of the results with those obtained by modulated DSC. 18 refs. HEXCEL COMPOSITES EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.842573 Item 37 Progress in Colloid & Polymer Science Vol.117, 2001, p.167-71 SURFACE CHARACTERISATION OF POLYLACTIDE/POLYGLYCOLIDE COPOLYMERS Kiss E; Lam C N C; Due T M; Vargha-Butler E I Budapest,Eotvos Lorand University; Toronto,University; Biophy Research The wettability and the surface composition of biodegradable polymers used as drug delivery particles are determined and compared. Films of polylactic acid, polyglycolic acid and their copolymers with four different lactide, glycolide ratios of 85/15, 75/25, 65/35 and 50; 50 are formed by solvent-casting on polar (silicone wafer glass and silica) substrates. Advancing and receding water contact angles are measured goniometrically and also by using the automated axisymmetric drop shape analysis method. Both the advancing and the receding water contact angles of the copolymers are higher than expected from the values obtained for the two homopolymers considering the increasing glycolide content of the copolymers. Surface analysis of the polyester films is performed by X-ray photoelectron spectroscopy at various take-off angles to get information on the depth distribution of the components. Surface enrichment of the nonpolar (lactide) component in the outermost layer of the copolymer films is detected. The wettability behaviour is in accordance with the surface composition, results suggesting a surface activity effect resulting in the orientation of the nonpolar segments of the copolymer chains towards the surface of the film and hence producing more hydrophobic character for the copolymer films than should be due to their bulk composition. 20 refs. Accession no.842190

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Item 38 Synthetic Metals 124, No.2-3, 22nd Oct.2001, p.407-14 STUDY OF THE SURFACE POTENTIAL AND PHOTOVOLTAGE OF CONDUCTING POLYMERS USING ELECTRIC FORCE MICROSCOPY Barisci J N; Stella R; Spinks G M; Wallace G G Wollongong,University The effect of the polymer composition, preparation method and nature of the substrate on the surface potential (SP) of conducting polymer films is investigated. Both the average value and the distribution of SP across the polymer surface are influenced by these factors. Polythiophenes, potentially useful for solar energy conversion, are used to examine the generation of lightinduced changes in SP. Results suggest the possibility of determining the local variations of the surface photovoltage and the photovoltaic properties of polymer films intended for use in photovoltaic devices. 16 refs. AUSTRALIA

Accession no.842093 Item 39 Polymer Degradation and Stability 75, No.1, 2002, p.185-91 STUDY ON METHANOLYTIC DEPOLYMERIZATION OF PET WITH SUPERCRITICAL METHANOL FOR CHEMICAL RECYCLING Yong Yang; Yijun Lu; Hongwei Xiang; Yuanyuan Xu; Yongwang Li Chinese Academy of Sciences Polyethylene terephthalate (PET) was subjected to methanolytic depolymerisation with supercritical methanol in a stirred stainless steel autoclave at temperatures of 523-543 deg.C, pressure 8.5-14.0 MPa, and a 3-8 methanol to PET weight ratio. The solid products obtained, consisting mainly of dimethyl terephthalate and small amounts of methyl-(2-hydroxyethyl) terephthalate, bis(hydroxyethyl) terephthalate, dimers, and oligomers, were analysed by high performance liquid chromatography (HPLC), and the liquid products, mainly ethylene glycol and methanol were analysed by gas chromatography (GC). The temperature, weight ratio of methanol to PET, and the reaction time had a very marked effect on dimethyl terephthalate yield and the degree of PET depolymerisation, but the effect of pressure was insignificant above the methanol critical point. The optimum PET depolymerisation conditions were: temperature 533-543 K, pressure 9.0-11.0 MPa, and a methanol to PET weight ratio of 6-8. The depolymerisation of several PET wastes from the Chinese market was studied under the optimum conditions. 28 refs. CHINA

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References and Abstracts

Item 40 Polymer Degradation and Stability 75, No.1, 2002, p.153-9 THE EFFECT OF ULTRAVIOLET STABILISERS ON THE PHOTODEGRADATION OF POLY(ETHYLENE TEREPHTHALATE) Fechine G J M; Rabello M S; Souto-Maior R M Pernambuco,Federal University; Paraiba,Universidad Federal The weathering behaviour of polyethylene terephthalate (PET) samples obtained by bi-axial tension in the laboratory over a period of up to about 1100 hours was studied. The mechanical properties of films obtained from the samples having different types of UV stabilisers, e.g. a triazine ultraviolet absorber (Tinivin 1577), carbon black, or a TiO2/BaSO4 mixture, were tested, and the films were examined by UV-VIS spectroscopy, titration, size exclusion chromatography, and FTIR. The results showed that the unstabilised films were easily degraded, resulting in considerable deterioration in mechanical properties and a molecular weight decrease. The triazine was the most effective stabiliser. 38 refs. BRAZIL

Accession no.841524 Item 41 Polymer Degradation and Stability 75,No.1, 2002, p.123-9 INITIAL STEPS AND EMBRITTLEMENT IN THE THERMAL OXIDATION OF STABILISED POLYPROPYLENE FILMS Fayolle B; Audouin L; Verdu J Ecole Nationale Superieure des Arts et Metiers Physicochemical and mechanical characterisation methods were used to study the oxidation of 100 micron stabilised polypropylene films at 130 deg.C in air. Stabiliser consumption (UV spectrophotometry) and molecular weight decrease (steric exclusion chromatography) could be observed during the induction period, when no carbonyl build-up could be detected by IR spectroscopy. These structural modifications had an effect on the fracture properties, as indicated by the essential work of fracture (EWF) method, whereas the ultimate tensile elongation showed no significant changes. The results show that the EWF method is useful for characterising the degradation induced embrittlement of initially ductile polymers. The experimental data reported suggest that the problem of the spatial heterogeneity of the oxidation process requires further discussion. 21 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.841521 Item 42 Biomaterials 23, No.6, March 2002, p.1439-46

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EFFECTS OF THE STERILISATION METHOD ON THE WEAR OF UHMWPE ACETABULAR CUPS TESTED IN A HIP JOINT SIMULATOR Affatato S; Bordini B; Fagnano C; Taddei P; Tinti A; Toni A Bologna,Istituti Ortopedici Rizzoli; Bologna,Universita Details are given of the effects of sterilisation methods on the wear and changes in physical properties of ultrahigh molecular weight PE acetabular cups. The crystallinity of the cups was evaluated by micro-Raman spectroscopy as a function of the inner surface position. The partial least square calibration was used to correlate the Raman spectra with the crystallinity of the polymer measured by DSC. 52 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.840964 Item 43 Polymer Preprints. Volume 41. Number 2. Conference proceedings. Washington, D.C., 20th-24th Aug.2000, p.1792-3 CHARACTERISATION OF PLANT FIBRES BY INFRA-RED SPECTROSCOPY Garside P; Wyeth P Southampton,University (ACS,Div.of Polymer Chemistry) The application of IR spectroscopy with respect to the characterisation of cellulosic (plant) fibres is demonstrated. The ability to characterise fibres is of importance to textile conservators, as this information aids in the determination of the age and origin of the artefact from which they are taken, and may influence the choice of treatment. The fibres under examination are taken largely from the bast group (flax, hemp, jute and ramie); in addition, sisal and cotton are compared. FT-IR microspectroscopy and ATR techniques are employed. To complement the conventional use of these methods, the inherent polarisation effects of the equipment are exploited to record polarised IR spectra. Jute, sisal and cotton are readily differentiated, but flax, hemp and ramie prove more difficult to distinguish. Peak ratio techniques are applied in the latter case. 2 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.840045 Item 44 Journal of Coatings Technology 73, No.923, Dec. 2001, p.43-50 ON THE USE OF THE ATOMIC FORCE MICROSCOPE TO MONITOR PHYSICAL DEGRADATION OF POLYMERIC COATING SURFACES VanLandingham M R; Nguyen T; Byrd W E; Martin J W US,National Inst.of Standards & Technology

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References and Abstracts

Changes in the surface properties of a model thermosetting acrylic melamine polymeric coating system similar to systems widely used as automotive clearcoats were followed using atomic force microscopy (AFM). The samples were exposed to a range of relative humidities, different temperatures and various UV wavelengths and a full factorial experimental design was utilised. A mechanism for the formation of pits in the surface of the coatings, as observed by AFM, was developed and the relationship between the chemical and physical degradation of the coatings discussed. 21 refs. USA

Accession no.839365 Item 45 Polymer Plastics Technology and Engineering 40, No.5, 2001, p.767-81 STABILISATION OF FREE RADICALS IN FILLED OLIGOESTER ACRYLATES Kadossov E B; Kovarski A L; Kasparov V V; Zapadinski B I; Tikhonov A P Russia,Academy of Science; Mendeleev University of Chemical Technology The results are reported of a study of the formation and decay of free radicals during the photocrosslinking of an oligocarbonate methacrylate filled with two types of silica differing in particle size or hydroxyapatite using ESR spectroscopy. The data are correlated with those obtained for molecular mobility using a spin probe and the kinetics of radical accumulation during photocrosslinking are discussed along with the kinetics of termination of radicals. 17 refs. RUSSIA

Accession no.839176 Item 46 Revista de Plasticos Modernos 81, No.537, March 2001, p.345-52 Spanish ANALYSIS OF SYNTHETIC POLYMERS BY CAPILLARY ELECTROPHORESIS Simo C; Barbas C; Cifuentes A Instituto de Fermentaciones Industriales; San PabloCEU,Universidad The principles of the various modes of capillary electrophoresis are examined, and applications of these techniques in the molecular weight characterisation of polymers are discussed. 40 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.839085 Item 47 Applied Spectroscopy 55, No.11, Nov. 2001, p.1514-22

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RAMAN SPECTROSCOPY DETERMINATION OF THE THERMOPLASTIC CONTENT WITHIN EPOXY RESIN-COPOLYETHERSULFONE BLENDS van Overbeke E; Devaux J; Legras R; Carter J T; McGrail P T; Carlier V Louvain,Universite Catholique; ICI Details are given of the possibility of using Raman spectroscopy to determine the local thermoplastic content within an epoxy resin/copolyethersulphone blend. The required calibration of the Raman data is presented. The applicability of the calibrations to blends containing chlorine-ended copolyethersulphone is discussed. Results obtained with small or large Raman confocal holes were also compared. 40 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.838755 Item 48 Polymer Degradation and Stability 74, No.2, 2001, p.321-6 XPS CHARACTERIZATION OF FRIEDELCRAFTS CROSS-LINKED POLYSTYRENE Jianqi Wang; Jianxin Du; Hongyang Yao; Wilkie C A Beijing,Institute of Technology; Marquette,University The combination of a difunctional alkylating agent, either hydroxymethylbenzyl chloride or alpha,alpha’dichloroxylene, with PS or high-impact PS together with a Friedel-Crafts catalyst, 2-ethylhexyldiphenylphosphate, and an amine for reaction with hydrogen chloride was studied by X-ray photoelectron spectroscopy. The results confirmed the theories proposed from previous investigations using TGA, i.e. crosslinking of the polymer occurred as the temp. was raised and the alcoholcontaining alkylating agent gave a greater amount of crosslinking than did the dichloro compound. 13 refs. CHINA; USA

Accession no.838285 Item 49 Macromolecular Chemistry & Physics 202, No.16, 7th Nov. 2001, p.3228-33 CHARACTERIZATION OF THE CROSSLINKING KINETICS OF A THIN POLYMERIC LAYER BY REAL-TIME DIELECTRIC RELAXATION SPECTROSCOPY Schonhals A; Fritz A; Pfeiffer K Berlin,University; Micro Resist Technology GmbH The crosslinking kinetics of a thin polymeric layer on a prepolymer of a phthalic acid diallyl ester was studied by real-time dielectric spectroscopy. Activation energies were estimated for the reaction using the temperature dependence of the time constant. The change of the relaxation rate of the dynamic Tg with the reaction time was obtained from dielectric loss data. 20 refs.

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EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.838158 Item 50 LCGC Europe 14, No.12, Suppl., Dec.2001, p.8/21 CONSIDERATIONS ON COLUMN SELECTION AND OPERATING CONDITIONS FOR LC-MS Sandra P; Vanhoenacker G; Lynen F; Li L; Schelfaut M Kortrijk,Research Institute for Chromatography; Ghent,University Mass spectrometry is slowly, but surely becoming the detection system of choice for liquid chromatography analysis in many areas. An overview is presented of column and mobile phase selection for LC-MS. Relatively simple guidelines are advanced to successfully optimise LC-MS for several applications. This article discusses the fundamentals of LC related to MS hyphenation, adapting LC to LC-MS methods, normal-phase liquid chromatography, supercritical fluid chromatography, reversed-phase liquid chromatography, size exclusion chromatography, ion-exchange chromatography, affinity chromatography and capillary electrophoresis. 25 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; WESTERN EUROPE

Accession no.837996 Item 51 Polymer 42, No.20, 2001, p.8461-7 STATES OF WATER IN DIFFERENT HYDROPHILIC POLYMERS - DSC AND FTIR STUDIES Ping Z H; Nguyen Q T; Chen S M; Zhou J Q; Ding Y D Fudan,University; Rouen,University Differential scanning calorimetry and Fourier transform infrared spectroscopy techniques were used to study the structure of water molecules in polyvinyl alcohol and polyethylene grafted acrylate hydrophilic polymers. Varying amounts of water were added to test samples and the samples conditioned to the sorption equilibrium state in sealed containers for 24 hours prior to evaluation. It was concluded that below a threshold water content, depending on the polymers physical and chemical structure, water molecules absorbed in hydrophilic polymer cannot form ice crystals in the polymer matrix. Above this threshold content, the water crystallises but below zero. It was also demonstrated that the absorbed water in hydrophilic polymers develops differing hydrogen bonds in the first and second hydration layers. It was concluded that the potential influence of these intermolecular interactions should therefore be taken into account whenever a polymer is used with a solvent. 25 refs. CHINA; EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

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Item 52 Polymer 42, No.20, 2001, p.8425-34 PHYSICAL AND MECHANICAL PROPERTIES OF POLYETHYLENE FOR PIPES IN RELATION TO MOLECULAR ARCHITECTURE. PART I. MICROSTRUCTURE AND CRYSTALLISATION KINETICS Hubert L; David L; Seguela R; Vigier G; Degoulet C; Germain Y Institute Nationale des Sciences Appliquees; Atofina Five high density polyethylene bimodal copolymers with varying molecular architectures designed for pipe applications were tested to evaluate the relationships between structure properties contributing towards improved end use properties. Crystallisation kinetics were studied in relation to molecular architecture using chromatography, density columns, differential scanning calorimetry, X-ray scattering, rising temperature elution fractionation and infrared spectroscopy. From the test results, it was concluded that the normal correlation between kinetics, molecular structure and molecular topology found with unimodal copolymers does not apply with bimodal copolymers as the crystal surface free energy was sensitive to topological changes resulting from architectural molecular changes. Complete details of the experimental procedures and test results are given with extensive discussion of the background theory and results. 60 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.837023 Item 53 LCGC Europe 14, No.9, Sept. 2001, p.564/9 INVESTIGATION OF A NOVEL SOL-GEL DERIVED STATIONARY PHASE FOR GAS CHROMATOGRAPHY Cervini R; Day G; Hibberd A; Sharp G; Froud A SGE International Pty Ltd.; SGE Europe Ltd. The effectiveness of using a novel, sol-gel material incorporating PEG or wax as a capillary column stationary phase is described. Chromatograms demonstrating inertness, partitioning capability and robustness for a range of applications are presented. 10 refs. AUSTRALIA; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.836916 Item 54 Polymer Engineering and Science 41, No.10, Oct.2001, p.1714-30 TEMPERATURE MODULATED DSC STUDIES OF MELTING AND RECRYSTALLIZATION IN POLY(OXY-1,4-PHENYLENEOXY-1,4-

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References and Abstracts

PHENYLENECARBONYL-1,4PHENYLENE)(PEEK) Kampert W G; Sauer B B DuPont Central Research & Development The thermal and crystal morphological properties of amorphous and melt-crystallised PEEK were investigated. Two different molec.wts. were studied by temp.modulated DSC(TMDSC) over a broad range of annealing times and temps. The lower molec.wt. PEEK under all crystallisation conditions was found to exhibit secondary crystal melting in the low endotherm region, followed by melting of primary crystals superimposed with a large recrystallisation contribution. Primary crystal melting broadly overlapped with melting of the recrystallised species and contributed to the broad highest endotherm. Recrystallisation contributions and the interpretation of TMDSC were partially confirmed by independent rapid heating rate m.p. determinations and variable heating rate DSC. The higher molec.wt. PEEK showed many similarities but generally had smaller levels of reorganisation above the annealing temp. under most higher temp. crystallisation conditions. TMDSC provided good resolution of recrystallisation and related events compared with standard DSC. The broad and substantial exothermic recrystallisation in amorphous samples was also examined, showing that recrystallisation continued through the final melting region. 42 refs. USA

Accession no.836355 Item 55 Macromolecular Symposia Vol.174, Aug.2001, p.413-34 STRATEGIES IN TWO-DIMENSIONAL LIQUID CHROMATOGRAPHIC SEPARATION OF COMPLEX POLYMER SYSTEMS Berek D Slovak,Academy of Sciences The separation of complex polymer systems by twodimensional liquid chromatography is discussed. Methods are reviewed in which the effect of polymer molec.wt. on polymer retention is suppressed. The resulting ‘one parameter separation systems’ can be on-line or off-line connected to another separation system such as size exclusion chromatography in order to provide more detailed characterisation of complex polymers. Selected procedures for the re-concentration of diluted polymer solutions are also considered. These could be used for increasing the concentration of sample(s) leaving the first dimension separation column. Some arrangements for controlled sample re-introduction into the second dimension separation column are outlined. 48 refs. (World Polymer Congress, IUPAC MACRO 2000, 38th Macromolecular IUPAC Symposium, Warsaw, Poland, July 2000) SLOVAK REPUBLIC; SLOVAKIA

Accession no.836231

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Item 56 Revista de Plasticos Modernos 81, No.536, Feb.2001, p.244-8 Spanish PERMEABILITY OF METHANOL, TOLUENE, FUELS AND OXYGENATED FUELS IN AN ETHYLENE-VINYL ALCOHOL COPOLYMER USED AS A BARRIER COMPONENT TO GASES, AROMAS AND HYDROCARBONS Lagaron J M; Powell A K Jaume I,Universitat; BP Chemicals Ltd. Measurements were made of the permeation rates of methanol, toluene, a 50/50 toluene/isooctane fuel (fuel C) and fuel C with 10% ethanol or 15% methanol through EVOH films. Large scale methanol and water induced plasticisation was suggested by large solvent uptakes and confirmed by the observation of considerable decreases in Tg. The permeability of fuel C increased significantly when methanol was present, while the high barrier properties of EVOH to hydrocarbons was maintained for fuel C containing ethanol. 9 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK; WESTERN EUROPE

Accession no.835449 Item 57 Revista de Plasticos Modernos 81, No.536, Feb.2001, p.236-43 Spanish ETHYLENE-VINYL ALCOHOL COPOLYMERS AND THEIR APPLICATIONS IN FOOD PACKAGING Cerrada M L Instituto de Ciencia y Tecnologia de Polimeros The gas barrier properties of ethylene-vinyl alcohol copolymers are examined as a function of ethylene and vinyl alcohol content, and their use in combination with other plastics in films, bottles and other containers for food packaging is discussed. Results are presented of a study of the crystal structure of three copolymers having different compositions. 11 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.835448 Item 58 Polymer Preprints. Volume 41. Number 2. Conference proceedings. Washington, D.C., 20th-24th Aug.2000, p.1423-4 MAPPING CHEMICALLY HETEROGENEOUS POLYMER SYSTEM USING CHEMICAL MODIFICATION AND ATOMIC FORCE MICROSCOPY Raghavan D; Gu X; VanLandingham M; Nguyen T Washington,Howard University; US,National Inst.of Standards & Technology

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References and Abstracts

(ACS,Div.of Polymer Chemistry) Interactions between a film and its external environment are strongly influenced by the surface chemistry and morphology of the film. Extensive research has been conducted to provide in-depth microstructural information of thin polymer films using analytical techniques such as small-angle X-ray scattering, X-ray photoelectron spectroscopy, neutron scattering and secondary ion-mass spec trometry. However, these techniques lack the lateral resolution to detect and map the heterogeneity in polymer films. With the advent of atomic force microscopy (AFM), it is possible to provide direct spatial mapping of surface topography and surface heterogeneity at nanometer resolution. A combination of tapping mode and force mode AFM techniques has been effective in mapping mechanically heterogeneous regions in multi-component polymer systems. Recent developments in chemically functionalised AFM tips have allowed mapping of chemically heterogeneous lithographically patterned surfaces by AFM at the molecular scale. This technique is known as chemical force microscopy. However, mapping chemical heterogeneity in a polymer system by chemical force microscopy pose difficulties because of chain length variation and irregular packing of chains at the probe surface. The objective is to chemically degrade one component of a model blend and then identify the degraded component by AFM. A model blend consisting of polyethylene acrylate (PEA) and PS is selected due to the difference in the hydrolysis characteristics of PEA and PS. Acid is selected as the aggressive chemical medium so as to accelerate the hydrolysis of one component in the model blend film. 9 refs. USA

Accession no.835296 Item 59 Polymer Preprints. Volume 41. Number 2. Conference proceedings. Washington, D.C., 20th-24th Aug.2000, p.1409-10 OVERVIEW OF STATE-OF-THE-ART SPM OF CRYSTALLINE POLYMERS Miles M J; Hobbs J K; McMaster T J; Baker A A; James P J; Blakely S T; Aissaoui M-N Bristol,University (ACS,Div.of Polymer Chemistry) Scanning probe microscopy is a family of a dozen or more microscopies essentially based on the concept and technology of the founding member, scanning tunnelling microscopy. The most appropriate and widely-used of these microscopies in the study of polymer systems is atomic force microscopy (AFM), which in many of its modes of operation is suitable for imaging relatively soft solids such as polymers and biological materials. In the simplest AFM modes of operation (contact and ‘tapping’), topographic images representing the surface of the polymer specimen can be obtained. At the lamellar crystal level, such images have generally confirmed morphology

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and crystalline structures deduced from transmission electron microscopy (TEM) or X-ray studies. However, the resolution of the AFM can go beyond that easily achievable with TEM imaging of polymers. At higher resolution, AFM has, in some cases, revealed unpredicted surface structures. 26 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.835289 Item 60 Polymer 43, No.1, 2002, p.159-70 QUANTIFYING SHORT CHAIN BRANCHING MICROSTRUCTURES IN ETHYLENE 1-OLEFIN COPOLYMERS USING SIZE EXCLUSION CHROMATOGRAPHY AND FOURIER TRANSFORM INFRARED SPECTROSCOPY (SEC-FTIR) Deslauriers P J; Rohlfing D C; Hsieh E T Chevron Phillips Chemical Co. Ethylene-1-olefin copolymers are used to demonstrate an SEC-FTIR method for the analysis of short chain branching distribution (SCBD) across the molecular weight distribution (MWD). The chromatograms were obtained using the root mean square absorbance in the 3000-2700 cm power -1 spectral range (with FTIR serving as a concentration detector). The spectra from individual time sections of the chromatogram were then analysed for comonomer branch levels using a chemometric method, and the error in the reported SCB content of each section was estimated. By using the appropriate training sets, chemometric models for giving SCB versus chemometric models were constructed for obtaining SCB versus MWD profiles of enough accuracy for detecting trends resulting from catalysis and process changes in lowand high-density polyethylene samples. The model was used for accurate quantification of branching levels in polyolefins within plus or minus 0.5/1000 total carbons (i.e. about 0.1 mol percentage) in samples having relatively low SCB levels, i.e. less than 10 SCB/total carbons and mixed branch types. 20 refs. USA

Accession no.835164 Item 61 Journal of Applied Polymer Science 82, No.7, 14th Nov.2001, p.1677-90 SURFACE MODIFICATION OF LOW DENSITY POLYETHYLENE (LDPE) FILM AND IMPROVEMENT OF ADHESION BETWEEN EVAPORATED COPPER METAL FILM AND LDPE Ju-Shik Kong; Dong-Jin Lee; Han-Do Kim Pusan,National University The effects of chromic acid treatment for periods of time between 1 and 60 minutes and oxygen plasma treatment

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References and Abstracts

for periods of time between 30 and 90 seconds on the surface of low density polyethylene films were examined by attenuated total reflectance fourier transform infrared spectroscopy, electron spectroscopy for chemical analysis (ESCA), scanning electron microscopy and water contact angle. The effect of chromic acid treatment on the tensile strength of the samples was evaluated and tensile strength reduced with increasing treatment time. Adhesion of copper film to the treated surface was evaluated by a scratch test. It was found that both surface roughness and number of polar groups on the surface increased with increasing treatment times of both chromic acid and oxygen plasma, resulting in lowered water contact angle. Blackening of a film sample occurred after 30 minutes treatment in chromic acid. Adhesion of copper film initially increased with increasing treatment times, but optimum adhesion properties consistent with tensile strength retention were established with 30 minutes chromic acid treatment followed by 30 seconds oxygen plasma treatment. 14 refs. KOREA

Accession no.834851 Item 62 Advanced Materials & Processes 159, No.10, Oct.2001, p.66-7 SURFACE ENGINEERING TECHNOLOGIES Sudarshan T S Materials Modification Inc. The 15th International Conference on Surface Modification Technologies will be held in November in Indianapolis. This article presents a few paper abstracts and lists the titles of the sessions. Papers include: structure and properties of HVOF sprayed amorphous polymer matrix nanocomposite coatings; field experience with advanced soft-metal surfaces on carbon steel bolting materials used in gall-prone gasketed joints that operate at elevated temperatures; characterisation of industrial coatings with atomic force microscopy; characterising aluminium pretreatments for structural adhesive bonding; the Air Force manufacturing technology laser peening initiative; and iron aluminide based coating deposited by high energy density processes. USA

Accession no.834668 Item 63 Journal of Applied Polymer Science 82, No.6, 7th Nov.2001, p.1382-90 PROPERTIES AND MORPHOLOGY OF POLY(ETHYLENE TEREPHTHALATE) AND HIGH-DENSITY POLYETHYLENE BLEND Guerrero C; Lozano T; Gonzalez V; Arroyo E Nuevo Leon,Universidad Autonoma Blends of polyethylene terephthalate (PET) and high density polyethylene (HDPE), widely used in the soft

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drinks industry, were studied with and without a compatibiliser. The compatibilising agent was a surlyn copolymer of ethylene and methacrylic acid partially neutralized with zinc, the olefinic segment of which is compatible with HDPE, whereas the carboxylic acid groups form hydrogen bonds with the PET carbonyl groups. Infrared spectroscopy, differential scanning calorimetry, scanning electron microscopy, and the mechanical properties were used to assess the effectiveness of the compatibiliser. 29 refs. MEXICO

Accession no.832040 Item 64 Polymer Degradation and Stability 73, No.3, 2001, p.467-70 CORRELATION BETWEEN THERMAL PROPERTIES AND CONFORMATIONAL CHANGES IN POLY(ETHYLENE TEREPHTHALATE)/POLY(ETHER IMIDE) BLENDS Ruvolo-Filho A; de Fatima Barros A Sao Carlos,Universidade Federal Virgin and recycled polyethylene terephthalate (PET) was blended with polyether-imide (PEI) in proportions between 0 and 50 percent PEI content and samples were examined by differential scanning calorimetry and Fourier transform infrared spectroscopy. All blends were completely miscible, as indicated by a single glass transition temperature which is dependent on blend composition. Crystallisation rates of PET were retarded strongly at 20 percent PEI content and above, but degree of crystallinity was easily determined from a linear correlation between a structural parameter measured spectroscopically and enthalpy of fusion. Trans conformer activation energy measurement confirmed the effects of PEI content on crystallisation of PET. 9 refs. BRAZIL

Accession no.831829 Item 65 Polymer Degradation and Stability 73, No.3, 2001, p.463-6 EFFECT OF INTERFACE MODIFICATION ON THE PHOTO-STABILITY OF PIGMENTED POLYETHYLENE FILMS Anna P; Bertalan G; Marosi G; Ravadits I; Maatoug M A Budapest,University of Technology & Economics Examination of the ageing characteristics of high density polyethylene films containing phthalocyanine green and titanium white and other pigments with those of lightly stabilised polymer film without pigments was carried out using tensile analysis, differential scanning calorimetry and ultraviolet spectroscopy. The early failure of the phthalocyanine pigmented sample, and subsequent UV

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spectroscopic examination showed that the cause was adsorption of stabilisers onto the pigment surface. Reactive surfactant coating of pigments was shown to considerably extend the film stability by reducing their adsorbency. 9 refs.

HIGH RESOLUTION SOLID-STATE CARBON 13 NMR STUDY OF AS-CURED AND IRRADIATED EPOXY RESINS Ngono-Ravache Y; Foray M-F; Bardet M Grenoble,University

EASTERN EUROPE; HUNGARY

Details are given of the effects of strong ionising radiations on the physico-chemical modifications of epoxy resins. The sensitivity of the epoxy resins to radiation was determined using carbon 13 NMR. 20 refs.

Accession no.831828 Item 66 Polymer Degradation and Stability 73, No.3, 2001, p.387-92 MECHANISM OF PHOTOSTABILIZATION OF PERFLUOROPOLYETHER COATINGS BY HINDERED AMINE STABILISERS Luda M P; Camino G; Laurenti E; Novelli S; Temtchenko T; Turri S Torino,Universita; Centro Ricerche Ausimont The mechanism of operation of hindered amine stabilisers (HAS) against photodegradation in perfluoro polyethers incorporated into a coating material of polyurethane has been studied by infrared spectroscopy, gas chromatography-mass spectrometry and electron spin resonance spectroscopy. Under curing conditions normally utilised for coil coating (280 degrees Centigrade for 1 minute in air), the HAS was found to increase the number of urea bridges in the polyurethane network, and reduce the amount of unreacted isocyanate, giving a structure which is more resistant to photooxidation. Byproducts of the high temperature cure process, caused by partial transformation of the HAS into -NH derivatives act as antioxidants. The unreacted HAS was found to slowly evaporate from the test film, but whilst present acted as a radical scavenger. 8 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.831816 Item 67 Plast’ 21 No.101, April 2001, p.77-9 Spanish INFRARED THERMOGRAPHY: THE COLOURS OF HEAT ASCAMM The use of IR thermography in the study of injection moulds and injection moulded plastics parts is discussed, and details are given of research and development projects being undertaken by ASCAMM of Spain using this technique. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.831329 Item 68 Polymers for Advanced Technologies 12, No.9, Sept, 2001, p.515-23

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EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.831124 Item 69 Applied Spectroscopy 55, No.8, Aug. 2001, p.984-91 RAMAN AND INFRARED MICROSPECTROSCOPIC MAPPING OF PLASMA-TREATED AND GRAFTED POLYMER SURFACES Keen I; Rintoul L; Fredericks P M Queensland,University of Technology A section of the surface of a predominantly PP substrate containing a small amount of PE copolymer and a small amount of blended EPM was characterised before and after plasma treatment and after graft copolymerisation with PS by means of Raman and ATR/IR mapping. The maps constructed indicated variations in crystallinity across the surface, the distribution of EPM and the distribution of hydroxy groups introduced onto the surface by plasma treatment. 24 refs. AUSTRALIA

Accession no.830453 Item 70 POLYMER PROCESSING ENGINEERING. 01. Proceedings of a conference held June 2001. London, IOM Communications Ltd., 2001, Paper 5, p.46-58, 012 AT-PROCESS RAMAN SPECTROMETRY OF POLYMER MELTS Dhamdhere M; Li J; Deshpande B; Patil P; Hansen M G Tennessee,University (Institute of Materials; Interdisciplinary Research Centre) In-line monitoring of EVA extrusion was carried out using in-line fibre optic Raman spectroscopy. Vinyl acetate content in the random copolymer and melt indices of various grades of the EVA were determined and vinyl acetate content in the samples correlated using linear least squares and PLS analysis. Hierarchical Cluster analysis was employed as a pattern recognition technique to follow the natural clustering tendencies of the EVA samples. 10 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; USA; WESTERN EUROPE

Accession no.830358

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References and Abstracts

Item 71 Polymer Testing 20, No.7, 2001, p.729-40 DIRECT SOLID SAMPLING METHODS FOR GAS CHROMATOGRAPHIC ANALYSIS OF POLYMER/ADDITIVE FORMULATIONS Bart J C J Messina,University The present ‘state of the art’ in direct solid sampling methods for gas chromatographic analysis of additives encapsulated in polymers is reviewed. Techniques considered are static and dynamic headspace methods, thermal desorption and solid phase microextraction. Applications for each method are discussed. 54 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.830211 Item 72 Antec 2001.Conference proceedings. Dallas, Texas, 6th-10th May, 2001, paper 620 DETERMINATION OF CONDENSABLE VOLATILES DURING POLYMER PROCESSING USING AN ANALYTICAL EXTRUDER Buzanowski W C; Gunderson J; Froelicher S Dow Chemical Co. (SPE) A method of collecting and analysing the volatiles created during extrusion is described, in which the extruder is part of the analytical instrumentation. A non-vented 19 mm (3/ 4 in) single screw extruder was fitted with a right angle 3.2 mm single strand die, which in turn carried a glass tube with a bulb near the die exit to allow for polymer swell, and a side arm for attachment of the sampling system. The polymer extruded into the glass tube, the less volatile materials condensing in the tube, and the more volatile materials being withdrawn by the side arm and trapped in a set of three impingers containing an appropriate chilled trapping solution. The volatiles from the glass tube were removed by rinsing and analysed by Fourier transform infrared spectroscopy and gas chromatography-mass spectrometry. The trapping solutions were analysed directly. The equipment was used to determine the influence of extrusion time on volatile emissions from polycarbonate, the influence of melt temperature on volatile loss from a polycarbonate/styrene-acrylonitrile copolymer blend, and the influence of additives on volatile loss from a glassfilled polymer. 6 refs. USA

Accession no.830052 Item 73 Journal of Applied Polymer Science 81, No.8, 22nd August 2001, p.1902-13 DYNAMIC MECHANICAL ANALYSIS STUDY OF THE CURING OF PHENOL-

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FORMALDEHYDE NOVOLAC RESINS Markovic S; Dunjic B; Zlatanic A; Djonlagic J Belgrade,University Using dynamic mechanical analysis the curing reactions of typical phenol-formaldehyde novolac resins were followed. The evolution of various rheological parameters was recorded for samples of the resins on cloth. A thirdorder phenomenological equation described the curing reaction. The influences of the structure, composition and physical treatment on the curing kinetics were evaluated. 20 refs. EASTERN EUROPE; YUGOSLAVIA

Accession no.829458 Item 74 Journal of Applied Polymer Science 81, No.11, 12th Sept.2001, p.2779-85 RIGID AMORPHOUS PHASE AND LOW TEMPERATURE MELTING ENDOTHERM OF POLY(ETHYLENE TEREPHTHALATE) STUDIED BY MODULATED DIFFERENTIAL SCANNING CALORIMETRY Song M Loughborough,University Three similar samples of polyethylene terephthalate (PET) prepared by isothermal cold crystallisation in the differential scanning calorimetry (DSC) cell (PET1), melt crystallisation at a steady cooling rate and annealing for various times in the DSC cell (PET2), and quenching from 300 degrees centigrade to -20 degrees over a period of 5 minutes (PET3) were used to study the glass transition effects in the rigid amorphous phase and the low temperature melting endotherm using modulated DSC. As annealing time increased in PET2 the increment of heat capacity (IHC) at annealing temperature increased and the IHC at the glass transition temperature decreased. It was deduced that the low temperature melting endotherm originated with transitions in the rigid amorphous fraction, and it was noted that the glasslike transition of this fraction occurred between glass transition and melting temperatures. 23 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.829381 Item 75 Journal of Applied Polymer Science 81, No.10, 6th Sept.2001, p.2387-98 COMPARISON OF THERMAL DEGRADATION CHARACTERISTICS OF POLY(ARYLENE SULFONE)S USING THERMOGRAVIMETRIC ANALYSIS/MASS SPECTROMETRY Li-Hsiang Perng Ta Hwa,Institute of Technology Thermogravimetric analysis with gas chromatography and mass spectrometry were used in the analysis of the thermal

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degradation of polyether sulphone (PES) and polysulphone (PSF). Evolution of sulphur dioxide and phenol from random chain scission in a one stage pyrolysis was observed in both cases with apparent initial thermal stability of the PES being lower than PSF, but fire retardation of PES was better due to reduction of the sulphone group by hydrogen radicals. More pyrolysis products were identified from the PSF than from the PES. Thermal stability of ether and sulphone groups appeared similar in PES but in PSF the sulphone groups proved the more stable. A simple kinetic model was developed which showed good agreement between theoretical and experimental pyrolysis curves for both polymers. 20 refs. TAIWAN

Accession no.829337 Item 76 Journal of Applied Polymer Science 81, No.12, 19th Sept.2001, p.3064-8 TEMPERATURE AND ATMOSPHERE INFLUENCES ON SMOKE COMPOSITION DURING THERMAL DEGRADATION OF POLY(ETHYLENE TEREPHTHALATE) Malgorzata Dzieciol; Jerzy Trzeszczynski Szczecin,Technical University The less volatile compounds formed during the thermal degradation of polyethylene terephthalate (PET) under different conditions at 200-700 deg.C in nitrogen and air atmospheres were studied. The compounds were trapped on a glass fibre filter and analysed by capillary gas chromatography using a mass spectrometer (GC-MS), and high performance liquid chromatography. The results were tabulated, and plots were drawn of the degradation temperatures in nitrogen and air atmospheres versus the weight changes of terephthalic acid and monovinyl terephthalate evolved from PET. The effects of the atmosphere and temperature on smoke emission and composition during PET thermal degradation were considered. 28 refs. EASTERN EUROPE; POLAND

Accession no.826911 Item 77 Macromolecules 34, No.15, 17th July 2001, p.5224-8 STUDIES OF MISCIBILITY BEHAVIOUR AND HYDROGEN BONDING IN BLENDS OF POLYVINYLPHENOL AND POLYVINYLPYRROLIDONE Kuo S W; Chang F C Taiwan,National Chiao Tung University Blends of polyvinyl phenol with polyvinyl pyrrolidone were prepared by solution casting from DMF solutions. DSC, FTIR, and NMR were used to investigate the hydrogen bonding and miscibility of the blend. The Tg of the blend was determined. 22 refs.

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CHINA

Accession no.825682 Item 78 Journal of Thermal Analysis and Calorimetry 64, No.2, 2001, p.549-55 CRYSTALLIZATION AND MELTING OF POLYCARBONATE STUDIED BY TEMPERATURE-MODULATED DSC (TMDSC) Schick C; Wurm A; Merzlyakov M; Minakov A; Marand H Rostock,University; Moscow,General Physics Institute; Virginia,Polytechnic Institute & State University TMDSC measurements conducted at reasonably high frequencies for bisphenol-A polycarbonate(PC, Lexan) allowed for the determination of base-line heat capacity. Vitrification and devitrification of the rigid amorphous fraction(RAF) could be directly observed. 0.01 Hz appeared to be a reasonably high frequency for PC. The RAF of PC was established during isothermal crystallisation. Devitrification of the RAF seemed to be related to the lowest endotherm. For PC, the melting of small crystals between the lamellae was expected to yield the lowest endotherm. 27 refs. GENERAL ELECTRIC CO. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; RUSSIA; USA; WESTERN EUROPE

Accession no.825045 Item 79 Shawbury, Rapra Technology Ltd., 2001, p.iv, 174, 25cm, 91T EASY IDENTIFICATION OF PLASTICS AND RUBBERS VERLAYE G A L; ROEGES N P G; DE MOOR MO KaHo Sint-Lieven This book presents an identification scheme developed over the last thirty years for thermoplastics, common thermosets, a few copolymers and elastomers. The techniques used are based on simple tests such as the behaviour of polymers in liquids and in a flame. The book also covers Infrared spectroscopy. Main headings are: Simple tests (melting, solubility, burning characteristics, odour recognition, dripping, flotation, halogen test, nitrogen- and sulphur-test); Recording an IR spectrum; Identification flow charts; Thermoplastics; Cellulose and starch; Thermosets; Elastomers. (15 Refs) BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.824868 Item 80 UTECH 2000. Proceedings of a conference held The Hague, Netherlands, 28th-30th March 2000. London, 2000, Other Rigid Foam Developments Session, Paper 1, pp.4, 012

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References and Abstracts

LONG-TERM ENERGY EFFICIENCY OF PUINSULATION FOR REFRIGERATION Seifert H; Biedermann A Elastogran GmbH (Crain Communications Ltd.; European Isocyanate Producers’ Association) The ageing behaviour of rigid PU foams was investigated using gas chromatographic quantitative evaluation of the cell gas composition in the foams. The change in thermal conductivity of the foams during ageing was also examined as was the dimensional stability of the foams under diffusion open conditions and the results obtained correlated with the K x A-values from refrigerator cabinets via the change in cell gas composition. The data obtained revealed that the ageing process of appliances could be simulated in a tenth of the time by measuring diffusion opened PU foams. 2 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; NETHERLANDS; WESTERN EUROPE

from different wood species was carried out. Studies were carried out on Pine (Pino Eliottis), eucaliptus (Eucaliptus Saligna) and marmelero (Ruprechia Laviflora), a softwood and two semi-hard woods, respectively. The particles were used untreated and chemically modified with maleic anhydride. For the characterisation of untreated and treated flours, thermogravimetric analysis and analytical techniques were utilised. Dispersion of the fibrous particles, in addition to maximum fibre concentration (accompanied by complete wetting of the wood fibres) was dependent on the treatment and on the wood species utilised. Bending and compression tests suggested some improvement in the performance of the composites, if the wood flour was previously esterified. Changes in the fracture surfaces due to maleic anhydride treatment of the fibres were observed using scanning electron microscopy. 12 refs. ARGENTINA

Accession no.824162

Accession no.824859 Item 81 International Polymer Science and Technology 28, No.5, 2001, p.T/79-80 STUDY OF POLYMER-FILLER INTERACTION BY INVERSE GAS CHROMATOGRAPHY Gukasyan S Z The surface modification of fillers with polymeric substances is discussed with reference to improvement of the properties of filled polymers. When the fillers are modified with polymers, the boundary layer contains not only the matrix filler, but also the modifying polymer, and when the modifying polymer interacts with the surface filler, the properties of both the mineral component and the modifier are altered. One characteristic which reflects the result of polymer-filler interaction is the glass transition temperature of the modifier. To determine this parameter for a very low content of polymer, the method of inverse gas chromatography was used using the modified filler as the stationery phase. The study investigated the use of travertine and tuff, the surfaces of which were modified with latices of a copolymer of styrene and methacrylic acid. 3 refs. (Article translated from Plasticheskie Massy, No.8, 2000, p.36) RUSSIA

Accession no.824324 Item 82 Molecular Crystals & Liquid Crystals Vol.353, 2000, p.95-108 COMPOSITES MADE FROM LIGNOCELLULOSICS AND THERMOSET POLYMERS Aramguren M I; Marcovich N E; Reboredo M M INTEMA Preparation and testing of composites from a styrene/ unsaturated polyester thermoset matrix and wood flours

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Item 83 Polymer Degradation and Stability 73, No.2, 2001, p.251-7 THERMAL CHARACTERISTICS OF ADDITIONCURED PHENOLIC RESINS Reghunadhan C P; Bindu R L; Ninan K N Vikram Sarabhai Space Centre The thermal cure characteristics, kinetics of thermal degradation and pyrolysis of four different addition cured phenolic resins were investigated using various techniques, including DSC, DMA, FTIR spectroscopy, TGA and X-ray diffraction. Resins investigated were propargyl ether resins and phenyl azo-, phenyl ethynyland maleimide-functional resins. A comparison of the data obtained for all the phenolic resins was made as a function of molecular structure. 12 refs. INDIA

Accession no.824043 Item 84 UTECH 2000. Proceedings of a conference held The Hague, Netherlands, 28th-30th March 2000. London, 2000, Innovations: Flexible Foam Developments Session, Paper 5, pp.4, 012 VOC DETECTION IN POLYURETHANE FLEXIBLE FOAMS Occhiello E; Tavan M; Pannocchia P; Fava F EniChem (Crain Communications Ltd.; European Isocyanate Producers’ Association) The detection of volatile organic compounds in polyols and PU foams using SPME, gas chromatography and gas chromatography-mass spectroscopy is demonstrated. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; NETHERLANDS; WESTERN EUROPE

Accession no.823982

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Item 85 Polymer Degradation and Stability 73, No.1, 2001, p.163-7 THERMAL, PHYSICAL AND CHEMICAL STABILITY OF POROUS POLYSTYRENE-TYPE BEADS WITH DIFFERENT DEGREES OF CROSSLINKING Yanhong Li; Yunge Fan; Jianbiao Ma Nankai,University The thermal decomposition of porous polystyrene beads with differing crosslinking degrees using divinyl benzene were evaluated using thermogravimetry and differential scanning calorimetry techniques. The test results showed that the thermal stability of the beads increased with higher degrees of crosslinking. DSC analysis revealed that the glass transition temperatures gradually increased with crosslinking levels up to 30% crosslinking by weight, but above this level beads were thermally stable as the glass transition temperature was replaced by an exothermic peak. Complete details of the testing procedures and results are given 15 refs. CHINA

Accession no.823950 Item 86 Polymer Degradation and Stability 73, No.1, 2001, p.69-74 EXAMINATION OF A LOW DENSITY POLYETHYLENE (LDPE) FILM AFTER 15 YEARS OF SERVICE AS AN AIR AND WATER BARRIER Moller K; Gervert T; Holmstrom A Sweden,National Testing & Research Institute Comparisons between accelerated ageing tests and tests on polymeric materials aged in actual service conditions to identify possible degradation mechanisms appear to be the only reliable method of predicting long term service lifetimes. A low density polyethylene film used as an air and water barrier for 15 years in an exterior wall construction was characterised using tensile testing, spectroscopy and chromatography techniques. Although the mechanical properties of the film were unaffected by ageing, its antioxidant stabilisers were severely degraded. Full details of the ageing conditions, test methods and results are given. 16 refs. EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN EUROPE

Accession no.823940 Item 87 Polymer Degradation and Stability 73, No.1, 2001, p.47-67 VACUUM PYROLYSIS OF COMMINGLED PLASTICS CONTAINING PVC. PART II. PRODUCT ANALYSIS Miranda R; Pakdel H; Roy C; Vasile C

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Quebec,Universite Laval; Pyrovac Institute Inc.; Petru Poni,Institute of Macromolecular Chemistry Vacuum pyrolysis was performed on HDPE, LDPE, PP, PS and PVC materials individually, and also on a mixed plastics sample containing the five polymers. The main gaseous and liquid products, including chlorinated hydrocarbons, were identified by chromatography, and the yields and pyrolysis products were compared for the individual and mixed runs. The results suggested that the pyrolysis yields of the plastics mixtures were similar to those calculated from the pyrolysis of the individual polymers. However, the chlorine content was lower than expected indicating limited interaction during pyrolysis. Full details of the experimental procedures are given including a detailed tabulation of all the pyrolysis products. 54 refs. CANADA; EASTERN EUROPE; RUMANIA

Accession no.823939 Item 88 Polymer Degradation and Stability 73, No.1, 2001, p.15-22 THERMO-OXIDATIVE STABILITY OF PP WASTE FILMS STUDIED BY IMAGING CHEMILUMINESCENCE The spread of oxidation in artificially recycled PP materials, with and without stabilisation, was monitored using imaging chemiluminescence techniques. The results were compared with estimates made using Fourier transform infrared spectroscopy and differential scanning calorimetry techniques. It was concluded that although the conventional techniques gave residual lifetimes of five cycles, imaging chemiluminescence showed that a significant reduction in oxidative stability had occurred after only two cycles. Full details of the imaging chemiluminescence technique used are given with detailed results. 12 refs. Accession no.823934 Item 89 DEVELOPMENTS IN POLYMER ANALYSIS AND CHARACTERISATION Proceedings of a conference held Shawbury, UK, 10th May 1999. Shawbury, 1999, Paper 4, p.1-15, 012 CHEMICAL CHARACTERISATION OF POLYURETHANES Forrest M J Rapra Technology Ltd. (Rapra Technology Ltd.) Polyurethane chemistry is briefly outlined, additives generally used in polyurethanes are indicated and the analytical techniques used to characterise the structure, composition and properties of PUs and PU-based products are discussed in a comprehensive manner. Techniques covered include spectroscopic, chromatographic techniques and miscellaneous techniques, such as wet chemistry

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References and Abstracts

techniques. Sections are included dealing with the characterisation of polymer structure and starting materials, molecular weight determinations, characterisation of additives and cure reaction studies. 14 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.822952 Item 90 Macromolecular Symposia Vol. 169, May 2001, p.45-55 CHARACTERIZATION OF THE INTERACTIONS IN POLYMER/SILICA SYSTEMS BY INVERSE GAS CHROMATOGRAPHY Voelkel A; Milczewsk K; Jeczalik J Poznan,University of Technology The inverse gas chromatography technique, (IGC) is presented as a method of characterisation of the interactions in polymer-modified silica systems. The authors propose to express the magnitude of modified filler/polymer interactions by means of the Flory-Huggins parameter. Polyether-urethane/modified silica systems containing different amounts of filler were investigated, and information relating to the physicochemical properties of oligomer and modified silicas were presented by means of the solubility factor to describe the properties of the polymer layer, and the Flory-Huggins parameter which describes the polymer-solute or mixture polymer/silicasolute interactions. These parameters are obtained from inverse gas chromatography experiments. The influence of the IGC experiment temperature, the content of modified silica, and the nature of test solute on the evaluated parameters are presented and discussed. 7 refs. EASTERN EUROPE; POLAND

Accession no.822644 Item 91 Journal of Applied Polymer Science 80, No.8, 23rd May 2001, p.1305-11 EFFECT OF RECYCLED POLYPROPYLENE ON POLYPROPYLENE/HIGH DENSITY POLYETHYLENE BLENDS Bonelli C M C; Martins A F; Mano E B; Beatty C I Rio de Janeiro,Universidade Federal; Florida,University A study was made of the effects of addition of recycled polypropylene on the incompatible blends of virgin polypropylene with high-density polyethylene. The characteristics of the recycled polypropylene were determined by spectrographic and thermal analysis means. The mechanical properties of the blends were determined. The 50/50 blend of the two virgin polymers benefited most from the addition of the recycled polypropylene. 9 refs. BRAZIL; USA

Accession no.821546

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Item 92 Polymer Degradation and Stability 72, No.1, 2001, p.175-86 CHEMICAL AND MORPHOLOGICAL MODIFICATIONS OF IRRADIATED LINEAR LOW DENSITY POLYETHYLENE (LLDPE) Guadagno L; Naddeo C; Vittoria V; Camino G; Cagnani C Salerno,University; Turin,University; Montell Italia SpA Spherilene technology produced films of linear low density polyethylene which were exposed to UV irradiation to simulate accelerated weathering. Comparison was made with a set of films annealed at 60C and no irradiation. The resulting chemical structures were examined using FTIR. The findings were that the degradation is dominated by the formation of carbonyl and vinyl species. 22 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.820850 Item 93 Polymer Degradation and Stability 72, No.1, 2001, p.31-45 FACTORS AFFECTING THE ADSORPTION OF STABILISERS ON TO CARBON BLACK (FLOW MICRO-CALORIMETRY STUDIES). IV. SECONDARY ANTIOXIDANTS Pena J M; Allen N S; Edge M; Liauw C M; Valange B Manchester,Metropolitan University; Cabot Corp. Using flow micro-calorimetry, X-ray photoelectron spectroscopy and Fourier transform infra-red spectroscopy techniques the surface activity of different types of carbon black with secondary antioxidants (aryl phosphites and phosphonites) have been examined. Both in the overall adsorption activity and the levels of probe adsorption significant differences were observed. Two factors were reported which were found to influence the behaviour of phosphite stabilisers. 29 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.820835 Item 94 Polymer International 50, No.6, June 2001, p.635-42 DEGRADATION OF HIGH BARRIER ETHYLENE-VINYL ALCOHOL COPOLYMER UNDER MILD THERMAL-OXIDATIVE CONDITIONS STUDIED BY THERMAL ANALYSIS AND INFRARED SPECTROSCOPY Lagaron J M; Gimenez E; Suara J J Jaume I,Universitat The thermooxidative degradation of a solution cast ethylene-vinyl alcohol copolymer (containing 32

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mol.percent ethylene) used in barrier applications was studied at three temperatures immediately above the melting point using thermogravimetric analysis, DSC and FTIR spectroscopy. The weight loss measured by thermogravimetric analysis was fast at short times and slowed down progressively. The weight loss of about 3.6 percent measured by thermogravimetric analysis resulted from chemical alterations in the polymer. DSC showed small changes in crystallinity, melting point and glass transition and broadening of the melting endotherms in samples exposed to the more severe thermooxidative treatments. FTIR showed a transformation of the vinyl alcohol hydroxyl groups into carbonyl groups and the creation of double bonds. Changes in degradation kinetics, and possibly mechanisms, were thought to occur with increasing time. FTIR measurements indicated that transformation of the hydroxyl groups led to a weakening of the overall hydrogen bonding strength in the degraded samples so a reduction in the intermolecular cohesion, and hence the barrier properties of the copolymer, could be anticipated. 19 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.819207 Item 95 Polymer Science Series B 43, Nos. 3-4,March/April 2001, p.105-8 TRANSFORMATIONS OF ANTIMONYHALOGEN- AND NITROGEN-PHOSPHORUSBASED FLAME RETARDANTS IN POLYOLEFINS AND THEIR PERFORMANCE Bogdanova V V Belorussian,State University Degradation products from both antimony-halogen based and nitrogen-phosphorus based flame retardants were studied using X-ray diffraction and atomic emission analysis. Evidence of the retardation mechanisms in use against combustion was obtained for each system and in each case emission of volatile combustion inhibitors at the degradation temperature of the polymer matrix was the critical factor. 11 refs BELARUS; BELORUSSIA

Accession no.818458 Item 96 Polimery 45, Nos.11-12, 2000, p.51-8 Polish PYROLYSIS GAS CHROMATOGRAPHY AND NEW POSSIBILITIES OF ITS USE IN THE ANALYSIS OF POLYMERS Hetper J Major conditions are formulated to ensure that pyrolysis gas chromatography yields reliable and repeatable results, particularly when non-volatile substances such as

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polymers are analysed. The author’s own modification of PGC is presented, involving the use of a pyrolysis attachment with the mobile reaction zone. Resulting data are compared with those obtained by conventional pyrolysis gas chromatography. 34 refs. Accession no.816530 Item 97 New York, John Wiley & Sons, Inc., 1999, pp.xv,752 CHEMICAL SEPARATIONS- PRINCIPLES, TECHNIQUES, AND EXPERIMENTS MELOAN, C E KANSAS STATE UNIVERSITY This combination laboratory manual and reference source provides a working knowledge of an array of separation methods. In forty-two chapters, it explores all major categories of separation. With an emphasis upon everyday practice rather that theory, this book explains the principles and parameters of these methods and provides 59 specific experiments to demonstrate proper procedures. These experiments feature step-by-step protocols for each separation scheme, precise instructions on setting up the apparatus, and checklists for essential chemicals and supplies. Main Headings include Separations involving phase changes; Separations involving extraction; Separations involving chromatography; Separations involving ion exchange resins; Separations involving electric fields; Separations involving flotation; Separations involving membranes; Separations involving miscellaneous techniques. USA

Accession no.816497 Item 98 Polymer Bulletin 46, No.2-3, April 2001, p.191-6 MISCIBILITY OF POLYETHERIMIDE AND POLYBUTYLENE NAPHTHALATE BLENDS Lin C H; Wang C S Taiwan,Kung Shan Institute of Technology; Taiwan,National Cheng Kung University DSC, optical microscopy, and SEM were performed to characterise the miscibility of a blend of polybutylene naphthalate and polyetherimide. Data were compared with theoretical predictions. 6 refs. CHINA

Accession no.816205 Item 99 Journal of the National Institute of Materials and Chemical Research 8, No.4, 2000, p.149-59 Japanese POSITRONIUM FORMATION AND DIFFUSION IN POLYMERS

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References and Abstracts

Hirata K; Kobayashi Y

Kyoto,University

High-energy positrons injected into condensed matter quickly lose their energy, become thermalised and annihilate with one of the electrons of the medium into gamma rays. In polymers, some of the positrons form a hydrogen-like bound state between a positron and an electron prior to the annihilation. This bound state is called positronium (Ps). Ps is formed by recombination of a positron and one of the electrons released from the molecules in terminal positron spur. Positron-electron recombination in the positron spur competes with other reactions, so that the Ps formation probability depends on various factors. The influence of additives, polar groups and external field on Ps formation in polymers is discussed. A possibility of using Ps as a radiation chemical probe for polymers is described. Ps formed as a result of positron-electron recombination interacts with a subnanometer-size free volume hole, and diffuses over a certain distance before annihilation. The diffusion coefficient of Ps is determined using a chemical reaction between Ps and an additive, and its diffusion length in amorphous polymers is estimated to be ca.1 nm. This result is of fundamental importance to apply Ps as a probe for studying free volume in polymers. 68 refs.

Dynamic viscosity measurements were used to determine the physical ageing at 110C of polycarbonate using samples quenched from the molten state. The test results showed that there was a memory effect in the polycarbonate of the quenching processes, but as equilibrium is reached then the memory becomes lost. Evidence is shown that the structure of the polymeric chain in the glassy state relaxes over larger segment scale lengths because the scale of the movable segments is related to temperature. 29 refs.

JAPAN

Accession no.815833 Item 100 Journal of Applied Polymer Science 80, No.11, 13th June 2001, p.2120-2 SOLID-STATE NMR AND XPS STUDIES OF PVA/ SUGARCANE COMPOSITES Tavares M I B; Stael G C; Gorelova M M; de Menezes SMC Rio de Janeiro,Cidade Universitaria Bagasse, taken directly from the sugarcane mills, was dried, cut to lengths of 5 mm, and blended with poly(ethylene-co-vinyl acetate) in proportions up to 60 wt%. The composites were characterised by solid-state nuclear magnetic resonance spectroscopy and X-ray photoelectron spectroscopy. A homogeneous copolymer covering on the surface of the fibres was achieved, the samples exhibiting homogeneity at the molecular level. The best physical interaction between the fibres and the matrix was achieved with the sample containing 60 wt% fibre. 10 refs. BRAZIL

Accession no.814366 Item 101 Journal of Polymer Science: Polymer Physics Edition 39, No.3, 1st Feb.2001, p.337-41 PHYSICAL AGING OF POLYCARBONATE INVESTIGATED BY DYNAMIC VISCOELASTICITY Apaki O; Horie M; Masuda T

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JAPAN

Accession no.814126 Item 102 Polymer 42, No.13, 2001, p.5523-9 SEC-FTIR CHARACTERIZATION OF SEMICRYSTALLINE HDPE AND PP Verdumen-Noel L; Baldo L; Bremmers S DSM Research A pressure transducer in combination with the size exclusion chromatography-FTIR technique was used to characterise semi-crystalline materials such as HDPE and random PP copolymers. The comonomer content (butene for HDPE and ethylene for PP) decreased with increasing molar mass. For two HDPE samples produced by the dual reactor process, this decrease occurred stepwise with a constant comonomer amount on either side of the step. For all the HDPE samples, the amount of end unsaturations decreased with molar mass. The concentration of side and trans unsaturations was too low to be determined. 8 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; WESTERN EUROPE

Accession no.813974 Item 103 Macromolecular Materials and Engineering 286, No.3, 30th March 2001, p.161-7 MATRIX-ASSISTED LASER DESORPTION/ IONIZATION MASS SPECTROMETRY OF SYNTHETIC POLYMERS, 5A. ANALYSIS OF POLY(PROPYLENE OXIDE)S BY COUPLED LIQUID CHROMATOGRAPHY AT THE CRITICAL POINT OF ADSORPTION AND MALDI-TOF MASS SPECTROMETRY Keil C; Esser E; Pasch H Darmstadt,Deutsches Kunststoff-Institut Poly(propylene oxide)s were analysed efficiently by coupled liquid chromatography and MALDI-TOF mass spectrometry. The techniques were coupled via a robotic interface where the matrix was coaxially added to the eluate and spotted dropwise onto the MALDI target. Size exclusion chromatography and liquid chromatography at critical conditions of adsorption coupled to MALDI-TOF

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gave useful structural information on oligomer masses and chemical composition; The technique showed the presence of diols and monools in addition to the triols in poly(propylene oxide) triols. The oligomer distributions of all functionality fractions were determined. 23 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.813967 Item 104 Polimery 45, No.10, 2000, p.701-6 Polish OXIDATION AND DESORPTION OF OXYGEN FROM THE UPPER LAYER OF ACTIVATED POLYPROPYLENE FILM Zenkiewicz M Photoelectron spectroscopy was used to study oxidation of biaxially oriented polypropylene film. X-rays and ultrahigh vacuum associated with the method of study were found to promote oxygen desorption from the upper layer. 6 refs. Articles from this journal can be requested for translation by subscribers to the Rapra produced International Polymer Science and Technology. Accession no.813667 Item 105 Macromolecules 34, No.8, 10th April 2001, p.2667-72 SELF-FOCUSING IN GRADIENT LIQUID ADSORPTION CHROMATOGRAPHY OF POLYMERS Degoulet C; Perrinaud R; Ajdari A; Prost J; Benoit H; Bourrel M TotalFinaElf; Atofina; Elf Atochem North America Inc.; ESPCI; Institut Curie; Institut Charles Sadron The separation process occurring during liquid chromatography of polymers in a gradient of composition of the eluent was examined. The main feature was that, after a transient regime, the concentration profile tended to move as a front, i.e. without diffusive spreading in time. This results in relatively sharp peaks and the observation that long columns were useless. A simple analytical model was proposed for this self-focussing process that allowed optimal conditions of operation to be determined. This analysis was supported by experimental tests. 13 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; USA; WESTERN EUROPE

Accession no.813456 Item 106 Macromolecules 34, No.8, 10th April 2001, p.2395-7 NONDESTRUCTIVE MEASUREMENT OF A GLASS TRANSITION TEMPERATURE AT SPINCAST SEMICRYSTALLINE POLYMER SURFACES

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Hyun J; Aspnes D E; Cuomo J J North Carolina,State University A non-destructive technique for characterisation of the surface Tg in PETP is described which involves analysis of the variation of the ellipsometrically measured refractive index with temp., using the spectral dependence of the penetration depth of light to discriminate between surface and bulk transitions. The surface Tg is shown to be lower than that of the bulk for spin-cast semicrystalline PETP films because of density variation and Tg is found to be lowered further by plasma processing. 18 refs. USA

Accession no.813421 Item 107 Macromolecular Symposia Vol.165, March 2001, p.91-8 RECENT DEVELOPMENTS IN POLYOLEFIN CHARACTERISATION Pasch H Deutsches Kunststoff-Institut A brief review is presented on techniques for the analysis of polyolefins and additives in polyolefins. Techniques considered include high-temperature GPC combined with FTIR spectroscopy for the analysis of chemical composition as a function of molar mass, crystallisation fractionation for the analysis of short-chain branching in LLDPE and of polyolefin blends and pyrolysis-gas chromatography-mass spectrometry for the determination of additives, such as antioxidants, in polyolefins. 13 refs. (3rd Annual UNESCO School & IUPAC Conference on Macromolecules and Materials Science, Stellenbosch, South Africa, 2000) EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.813085 Item 108 Vinyltec 2000. Conference proceedings. Philadelphia, Pa., 11th-12th Oct.2000, p.198-202 USE OF ADVANCED ANALYTICAL METHODS TO ENHANCE THE PERFORMANCE OF VINYL MATERIALS Isner J D; Eiden R W Polymer Diagnostics Inc. (SPE,Vinyl Div.; SPE,Philadelphia Section) Analytical laboratories are asked to perform a variety of test methods in order to solve problems relating to the performance or otherwise of vinyl materials, and whilst there are many individual problems that need to be solved, they can be categorised, it is argued, by a relatively small number of questions. Five of these questions are addressed, and ways in which a laboratory may answer them are discussed. Suggestions are made for techniques that may be used for each question, and examples of problems are given. Recent advances in analytical

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References and Abstracts

techniques can be used to address topics such as lifetime prediction and failure analysis. Questions related to identification, commercialisation, competitiveness, failure and performance. USA

Accession no.811310 Item 109 Journal of Materials Science Letters 20, No.3, 1st Feb.2001, p.257-8 COMMENTS ON A NEW RAMAN PEAK IN A HIGH-DENSITY POLYETHYLENE Rodriguez A B; Young R J Navarra,Universidad Publica; Manchester,University; UMIST Raman spectroscopy yields information about the molecular structure of materials based on the observation of scattered light spectra, and has been used extensively in the investigations of polymer structure and composition: chemical structure and interactions, morphology, crystalline and amorphous structure, processing effects and orientation, etc. As an analytical technique, however, it is not free from artefacts, i.e. apparent experimental results that are not actually real but are due to the experimental methods or conditions. One factor that may be responsible for the presence of artefacts in Raman spectroscopy is external background light. There are numerous potential sources of external background light that lead to sharp spectral peaks. If they are not excluded from the collection optics of the Raman instrument, they can lead to noise, or artefacts, superimposed on the Raman spectrum from the sample. This background light can come from either the sample or from the environment around the sample. A study of the latter is reported. 14 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK; WESTERN EUROPE

Accession no.811165 Item 110 Journal of Applied Polymer Science 80, No.7, 16th May 2001, p.1071-84 PHASE BEHAVIOUR AND MOLECULAR MOBILITY IN POLYURETHANE/STYRENEACRYLONITRILE BLENDS Vatalis A S; Kanapitsas A; Delides C G; Viras K; Pissis P Kozani,Technological Education Institute; Athens,University; Athens,Kapodistrian University The molecular mobility and microphase separation in blends of crosslinked polyurethane (PUR) and styreneacrylonitrile (SAN) copolymer were investigated. The PUR and SAN copolymer were prepared by reactive blending with polymer polyols. DSC, thermally stimulated depolarisation currents (TSDC) techniques, dielectric relaxation spectroscopy (DRS) and dynamic mechanical thermal analysis over a wide range of

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temperatures and frequencies were used in the investigation. Results by each technique indicated that the degree of microphase separation of PUR into hardsegment (HS) microdomains and soft-segment (SS) microphase increases on addition of SAN. The various techniques used were initially compared with each other. Results showed that for the dynamic glass transition of the PUR SS microphase the characteristic time scales at the same temperature are similar for DSC, TSDC and DMTA and shorter for DRS. The PUR/SAN blends are classified as fragile systems. 40 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; WESTERN EUROPE

Accession no.810314 Item 111 Macromolecular Rapid Communications 22, No.2, 8th Feb.2001, p.51-67 EVANESCENT WAVE LIGHT SCATTERING. FUSION OF THE EVANESCENT WAVE AND LIGHT SCATTERING TECHNIQUES TO THE STUDY OF COLLOIDS AND POLYMERS NEAR THE INTERFACE Matsuoka H Kyoto,University The evanescent wave light scattering technique, which is produced by a fusion of the evanescent wave technique and light scattering technique, is a very powerful an useful tool for investigation of colloidal particles and polymers near the surface and interfaces. Two kinds of evanescent wave light scattering apparatuses are developed. One is the evanescent wave dynamic light scattering (EVDLS) technique and the other is the evanescent wave light scattering microscope (EVLSM). By EVDLS, the diffusion behaviour of a colloidal particle near the interface can be extracted quantitatively as a function of the distance from the interface. The diffusion coefficient is smaller than those for particles in bulk, reflecting electrostatic and hydrodynamic interactions. By EVLSM, the interaction potential profile between a colloidal particle and the surface in dispersion can be directly evaluated. EVLSM will play an import role in colloidal interaction studies, especially at a low ionic strength. It is also shown that a particle dynamics study is possible by the EVLSM technique. A new field will be developed in colloid science and polymer science by application of the evanescent wave light scattering technique, i.e. fusion of the evanescent light and a scattering techniques. 41 refs. JAPAN

Accession no.809623 Item 112 Journal of Applied Polymer Science 79, No.6, 7th Feb.2001, p.1101-12 ULTRASONICATION AND MICROWAVE ASSISTED EXTRACTION OF DEGRADATION PRODUCTS FROM DEGRADABLE

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POLYOLEFIN BLENDS AGED IN SOIL Contat-Rodrigo L; Haider N; Ribes-Greus A; Karlsson S Stockholm,Royal Institute of Technology; Valencia,Polytechnical University Degradation in soil of samples of a polyolefin blend treated with two different biodegradable additives (a starch/iron mixture and a commercial product (Mater-Bi AF05H)) was studied using two non-conventional extraction techniques. The period studied was from 0 to 21 months, and extracted products were analysed by gas chromatography mass spectroscopy. Molecular weight changes were monitored using high-temperature size exclusion chromatography. Extraction techniques were ultrasonication and microwave assisted extraction (MAE). Reproducibility of ultrasonification was found better with improved extraction of carboxylic acids and other products than MAE methods, but both were found faster than conventional (soxhlet) extraction techniques. Tables indicate the relative amounts of different extraction products and molecular weight changes in the polymer blend found over the 21-month period for both biodegradable additive types. 17 refs EUROPEAN COMMUNITY; EUROPEAN UNION; SCANDINAVIA; SPAIN; SWEDEN; WESTERN EUROPE

Accession no.808785

segments capable of establishing strong intermolecular hydrogen bonds. Characterisation was carried out using proton NMR, size exclusion chromatography, DSC, and dynamic mechanical analysis. The influence of the ratio of hard and soft segments on degree of crystallinity, Tg, melting point, tensile strength, elongation and Young’s modulus was examined. 24 refs. EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN EUROPE

Accession no.808057 Item 115 Journal of Applied Polymer Science 80, No.1, 4th April 2001, p.1-9 CROSSLINKING AND ITS EFFECTS ON POLYANILINE FILMS Tan H H; Neoh K G; Liu F T; Kocherginsky N; Kang E T Singapore,National University Polyaniline base films with varying degrees of crosslinking were cast from methylpyrrolidone solutions at different processing temperatures. The effects of crosslinking on solubility, morphology, tensile strength, doping characteristics and transport of ions across the films were investigated. Characterisation was undertaken using UV visible spectroscopy, atomic force microscopy, and elemental analysis. 18 refs. SINGAPORE

Item 113 Polimeros: Ciencia e Tecnologia 10, No.4, Oct./Dec.2000, p.202-8 Portuguese ETHYLENE COPOLYMERS ANALYSIS BY FRACTIONATION TECHNIQUES Escher F F N; Silva L P; Galland G B; Benetti A Rio Grande do Sul,Universidade Federal; Ipiranga Petroquimica SA Ethylene-butene copolymers were fractionated according to molecular size by direct extraction by different solvents and at different temperatures. Samples were also fractionated by differences in crystallinity using DSC. Fractions were characterised using carbon 13 NMR, FTIR, GPC and DSC. 9 refs. BRAZIL

Accession no.808128 Item 114 Journal of Polymer Science: Polymer Chemistry Edition 39, No.5, 1st March 2001, p.630-9 NEW SEGMENTED POLYESTER-URETHANES FROM RENEWABLE RESOURCES Liu Y; Lindblad M S; Ranucci E; Albertsson A-C Sweden,Royal Institute of Technology The physical and mechanical properties of aliphatic polyesters from propanediol and succinic acid were improved by their combination with aromatic urethane

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Accession no.807643 Item 116 Macromolecular Symposia Vol.162, Dec.2000, p.227-33 STUDY OF POLYMER COMPLEXES BY EXCLUSION CHROMATOGRAPHY COUPLED WITH LIGHT SCATTERING IN COMBINATION WITH FLUORESCENCE SPECTROSCOPY Mrkvickova L; Pokorna V; Pecka J Czech Republic,Academy of Sciences PMMA stereocomplexes prepared at different concentration in dilute tetrahydrofuran solutions are studied by size exclusion chromatography coupled with refractive and light scattering detectors in combination with fluorescence spectroscopy. A considerable increase in segment density due to complexation compared with free PMMA chain is only slightly affected by the polymer concentration in solution where stereocomplexes are formed. At polymer concentrations up to 3 x 10-3 g cm-3, an increase in non-uniformity of polymer complex molecular weight and size and a shift to higher values of both are observed. In semidilute solutions stereocomplexes virtually do not become heavier and larger. 6 refs. CZECH REPUBLIC

Accession no.806260 Item 117 Polymer 42, No.8, 2001, p.3859-66

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References and Abstracts

STRUCTURE FORMATION DURING THE ISOTHERMAL CRYSTALLISATION OF ORIENTED AMORPHOUS POLY(ETHYLENE TEREPHTHALATE) FILMS Radhakrishnan J; Kaito A Japan,National Institute of Materials & Chemical Research A study was made of structure formation during the isothermal crystallisation of oriented, amorphous PETP film from the glassy state using in situ FTIR spectroscopy, in situ wide-angle X-ray diffraction and small angle Xray scattering. The PETP films were prepared by rolling melt quenched films to a draw ratio of 2 and an evaluation made of the changes in the conformation and orientation order of the PETP chains during crystallisation along with the development of crystalline structure. Structure organisation before and during isothermal crystallisation is discussed and a comparison made of the crystallisation behaviour of oriented with that of isotropic PETP. 27 refs. JAPAN

Accession no.806185 Item 118 Antec 2000.Conference proceedings. Orlando, Fl., 7th-11th May, 2000, paper 678 USE OF CONTACT-ATOMIC FORCE MICROSCOPY IN PLASTIC MATERIAL SURFACES Reyes E; Guerrero C Nuevo Leon,Universidad Autonoma (SPE) Using thin films of isotactic polypropylene, poly(ethylene terephthalate) and polystyrene, the range of atomic force microscopy contact forces and the scanning frequencies required to obtain sharp and clear 3-D images of polymer surfaces was determined, by systematically varying these parameters, starting with typical values used for rigid surfaces. The optimum values were determined to be a contact force of 88-150 nN, and a scanning frequency of 1.0-1.5 Hz. 12 refs. MEXICO

Accession no.805686 Item 119 Journal of Applied Polymer Science 79, No.3, 18th Jan.2001, p.473-8 PYROLYSIS GAS CHROMATOGRAPHIC ANALYSIS OF POLYACRYLONITRILE Minagawa M; Onuma H; Ogita T; Uchida H Yamagata,University In the pyrolytic gas chromatographic analysis (PGCA) of acrylonitrile polymer under an inert atmosphere at 500-900 deg.C, lower nitriles, including methyl cyanide, HCN, and acrylonitrile were the main degradation products, but lower hydrocarbons, e.g. methane and ethylene, resulting from secondary decomposition, were also detected. Thermo-

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analytical data, including data on the relation between retention time and nitrile polarity, and the limiting yield on pyrolysis as a function of temperature were obtained. On the basis of these results, specific applications of PGCA and the usefulness of this method for studying the thermal degradation of acrylonitrile polymer are indicated. 20 refs. JAPAN

Accession no.804442 Item 120 West Conshohocken, Pa., 2000, pp.3. NALOAN ASTM D 3465-. TEST METHOD FOR PURITY OF MONOMERIC PLASTICISERS BY GAS CHROMATOGRAPHY American Society for Testing & Materials ASTM D 3465Version 2000. Photocopies and loans of this document are not available from Rapra. USA

Accession no.801052 Item 121 Polymer News 25, No.10, Oct.2000, p.359-60 ANALYSIS OF AIRCRAFT COATING BY SECONDARY ION MASS SPECTROSCOPY Usmani A M; Donley M UDC; Wright-Patterson Air Force Base An analysis was made of a flat aircraft coating using secondary ion mass spectroscopy, which revealed that the coating was a polyurethane C type based on isophorone diisocyanate, diethylene glycol and adipic acid. X-ray photoelectron spectroscopy was employed to determine pigments and extenders. 10 refs. USA

Accession no.800157 Item 122 Antec 2000.Conference proceedings. Orlando, Fl., 7th-11th May, 2000, paper 441 THERMODYNAMIC AND KINETIC ANALYSIS OF SEMICRYSTALLINE RECYCLATES BY DSC Cassel R B; Li L Perkin-Elmer Inc. (SPE) Developments in differential scanning calorimetry (DSC) for the characterisation of semicrystalline thermoplastics, including mixed recyclates are discussed. The techniques include stepwise DSC for the accurate determination of specific heat capacity, rapid determination of crystallinity using the Gray-Mathot total enthalpy technique, and analysis of crystallisation kinetics. The techniques show the influence of impurities on the glass transition temperature, crystallinity and crystallisation. 6 refs. USA

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Item 123 Antec 2000.Conference proceedings. Orlando, Fl., 7th-11th May, 2000, paper 439 NOVEL TECHNIQUE FOR THE DETECTION OF A HINDERED AMINE LIGHT STABILIZER (HALS), BASED ON SILICON TECHNOLOGY Narayan S; Lee R E; Hallberg D; Malatesta V Great Lakes Chemical Corp.; Great Lakes Chemical Italia (SPE) A technique for the determination of HALS in polypropylene was developed. The HALS, based on a polysiloxane backbone with tetramethyl piperidine side chains, was melt blended with the polypropylene which was then spun into fibres. The chopped fibres were dissolved in toluene, the polymer precipitated using methanol, and the filtrate dried. A solution of the filtrate was then prepared and analysed by proton nuclear magnetic resonance spectroscopy. The peak at 0.1 ppm was attributed to the methyl group on the silicon atom of the HALS, and was used for quantitative purposes. Polypropylene pellets were also prepared containing a lower concentration of HALS, which was subsequently subjected to direct extraction to prevent the loss which may occur during polymer reprecipitation. 3 refs.

PHASE SEPARATION IN MISCIBLE POLYMER BLENDS AS DETECTED BY MODULATED TEMPERATURE DIFFERENTIAL SCANNING CALORIMETRY Dreezen G; Groeninckx G; Swier S; Van Mele B Leuven,Catholic University; Brussels,Free University The phase separation of two partially miscible polymer blends was studied using modulated temp. DSC(MTDSC). The lower critical solution temp. demixing behaviour of PEO blended with polyether sulphone(PES) and with poly(3,4'-diphenylene ether isophthaloyl amide), as determined by cloud point temps. with optical microscopy, was in good agreement with results obtained from non-isothermal MTDSC measurements. The non-isothermal MTDSC apparent heat capacity evolution was time-dependent. It was influenced by the endothermic demixing enthalpy and, in the case of PEO/PES blends, by the vitrification of a high-Tg phase formed. Quasi-isothermal MTDSC measurements contained information on the kinetics of demixing and remixing, emphasising the added value of MTDSC to follow in situ the diffusion-controlled phase separation processes of partially miscible polymer blends. 32 refs.

USA

BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; WESTERN EUROPE

Accession no.799954

Accession no.798922

Item 124 Antec 2000.Conference proceedings. Orlando, Fl., 7th-11th May, 2000, paper 438 ANALYTICAL METHODOLOGIES EMPLOYED IN A COMPREHENSIVE FDA FOOD CONTACT COMPLIANCE INVESTIGATION: ANALYSIS FOR RESIDUAL MONOMERS, RESIN OLIGOMERS, ADDITIVES AND MODIFIERS IN SEVERAL FOOD SIMULATING SOLVENTS Eberhard J S; McCort-Tipton M M Covance Laboratories (SPE)

Item 126 Macromolecular Materials and Engineering Vol.283, Nov.2000 p.153-62 CHARACTERIZATION OF FLAME-SPRAYED PEEK COATINGS BY FTIR-ATR, DSC AND ACOUSTIC MICROSCOPY Simonin L; Liao H CREST; Belfort-Montbeliard,Universite de Technologie

The FDA considers that materials which come into contact with food, such as processing machinery and packaging, to be indirect food additives, and the potential migration of materials into the food requires determination. Ethanol/ water solutions and food oils are commonly used as food simulating solvents when determining migration. The subsequent determination of the migrating species (which may include residual monomers, oligomers, additives and modifiers) may be by liquid and gas chromatography, and mass spectroscopy. USA

Accession no.799953 Item 125 Polymer 42, No.4, 2001, p.1449-59

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Poly (aryl ether ether ketone) (PEEK) was utilised as a name-sprayed coating because of its good mechanical properties, low friction coefficient and high thermal stability. Fine polymeric powders were warmed up in oxyacetylene flame and sprayed onto a previously heated aluminium substrate. Investigation of the degree of crystallinity of PEEK coatings was carried out using differential scanning calorimetry (DSC), according to the rate of cooling after the spraying process. Structural modifications were revealed by FTIR-ATR, attributed to interactions between the flame and the polymeric powders. Ultrasonic methods were developed, especially acoustic microscopy, to study the variations of mechanical properties at the surface and the defects inside the material. In general terms, flame-sprayed coatings contain a large amount of porosity. Particularly suited to the observation of large defects (exceeding 50 microns) inside the polymeric materials is low-frequency microechography, a non-destructive technique. 19 refs. Accession no.798668

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References and Abstracts

Item 127 Polymer Preprints, Volume 40, Number 2, August 1999, Conference proceedings. New Orleans, La., August 1999, p.1043-4 MALDI/TOF/MS STUDY OF HOMOPOLYMERS AND AMPHIPHILIC DIBLOCK COPOLYMERS BASED ON SULPHONATED POLYSTYRENE Yang A; Nonidez W K; Mays J W Birmingham,University of Alabama (ACS,Div.of Polymer Chemistry) Matrix-assisted laser desorption ionisation time of flight mass spectroscopy (MALDI/TOF/MS) provides a new way to probe polymers; it can provide information on molecular weight, molecular weight distribution, mass of end groups and mass of repeating units. Further information, such as reactivity ratios, individual block chain length and its distribution, etc., can be obtained based on mass information. Polystyrene sulphonic acid and its sodium salt form have been successfully characterised by MALDI/TOF/MS, but no MALDI/TOF/ MS study of diblock copolymers containing a polystyrene sulphonic acid block appears to be evident. The results of such a study of amphiphilic diblock copolymers, NaPSS-b-PtBS, and their precursors, PSb-PtBS, are reported. Number-average and weight-average molecular weights (Mn and Mw), polydispersity indices and extents of sulphonation are obtained. 13 refs. USA

Accession no.798428 Item 128 Polymer Degradation and Stability 71, No.1, 2001, p.123-34 QUALITY-DETERMINATION OF RECYCLED PLASTIC PACKAGING WASTE BY IDENTIFICATION OF CONTAMINANTS BY GCMS AFTER MICROWAVE ASSISTED EXTRACTION (MAE) Camacho W; Karlsson S Sweden,Royal Institute of Technology The resulted are reported of an investigation into the quality of recycled HDPE and PP separated from mixed municipal solid waste carried out using gas chromatography-mass spectrometry. The development of a simple and rapid microwave assisted extraction method for the systematic analysis of low molec.wt. compounds, such as decomposition products and additives, in polymers is also reported and successfully applied to the analysis of contaminants in the above recycled plastics. 15 refs. EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN EUROPE

Accession no.796627 Item 129 Polymer Degradation and Stability 70, No.2, Nov.2000, p.269-75

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RAMAN SPECTRAL MAPPING OF PHOTOOXIDISED POLYPROPYLENE Blakey I; George G A Queensland,University of Technology The photooxidation of unstabilised, isotactic PP was investigated using Raman spectral mapping in combination with SEM/energy dispersive X-ray analysis, which permitted the determination of Ziegler-Natta catalyst residue distribution throughout the PP. It was found that oxidation was heterogeneous at a microscopic scale and that a high local concentration of catalyst residues resulted in the stabilisation of the polymer in the immediate vicinity and the formation of mobile reactive species, which initiated oxidation at sites away from the catalyst. 30 refs. AUSTRALIA

Accession no.795269 Item 130 Macromolecules 33, No.19, 19th Sept.2000, p.7088-92 SOLUTION CARBON-13 NMR CHARACTERIZATION OF NYLON 66: QUANTITATION OF CIS AMINE CONFORMERS, ACID AND AMINE GROUPS, AND CYCLIC UNIMERS Southern Mississippi,University Edited by: Davis R D; Steadman S J; Jatterr W L; Mathias L J Using a mixed 2,2,2-trifluoroethanol/deuteriochloroform solvent system, well-resolved solution carbon-13 NMR spectra of nylon-66 samples were obtained which showed several low intensity peaks which were not seen in more acidic solvents. The low intensity peaks were correlated with the methylene carbons near cis amide conformers, acid and amine end groups and within cyclic oligomers. The quantitative contents of these components for a typical nylon-66 sample were 1.1 mol% cis amide conformers, 1.0 mol% acid end groups and 0.5 mol% amine end groups. From end group concentrations, the number-average molecular weight of the nylon-66 was calculated to be 30 177 g/mol. The chemical shift values of methylene carbons in the end groups and in cyclic oligomers was pH sensitive and thus depended on the relative concentrations of acid and amine groups in each sample. 12 refs. USA

Accession no.794402 Item 131 Polymer Engineering and Science 40, No.11, Nov.2000, p.2442-55 EVALUATION OF THREE METHODS FOR THE MEASUREMENT OF CRYSTALLINITY OF PET RESINS, PREFORMS, AND BOTTLES Bashir Z; Al-Aloush I; Al-Raqibah I; Ibrahim M

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SABIC R & D

EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

The crystallinity of PETP resins, preforms and bottles was investigated using DSC, modulated DSC and density measurements. The PETP employed was a bottle-grade PETP copolymer containing 1.5% isophthalic acid. The accuracy, precision and validity of the techniques employed were evaluated and problems encountered in interpreting the results assessed. 47 refs.

Accession no.792350

SAUDI ARABIA

Accession no.793608 Item 132 Kautchuk und Gummi Kunststoffe 53, No.10, Oct.2000, p.574/81 German DIRECT ANALYSIS OF ADDITIVES IN POLYMERIC MATERIALS BY PYROLYSIS-GAS CHROMATOGRAPHY-MASS SPECTROMETRY Meyer-Dulheuer T; Pasch H; Geissler M Deutsches Kunststoff-Institut This article describes the direct analysis of additives by pyrolysis-gas chromatography-mass spectrometry. Using this method it is possible to identify additives quickly and reliably without separation of the polymer matrix. A small specimen of the sample is pyrolysed, i.e. degraded under inert gas atmosphere. The pyrolysis products are separated by gas chromatography and ionised in the mass spectrometer by electron-impact ionisation. By comparing the results with library data it is possible to identify unknown additives unambiguously and with high accuracy. 10 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.792613 Item 133 Journal of Thermal Analysis and Calorimetry 61, No.2, 2000, p.589-96 CALORIMETRIC ANALYSIS OF AN ISOTACTIC POLYPROPYLENE GAMMA-IRRADIATED IN VACUUM Spadaro G; Valenza A Palermo,University The molecular modifications induced in an isotactic PP gamma-irradiated in vacuum under a complete set of experimental conditions are studied by means of calorimetric analysis. The influence of the irradiation parameters, the total absorbed dose, D, and the dose rate, I, has previously been analysed and a simple kinetic model based on the rates of the main reactions occurring during irradiation, i.e. betascission, addition to double bonds and termination, was also discussed. It is shown how thermal analysis confirms the model forecasts and in particular the existence of the ‘inversion conditions’: below them the main effect is molecular degradation, while above them the main effects are chain-branching and crosslinking. 12 refs.

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Item 134 ICAC 99. Conference proceedings. Bristol, UK, 23rd-24th Sept.1999, p.133-43 IDENTIFICATION OF KEY CURE STAGES IN LIQUID MOULDING PROCESSES BY PARALLEL PLATE DIELECTRIC ANALYSIS McIlhagger A T; Matthews S T; Brown D; Hill B Ulster,University (IOM Communications Ltd.; Ulster,University; IMechE) The aerospace industry has recognised the major benefits associated with fibre reinforced composite materials. The more popular techniques available for composite production are the traditional wet lay-up or autoclave and resin transfer moulding (RTM). Efforts to further reduce processing time and improve part quality have focused on improved process control. To date this has been based on off-line techniques. The need for on-line cure monitoring is widely recognised and this will require the development of suitable in-mould sensors. The Engineering Composites Research Centre (ECKE) has investigated and concentrated on the specific problems encountered in the aerospace industry. Of the available cure monitoring methods, parallel plate dielectric analysis (DEA) appears to offer the greatest potential for determining the through-thickness cure state of the resin during cure. A laboratory dielectric instrument is utilised to simulate RTM and autoclave cure cycles for composite structures containing non-conductive and conductive fibres and for different resin systems used in the aerospace industry. Key resin cure stages are identified by an appropriate dielectric signal and correlated with data from other thermal and mechanical techniques. Insulated parallel plate dielectric sensors are being developed for use in the laboratory instrument with the potential for incorporation into composite production tooling. 26 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.790059 Item 135 Polymer Journal (Japan) 32, No.7, 2000, p.610-5 INFRARED SPECTROSCOPIC AND MODULATED DIFFERENTIAL SCANNING CALORIMETRY STUDY OF PHYSICAL AGING IN BISPHENOL A POLYCARBONATE Jin Lu; Yong Wang; Deyan Shen Academia Sinica FTIR spectroscopy was used to study the conformational changes in quenched bisphenol A polycarbonate films during physical ageing. The conformation changed gradually from the high energy trans-cis conformation to

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References and Abstracts

the low energy trans-trans conformation on sub-glass transition temperature annealing. In-situ FTIR studies on the conformational changes of films quenched from the rubbery and sub-glass transition temperature annealed for different times were carried out while increasing the temperature through the glass transition region. The results indicated that incremental changes in the population of trans-cis conformers in the quenched sample were gradual, whereas rather abrupt changes occurred in the sub-glass transition temperature annealed samples. The energy absorbed during the abrupt conformational change represented only part of the endothermic peak observed by modulated DSC. The authors concluded that some new cohesional entanglements may be formed during physical ageing. 28 refs. CHINA

Accession no.789734

Item 138 Polymers Paint Colour Journal 190, No.4432, Sept.2000, p.25-6 WATCHING PAINT DRY Middleton J The development of nuclear magnetic resonance imaging, a technique previously only used in medicine, to provide various information, including the drying rate, position of water and curing in waterborne coatings, is discussed. The principles of magnetic resonance imaging are outlined and work conducted at Surrey University in conjunction with Resonance Instruments to design equipment for coatings analysis is described. SURREY,UNIVERSITY; RESONANCE INSTRUMENTS EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.789465 Item 136 Polymer Journal (Japan) 32, No.7, 2000, p.560-6 CALORIMETRIC AND INFRARED SPECTROSCOPIC ANALYSIS OF MULTIPLE MELTING ENDOTHERMS OF POLY(ETHYLENE TEREPHTHALATE) Yong Wang; Jin Liu; Deyan Shen Chinese Academy of Sciences The multiple melting behaviour of PETP was studied using DSC, FTIR spectroscopy and temperature modulated DSC by examining PETP samples subjected to special schemes of crystallisation and annealing treatment at different temperatures. On one-step and twostep annealing, a series of multiple endothermic minor peaks was observed, resulting from the melting of imperfect crystals during crystallisation. Both dual morphology and melting-recrystallisation-remelting mechanisms were probably responsible for the observed multiple melting behaviour which was dependent on the thermal history of the PETP samples. 34 refs. CHINA

Accession no.789727 Item 137 Analytical Chemistry 72, No.19, 1st Oct.2000, p.4550-4 GPC SEPARATION OF POLYMER SAMPLES FOR MALDI ANALYSIS Hanton S D; Liu X M Air Products & Chemicals Inc.; Lab Connections Inc. MALDI mass spectrometry was combined with GPC analysis for broad polydispersity polymers with the use of liquid chromatography interface. Results for PMMA were compared with a blend of five narrow PMMA standards that mimic the broad dispersed material. 24 refs. USA

Accession no.789529

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Item 139 Journal of Applied Polymer Science 78, No.5, 31st Oct.2000 p.1009-16 CRYSTALLIZATION OF LOW-DENSITY POLYETHYLENE- AND LINEAR LOW-DENSITY POLYETHYLENE-RICH BLENDS Drummond K M; Hopewell J L; Shanks R A RMIT University Using differential scanning calorimetry (DSC) the crystallisation of a series of low-density polyethylene (LDPE)- and linear low-density polyethylene (LLDPE)rich blends was examined. After continuous slow cooling DSC analysis showed a broadening of the LLDPE melt peak and subsequent increase in the area of a second lower-temperature peak with increasing concentration of LDPE. Melt endotherms following stepwise crystallisation (thermal fractionation) detailed the effect of the addition of LDPE to LLDPE, showing a nonlinear broadening in the melting distribution of lamellae, across the temperature range 80-140 degrees Celsius, with increasing concentration of LDPE. A rise in the population of crystallites melting in the region between 110 and 120 degrees Celsius, a region was observed where as a pure component LDPE does not melt. A decrease in the crystallite population over the temperature range where LDPE exhibits its primary melting peaks (90-110 degrees Celsius) was noted, indicating that a proportion of the lamellae in this temperature range (attributed to either LDPE or LLDPE) were shifted to a higher melt temperature. 30 refs. Accession no.789066 Item 140 Polymer International 49, No.9, Sept.2000, p.1007-13 USING SPECTROSCOPY WITH CHEMOMETRICS TO MEASURE POLYMER

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MOLAR MASS Shenton M J; Herman H; Stevens G C Surrey,University The ability to determine the molar mass of a polymer is of fundamental importance to describe polymer molecular characteristics. Conventional methods for measuring molar mass include viscometry, osmometry, light scattering and analytical gel permeation chromatography. Although high quality data can be obtained by these methods, the results can be significantly affected by sample preparation, and they are often time consuming and unsuitable for real-time on-line processing. The potential of determining polymer molar mass using optical spectroscopy combined with chemometric analysis is demonstrated. This is technically attractive because optical spectroscopy is routinely used to collect process data on-line and some refineries routinely monitor and control blending using near-infrared spectroscopy. A comparable development to monitor polymer molar masses on-line from systems already being used to measure density and melt index, would be of potential value to many sectors of the polymer production and processing industry. Chemometrics is a multivariate methodology that allows the information from entire spectra to be used; it can be considered as a maximal compression technique. Extracted ‘factors’ can then be regressed against property data by using a wellcharacterised set of ‘training’ samples to produce predictive regression models. It is shown that simple spectroscopic methods, such as the Raman technique discussed, when coupled with chemometrics, are capable of providing molar mass and distribution information. This is illustrated with reference to polydimethylsiloxanes in the liquid phase. 18 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.787562 Item 141 Composite Interfaces 7, No.2, 2000, p.81-92 INVESTIGATING INTERPHASE DEVELOPMENT IN WOOD-POLYMER COMPOSITES BY INVERSE GAS CHROMATOGRAPHY Rials T G; Simonsen J USDA; Oregon,State University The influence of secondary interactions on the development of interfacial structure in composites of wood and amorphous thermoplastic polymers is not well understood. Inverse gas chromatography is used to investigate the effect of different polymers on the surface energy of partially or fully coated white pine wood meal. In this way, the development of the interphase is monitored as a function of polymer depth on the wood surface. The polymers are selected to provide a range of functional groups and include PS, PMMA, PVC,

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polymethacrylic acid and polymethacrylonitrile. The overall variation of the dispersive component of the surface energy and the ratio of acceptor to donor coefficients appear to group themselves into two categories based upon the polarity of the polymer’s functional groups. In addition, the high loadings required for stabilisation of the less polar polymers suggest that a relatively large volume of the matrix phase isaffected by the wood filler. 20 refs. USA

Accession no.786897 Item 142 Polymer Science Series B 42, Nos.5-6, May-June 2000, p.169-74 IR SPECTROSCOPY STUDY OF POLYMER POROSITY Pakhomov P M; Kruglova E V; Khizhnyak S D Tver,State University IR spectroscopic method is developed for evaluating the porosity (concentration and size of pores) in polymers. PE and PAN films of various porosity are prepared from the solutions in liquid and solid paraffins. The concentration and maximum pore size in the bulk and in a surface layer of the samples are determined by IR spectroscopy in the transmission and reflection modes, respectively. The results obtained are in agreement with the data of optical and atomic force microscopy. 12 refs. RUSSIA

Accession no.786845 Item 143 Iranian Polymer Journal 9, No.2, April 2000, p.117-24 STUDY OF CRYSTALLINITY OF HIGHDENSITY POLYETHYLENE BY INVERSE GAS CHROMATOGRAPHY Ghaemy M; Hadjmohammadi M R; Tabaraki R Mazandaran,University The crystallinity of HDPE (Poliran-HD0035 and Irapol5620) was investigated using inverse gas chromatography. The effects of flow rate of carrier gas and sample size on peak retention volume and of the amount of injection on retention volume were evaluated. Retention diagrams and degrees of crystallinity of the HDPEs were determined and compared with those of LDPE. 15 refs. IRAN

Accession no.786383 Item 144 Journal of Applied Polymer Science 77, No.7, 15th Aug.2000, p.1419-31 CURE MODELING AND MONITORING OF EPOXY/AMINE RESIN SYSTEMS. 1. CURE KINETICS MODELING

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References and Abstracts

Karkanas P I; Partridge I K Cranfield,University An investigation using differential scanning calorimetry was carried out under both isothermal and dynamic curing conditions to determine the cure kinetics of four epoxy/ amine resins. Various cure kinetic models were used to compare them with the results of the DSC results. Good fits were found, in good agreement with the experimental results for the resin systems. 22 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.786048 Item 145 International Polymer Science and Technology 27, No.6, 2000, p.T/7-T/9. (Translation of Muanyag es Gumi, No.3, 2000, p.89) APPLICATION OF STATE-OF-THE-ART METHODS IN ADHESION TECHNOLOGY. 1 Vabrik R; Czajlik I; Bertoti I; Keresztes Z; Ille A; Rusnak I; Vig A; Kalman E The use is demonstrated of microscopic analysis techniques for the investigation of adhesive failure. PVC sheet was bonded to glass using a M35R hybrid UV curable adhesive based on epoxy resin. Atomic force microscopy and X-ray induction photoelectron spectroscopy were used for the chemical characterisation of of failure surfaces. 11 refs. EASTERN EUROPE; HUNGARY

Accession no.785593 Item 146 Journal of Applied Polymer Science 78, No.1, 3rd Oct. 2000, p.166-72 EFFECT OF POLY(VINYL CHLORIDE)/ CHLORINATED POLYETHYLENE BLEND COMPOSITION ON THERMAL STABILITY Klaric I; Vrandecic N S; Roje U Split,University The miscibility of PVC and chlorinated PE and the effect of the blend composition on the heat stability of the PVC were investigated using several techniques, including TGA and DSC. The apparent activation energy of PVC dehydrochlorination in the blends was calculated and experimental TGA curves compared with those predicted using the additivity rule. It was found that the blends were heterogeneous and that addition of chlorinated PE in a specific temperature range resulted in an improvement in the heat stability of the PVC. 22 refs. CROATIA

Accession no.784861 Item 147 Polymer 41, No.22, Oct.2000, p.8161-5

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APPLICATION OF MODULATEDTEMPERATURE DIFFERENTIAL SCANNING CALORIMETRY TO THE STUDY OF CRYSTALLISATION KINETICS IN POLY(ECAPROLACTONE)-POLY(STYRENE-CO ACRYLONITRILE) BLENDS Song M; Hourston D J Loughborough,University In order to evaluate the application of modulatedtemperature differential scanning calorimetry (M-TDSC) to the study of the crystallisation kinetics of semicrystalline polymers, isothermal crystallisation kinetics in poly(e-caprolactone)-SAN blends are investigated. The temperature dependence of d ln G/dT (G =crystal growth rate), determined by M-TDSC agrees approximately with previous experimental data and theoretical values. These were obtained from direct measurements of spherulite growth rate by optical microscopy. Here, theoretical and M-TDSC experimental results show that the d ln G/dT versus temperature plots are not sensitive to the noncrystalline component in the poly(e-caprolactone)-SAN blends. 15 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.784242 Item 148 Polymer 41, No.22, Oct.2000, p.8151-4 PORE DIMENSION OF WATER TREES IN PE: NMR STUDIES Judeinstein P; Carmo Lanca M; Marat-Mendes J; Rault J Paris-Sud,Universite; Portugal,Universidade Nova de Lisboa In PE films aged under electric field the crystallisation of water (and melting of ice) is studied by quadrupolar NMR, this technique allows determination of water concentration as low as 10 -4. It is shown that the pore dimensions of the tracks forming the water trees of the order of 2.5 nm are independent of the ageing time. The mobility of water in these water trees and in porous glass, of similar pore dimensions, are compared. 17 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; PORTUGAL; WESTERN EUROPE

Accession no.784240 Item 149 Journal of Applied Polymer Science 77, No.10, 6th Sept.2000, p.2178-8 CURE MODELLING AND MONITORING OF EPOXY/AMINE RESIN SYSTEMS. II. NETWORK FORMATION AND CHEMOVISCOSITY MODELLING Karkanas P I; Partridge I K Cranfield,University The glass transition temperature (Tg) advancement and the chemoviscosity development under isothermal

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conditions are investigated for four epoxy/amine systems, including commercial RTM6 and F934 resins. Differential scanning calorimetry is the thermoanalytical technique used to determine the Tg advancement, and rheometry for determination of the chemoviscosity profiles of these resin systems. The complex cure kinetics are correlated to the Tg advancement via a one-to-one relationship using Di Benedetto’s formula. It is revealed that the threedimensional network formation follows a single activated mechanism independent of whether the cure kinetics follow a single or several activation mechanisms. The viscosity profiles show the typical characteristics of epoxy/amine cure. A modified version of the WilliamsLandel-Ferry equation (WLF) is adequate to model the viscosity profiles of all the resin systems, in the temperature range 130 to 170 deg.C, with a very good degree of accuracy. The parameters of the WLF equation are found to vary in a systematic manner with cure temperature. Further correlation between Tg and viscosity shows that gelation, defined as the point where viscosity reaches 10 4 Pas, occurs at a unique Tg value for each resin system, which is independent of the cure conditions. 16 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.784172 Item 150 Fire & Materials 24, No.2, March/April 2000, p.101-12 SMOKE GAS ANALYSIS BY FOURIER TRANSFORM INFRARED SPECTROSCOPY SUMMARY OF THE SAFIR PROJECT RESULTS Hakkarainen T; Mikkola E; Laperre J; Gensous F; Fardell P; Le Tallec Y; Bajocchi C; Paul K; Simonson M; Deleu C; Metcalfe E VTT Building Technology; Centexbel; Elf Atochem SA; UK,Building Research Establishment; CEMATE; LSF SUD srl; Rapra Technology Ltd.; Sweden,National Testing & Research Institute; Ghent,University; Greenwich,University The determination of toxic components from fire gases is difficult because the environment is hot, reactions are often temperature dependent, and a lot of soot may be produced. Due to the different properties of the gas components, a different time-consuming procedure for each species has traditionally been used. The use of FTIR (Fourier transform infrared) spectrometers as a continuous monitoring technique overcomes many of the problems in smoke gas analyses. FTIR offers an opportunity to set up a calibration and prediction method for each gas showing a characteristic spectral band in the infrared region of the spectrum. The objective of the SAFIR project was to further develop the FTIR gas analysis of smoke gases to be an applicable and reliable method for the determination of toxic components in combustion gases related to fire test conditions. The optimum probe design,

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filter parameters and the most suitable sampling lines in terms of flow rate, diameter, construction material and operating temperature have been specified. In the large scale, special concern was given to the probe design and the effects of the probe location as well as practical considerations of the sampling line length. Quantitative calibration and prediction methods have been constructed for different components present in smoke gases. Recommendations on how to deal with interferents, nonlinearities and outliers have been provided and a verification method for the spectrometer for unexpected variations and for the different models have been described. FTIR measurement procedures in different fire test scenarios are studied using the recommendations of this project for measurement techniques and analysis and an interlaboratory trial of the FTIR technique in smoke gas analysis is carried out to define the repeatability and reproducibility of the method in connection with a small scale fire test method, the cone calorimeter. 9 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; FINLAND; FRANCE; ITALY; SCANDINAVIA; SWEDEN; UK; WESTERN EUROPE

Accession no.784096 Item 151 Polymer 41, No.23, Nov.2000, p.8241-5 USE OF RAMAN SPECTROSCOPY TO STUDY THE REACTION BETWEEN AN AMINETERMINATED THERMOPLASTIC AND EPOXY RESINS van Overbeke E; Carlier V; Devaux J; Carter J T; McGrail P T; Legras R Louvain,Universite Catholique; ICI Plc Reactive thermoplastics are often used as toughening modifiers for epoxy resins. Raman spectroscopy was used to follow the reaction of aromatic amines with epoxide monomers through the evolution of an amine-substituted aromatic vibration. A double shift of this peak was correlated with the formation of secondary and tertiary amines. Band assignment was confirmed by the study of model compounds. Using this method, qualitative observation of the reaction between an amine-terminated copolyethersulphone thermoplastic and epoxide was performed. Unfortunately, in the blend studied containing the curing agent, a band appearing upon curing overlapped with the band characterising the end group reaction. 17 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.783075 Item 152 Polymer Degradation and Stability 68, No.3, 2000, p.437-43 SEMI-QUANTITATIVE ANALYSIS OF THERMAL DEGRADATION IN POLYPHENYLENE ETHER

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References and Abstracts

Kinoshita M; Nemoto T; Souda T; Takeda K Koito Mfg.Co.Ltd.; Shibaura,Institute of Technology The use of simple computer simulation and analysis of the thermal degradation products of differently thermally aged samples of melt processed polyphenylene ether film gave information on possible degradation routes for this polymer. An increase in dimeric products was noted with increased thermal ageing, but not in monomeric products. To explain the distribution of scission products found experimentally, the simple computer model was arranged to simulate cleavage rates of methylene bridge, ether and sidechain links. Although results were not totally conclusive, it was noted that both ether bridge and side chain cleavage rates were similar, and approximately nine times lower than cleavage rates of the methylene bridge. It is suggested that quantitative results determined will give detailed information on flame retardance due to the understanding of rates of volatile product generation at the polymer surface. 28 refs. JAPAN

Accession no.782776 Item 153 Polymer Degradation and Stability 68, No.3, 2000, p.321-6 COMPARATIVE ANALYSIS OF THE PHOTOOXIDATION OF POLYSTYRENE AND POLY(ALPHA-METHYLSTYRENE) Mailhot B; Jarroux N; Gardette J-L Ensemble Universitaire des Cezeaux Fourier transform infrared spectroscopy (FTIR) and mass spectroscopy were used to study the photo-oxidation of both poly(alpha-methylstyrene) (PMS) and polystyrene (PS) films which had been irradiated at different temperatures and with different radiation sources under an oxygen atmosphere. The oxidised films were treated with ammonia or sulphur tetrafluoride and photolysis carried out under vacuum. Photoproducts from both polymers were broadly similar, but aromatic ketone concentration was higher from the PMS and a new ketone was also identified from this source. Routes for formation of identified photoproducts are proposed. 13 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.782763 Item 154 ACS, Polymeric Materials Science & Engineering Fall Meeting 1999. Volume 81. Conference proceedings. New Orleans, La., 22nd-26th Aug.1999, p.242-3 ANALYSIS OF THE NANOPHASE STRUCTURE OF SEMICRYSTALLINE POLYMERS WITH ATOMIC FORCE MICROSCOPY (AFM), MICROCALORIMETRY (MC) AND TEMPERATURE-MODULATED CALORIMETRY (TMC)

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Wunderlich B Tennessee,University; Oak Ridge National Laboratory (ACS,Div.of Polymeric Materials Science & Engng.) Semicrystalline, polymeric materials consist usually of metastable aggregates of strongly coupled microphases or nanophases with their constituent, micrometre-long, flexible molecules traversing multiple phase domains. Some 40 years ago it was established that well-formed crystals are often lamellar with a thickness of only about 10 nm. Between these lamellae one can find the remaining amorphous phase with even smaller dimensions. Less perfect crystallisation can decrease the crystal dimensions to as little as 1-2 nm in all dimensions. An operational definition of the microphase is its having at least one dimension smaller than a micrometre, while nanophases are approached when the small dimension approaches 10 nm. Characteristic of the microphases is the need to consider the surface properties for their description, i.e. the melting temperature depends on the surface free energy. Nanophases, in turn, show an interaction between opposing surfaces, i.e. they may show no bulk properties. If the dimensions decrease below 1 nm, the macroscopic phase description has reached its limit. Many macromolecules can, however consist of alternating sequences of nanometerlength chain segments that are immiscible, so that in all their phase structures there is a strong tendency of nanophase separation. It is shown that special tools must be developed to probe the nanophase structures and properties of polymers. Some new information available by using three rather new techniques their combinations are described. 10 refs. USA

Accession no.780666 Item 155 ACS, Polymeric Materials Science & Engineering Fall Meeting 1999. Volume 81. Conference proceedings. New Orleans, La., 22nd-26th Aug.1999, p.236-7 CRYSTALLISATION AND MELTING OF POLYMER CRYSTALS REVEALED BY T-M DSC Toda A; Oda T; Tomita C; Hikosaka M; Arita T; Saruyama Y Hiroshima,University; Kyoto,Institute of Technology (ACS,Div.of Polymeric Materials Science & Engng.) Temperature-modulated differential scanning calorimetry (T-MDSC) applies a thermal modulation in temperature to a conventional DSC run and determines a dynamic heat capacity from the relationship between the modulation components of temperature and of heat flow. Primary application of this technique has been the measurement of specific heat capacity and the examination of the anomaly in a relaxation process such as alpha process related to the glass transition. An application to the firstorder phase transitions of crystallisation and melting of polymer crystals has recently been suggested. The method and typical results are described. 13 refs. JAPAN

Accession no.780663

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Item 156 ACS, Polymeric Materials Science & Engineering Fall Meeting 1999. Volume 81. Conference proceedings. New Orleans, La., 22nd-26th Aug.1999, p.173-4 FILM FORMATION IN POLYMER LATEX BLENDS: MICROSPECTROSCOPIC 3D STUDIES Zhao Y; Urban M W North Dakota State University (ACS,Div.of Polymeric Materials Science & Engng.)

Item 158 Analytical Chemistry 72, No.11, 1st June 2000, p.2490-8 CHARACTERISATION OF POLYETHER AND POLYESTER POLYURETHANE SOFT BLOCKS USING MALDI MASS SPECTROMETRY Mehl J T; Murgasova R; Dong X; Hercules D M; Nefzger H Vanderbilt University; Bayer Corp.

A series of previous studies on latex films indicates that mobility of low molecular weight species in particular surfactant molecules, may be affected by latex glass transition temperature, and subsequently, by free volume of a polymer matrix, surface tension at the film/air and film/substrate interfaces, compatibility and coalescence times, to name just a few. It appears that there are other factors that not only influence distribution of individual components including distribution of surfactants, but also may significantly affect film formation. In an effort to enhance understanding of these multi-phase latex blends and their coalescence, a series of experiments on latexes containing PS and poly-n-butyl acrylate (p-nBA) blends is presented. An attempt is made to identify factors affecting film formation of PS/p-nBA latex blends using multi-dimensional vibrational spectroscopic methods, and these findings are compared with respective copolymers. The effects of SDOSS exudation by latex composition, particle and annealing temperatures are also addressed in terms of phase separation and dynamics of macromolecular segments. 21 refs.

Selective degradation reactions combined with MALDI analysis were applied for molecular weight determination of polyether and polyester polyurethane soft blocks. Size exclusion chromatography was combined with MALDI to provide accurate molecular weight determination. 44 refs.

USA

Accession no.780632 Item 157 ACS, Polymeric Materials Science & Engineering Fall Meeting 1999. Volume 81. Conference proceedings. New Orleans, La., 22nd-26th Aug.1999, p.387-8 FAILURE STUDIES OF ADHESION BY UV REFLECTION AND FLUORESCENCE TECHNIQUES Kim N-J; Jeong C N; Sung C S P; Sung N-H Connecticut,University; Tufts University (ACS,Div.of Polymeric Materials Science & Engng.) Various techniques such as optical and electron microscopy, IR-ATR ESCA and SIMS have been used for failure mode analysis in polymeric adhesive joints. However, these techniques are not amenable for in situ, non-destructive examination of the failure surfaces as failure occurs. In order to develop in situ techniques, UV reflection and fluorescence methods are evaluated, as they can be applied via optical fibres to the actual failure surface. Failure surfaces of two types of adhesive joints are examined by UV reflection and fluorescence, complemented by FT-IR ATR studies. The first joint studied is PU on epoxy-coated steel. The second is PETP/PE/PETP. 8 refs.

USA

Accession no.778970 Item 159 Macromolecular Symposia Vol.152, March 2000, p.267-78 ANALYSIS OF COMPLEX POLYMERS BY MALDI-TOF MASS SPECTROMETRY Pasch H; Ghahary R German Plastics Institute The results are reported of an analysis of the functionality, molar mass and chemical composition of complex polymers, using MALDI-TOF mass spectrometry and a combination of MALDI-TOF mass spectrometry and liquid chromatography. Polymers investigated included polyamide-12, bisphenol A polycarbonate, methoxylated melamine-formaldehyde resin, carboxy-terminated PS and PMMA. 33 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.778702 Item 160 Journal of Injection Molding Technology 4, No.2, June 2000, p.84-91 ANALYSIS OF STYRENE PLASTIC RESIDUES ON INJECTION MOULDING TOOLS Makinen M; Astola J; Poutanen J; Alen R; Paakkonen E Tampere,University of Technology; Jyvaskyla,University The contaminating substances formed during the injection moulding of ABS and PS parts were removed from the mould surface. The residues were characterised using FTIR, gas chromatography, pyrolysis gas chromatography, elemental analysis, detection reaction test of bromine, and different dissolving tests. The chemical composition of the contamination was clarified and suitable solvents for dissolving these products were selected. 6 refs.

USA

EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN EUROPE

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Accession no.776471

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Item 161 Polymer 41, No.15, 2000, p.5949-55 UNDERSTANDING VITRIFICATION DURING CURE OF EPOXY RESINS USING DYNAMIC SCANNING CALORIMETRY AND RHEOLOGICAL TECHNIQUES Lange J; Altmann N; Kelly C T; Halley P J Queensland,University The gelation and vitrification transitions during cure of an epoxy resin-amine system were examined using rheological, modulated DSC and FTIR techniques. The results of DMA showed that gelation was observed before vitrification at all temps. where it could be rheologically defined. By comparing different rheological criteria for vitrification, it was seen that the vitrification transition was a gradual process that extended over a large part of cure at all temps. where it occurred. Results from modulated DSC measurements showed that the calorimetric vitrification times were longer than the vitrification times obtained from rheological measurements at cure temps. above 100C, but that at lower temps. calorimetric vitrification occurred before, or at the same time as, rheological vitrification. Theoretical gelation times, estimated from FTIR conversion data, were found to be consistently shorter than the observed gelation times. Theoretical vitrification times agreed well with the observed times. The magnitude of the vitrification transition, expressed either as amount of change in heat capacity or as maximum value of loss tangent, was found to decrease approximately linearly with increasing cure temp. 34 refs. AUSTRALIA

CHARACTERISATION OF POLYURETHANE COATINGS USING THERMOANALYTICAL TECHNIQUES Ginic-Markovic M; Choudhury N R; Matisons J G; Williams D R G South Australia,University; Adelaide,University A two-pack PU coating was analysed using thermoanalytical techniques. The curing reaction was monitored using pressure differential calorimetry, rheometry and dynamic mechanical analysis. The decomposition behaviour was examined using TGA. 13 refs. AUSTRALIA

Accession no.776090 Item 164 Injection Molding 8, No.6, June 2000, p.42/50 MATERIALS ANALYST: PART 33 DETERMINING COMPOSITION Sepe M Dickten & Masch Mfg. This article focuses on the problems associated with identifying a polymer. There are three major techniques that are particularly helpful in identifying the type of polymer used in a compound. These are DSC, TGA and IR spectroscopy. Each of these techniques has its strengths, and in determining the composition of the polymer, the task is to highlight properties and behaviour that are distinctive. USA

Accession no.775805

Accession no.776348 Item 162 Macromolecules 33, No.8, 18th April 2000, p.3180-3 COMPLETE ASSIGNMENT OF PROTON AND CARBON 13 NMR SPECTRA OF POLYVINYLCARBAZOLE Karali A; Froudakis G E; Dais P; Heatley F Crete,University; Manchester,University Details are given of the assignment of the proton and carbon 13 spectra of polyvinylcarbazole by using a number of modern gradient two-dimensional NMR experiments. The relationship between the assignments and the conformational and dynamic properties of the polymer is discussed. 13 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; UK; WESTERN EUROPE

Accession no.776167 Item 163 Journal of Thermal Analysis and Calorimetry 59, Nos.1-2, 2000, p.409-24

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Item 165 Polymer 41, No.11, 2000, p.4361-5 RAPID MICROWAVE INDUCED DEPOLYMERISATION OF POLYAMIDE 6 Klun U; Krzan A Ljubljana,National Institute of Chemistry Polyamide 6 depolymerisation was performed using microwaves as the energy source for the acid catalysed hydrolysis, with phosphoric acid as the catalyst. The product mixture was analysed by chromatographic and spectroscopic methods. 19 refs. SLOVENIA

Accession no.774158 Item 166 Polymer 41, No.11, 2000, p.4039-46 MATRIX-ASSISTED LASER DESORPTION/ IONISATION MASS SPECTROMETRY OF SYNTHETIC POLYMERS. IV. COUPLING OF SIZE EXCLUSION CHROMATOGRAPHY AND

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MALDI-TOF USING A SPRAY-DEPOSITION INTERFACE Esser E; Keil C; Braun D; Montag P; Pasch H Darmstadt,Deutsches Kunststoff-Institut Size exclusion chromatography and MALDI-TOF mass spectrometry was coupled via a robotic interface. For polydisperse synthetic polymers a continuous track of matter was deposited onto the matrix surface. Spectra were taken from different positions of the polymer track. Data are presented for PS, PMMA and butyl methacrylatemethyl methacrylate copolymers. 20 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.774127 Item 167 Muanyag es Gumi 37, No.3, 2000, p.89-91 Hungarian APPLICATION OF STATE-OF-THE-ART METHODS IN ADHESION TECHNOLOGY. I. Vabrik R; Czajlik I; Bertoti I; Keresztes Zs; Ille A; Rusznak I; Vig A; Kalman E Atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) were used to study the nature of the failure interface and the failure mechanism in a PVC film/ adhesive/glass system. The failure mode was found to be mostly interfacial, occurring at the glass/adhesive interface, and also partially cohesive, located in the adhesive layer very close to the interface. The results are discussed in relation to the chemical nature of the interface and the failure mechanism. 11 refs. Articles from this journal can be requested for translation by subscribers to the Rapra produced International Polymer Science and Technology. Accession no.773793 Item 168 Revista de Plasticos Modernos 78, No.521, Nov.1999, p.541-6 Spanish STRUCTURAL CHARACTERISATION OF MULTILAYER POLYMERIC MATERIALS BY MICRORAMAN SPECTROSCOPY Sanz R; Martin B; Merino J C; Pastor J M Valladolid,Universidad Results are presented of a study in which confocal microRaman spectroscopy was used to determine the structure of the individual polymers present in a series of multilayer food packaging films. 8 refs. AMCOR FLEXIBLES ESPANA SA EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.773260 Item 169 Iranian Journal of Polymer Science & Technology 12, No.2, Summer 1999, p.1-8

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Persian KINETIC STUDY OF THE AUTO-OXIDATION OF POLYURETHANE Semsarzadeh M A; Salehi H Tarbiat Modarres University Gel permeation chromatography was used to study the kinetics of the auto-oxidation of polyurethane. The stationary state rate and the induction time were determined at various temperatures. FTIR and H NMR were used to determine the alcohol, acetate and formate compounds in the auto-oxidation products. IRAN

Accession no.773140 Item 170 Journal of Macromolecular Science B B39, No.2, 2000, p.279-96 TIME-RESOLVED FTIR STUDY OF CRYSTALLISATION BEHAVIOUR OF MELTCRYSTALLISED POLYPHENYLENE SULPHIDE Yu J; Asai S; Sumita M Tokyo,Institute of Technology; China,Textile University The crystallisation behaviour of polyphenylene sulphide was studied using time-resolved FTIR spectroscopy and the results obtained correlated with DSC measurements. The 1073 cm/1 amorphous band was selected for the timeresolved measurements. The procedure provided details on the microstructure of the PPS, including heterogeneity of the amorphous phase above and below Tg. A method is proposed for calculating the rigid, amorphous fraction in terms of the increase in the slope of the absorbance variation with temperature at the glass transition. 43 refs. CHINA; JAPAN

Accession no.772147 Item 171 Journal of Applied Polymer Science 76, No.6, 9th May 2000, p.938-46 OPTIMIZATION OF EXPERIMENTAL PARAMETERS FOR THE QUANTIFICATION OF POLYMER ADDITIVES USING SFE/HPLC Thilen M; Shishoo R Swedish Institute for Fibre & Polymer Research A study was conducted with the aim of extracting the antioxidants Irganox 1010 and Irgafos 168 from a PP matrix by using the supercritical fluid extraction(SFE) technique and by subsequent analysis using highperformance liquid chromatography(HPLC). The experimental parameters of temp., pressure and modifiers were varied to find the best extraction conditions. The optimum temp. and pressure for extraction of these polymer additives were found to be 120 and 384 bar, with methanol as the modifier. The quantitative extractions were significantly faster than those reported previously in the literature. The results showed that the SFE/HPLC

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References and Abstracts

technique used in these experiments was a reliable and environmentally-friendly alternative to the commonlyused liquid extraction and analytical methods. 22 refs. EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN EUROPE

Accession no.770687 Item 172 Macromolecular Symposia Vol.148, Dec.1999, p.463-81 CHARACTERIZATION OF ACRYLIC DENTAL POLYMERS Vera-Graziano R; Martinez-Richa A; Palacios-Alquisira J; Barcelo-Santana F; Castano-Meneses V Mexico,Universidad Nacional Autonoma; Guanajuato,Universidad The chemical composition, dimensions and the molecular parameters of four dental acrylic polymer materials and two polyacrylic acids of different molec.wt. used as model compounds were studied by NMR and IR spectroscopies, GPC, intrinsic viscosity and light scattering measurements. Two of the dental polymers were shown to be mainly polyacrylic acid, while one showed the peak pattern for an acrylic acid/methyl acrylate copolymer of about 2:1 composition and one was an oligomer derived from 2-hydroxyethyl methacrylate. The steric hindrance parameter, molecular stiffness and second virial coefficient were calculated using different thermodynamic models. The Flory-Fox-Shafgagen and the StockmayerFixman models fitted the experimental data reasonably well and could be use to describe the molecular parameters of the acrylic polymers. 18 refs. (7th International Conference on Polymer Characterization (POLYCHAR7), Denton, Texas, USA, Jan.1999) MEXICO

Accession no.770356 Item 173 Flame Retardants 2000. Conference proceedings. London, 8th-9th Feb.2000, p.185-92 PRACTICE OF FTIR ANALYSIS FOR FIRE GASES (SAFIR) Mikkola E VTT Building Technology (BPF; Interscience Communications Ltd.; APME; European Flame Retardant Assn.; Fire Retardant Chemicals Assn.) The use of FTIR (Fourier transform infrared) spectrometers as a continuous monitoring technique overcomes many of the problems associated in analyses of hot fire gases. FTIR offers an opportunity to set up a calibration and prediction method for each gas showing a characteristic spectral band in the infrared region of the spectrum. A European project, SAFIR, aims to further develop the FTIR gas analysis of smoke gases to be an applicable and reliable method for the determination of toxic components in combustion gases related to fire test

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conditions. Within this project, optimal working conditions including sampling, calibration and analysis for FTIR fire gas method are defined and verified under a variety of fire test scenarios. The FTIR method are shown to be a repeatable and reproducible method for the determination of the most important toxic gas components of real fires. Moreover, the findings of this project concerning sampling techniques are most relevant for other methods used for defining fire gases. 5 refs. EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN EUROPE

Accession no.768669 Item 174 Surface Coatings International 83, No.3, March 2000, p.111-8 DETERMINATION OF VOC EMISSIONS FROM LATEX PAINTS DURING AND AFTER APPLICATION; METHODS, PERFORMANCE AND PRECISION Zeh H Wacker Polymer Systems GmbH VOC emissions from indoor latex paints during and after application is determined by four different test methods: a chamber method in which an emission chamber is combined with gas chromatography, two practical methods in which VOC emitted in a room is measured either by the determination of the total organic carbon or by infrared spectroscopy, and an ‘in-can-individual-VOC method’ which determines the VOC of a liquid paint by the quantitative analysis of each volatile component. VOC emission data gathered by these methods are compared with calculations from a dynamic computer model describing the time-dependence of the VOC emission in the room atmosphere. This comparison indicates that the ‘in-can-individual-VOC method’ with computer calculation allows variations in the size of the room, the application rate, VOC content of the paint and the rate of air change, without the necessity of additional experiments, and therefor, offers an approach with a reduction in costs. 10 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.768107 Item 175 Journal of Coatings Technology 72, No.902, March 2000, p.53-61 ACID ETCH OF AUTOMOTIVE CLEARCOATS. II. COMPARISON OF DEGRADATION CHEMISTRY IN LABORATORY AND FIELD TESTING Schmitz P J; Holubka J W; Xu L-F Ford Motor Co. X-ray photoelectron spectroscopy was used to determine whether exposure conditions used in the laboratory gravimetric etch testing of acrylic melamine clearcoats

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simulated field degradation pathways. The surface chemistry of the field exposed panels was examined and the results compared with those for laboratory treated powders having identical technologies. Consistency in the formation of a melamine salt and ammonium sulphate upon field exposure and laboratory acid treatment indicated that the laboratory treatment conditions simulated the field exposure conditions. 7 refs. USA

Accession no.767768 Item 176 Journal of Adhesion Science and Technology 14, No.5, 2000, p.745-64 XPS ANALYSIS OF THE COVERAGE AND COMPOSITION OF COATINGS ON GLASS FIBRES Thomason J L; Dwight D W Owens-Corning Science & Technology Center The use of X-ray photoelectron spectroscopy as a method for characterising different sizings on glass fibres was evaluated. A model, based on a patchy sizing overlay hypothesis, was developed to aid in the reduction of data obtained from the X-ray photoelectron spectroscopic analysis. It is shown that the spectroscopic results, when combined with the weight fraction of the sizing, provide a quantitative value for the coverage of the fibre surface by the sizing. 25 refs. USA

Accession no.767755 Item 177 Polymer News 25, No.2, Feb.2000, p.56-8 POLYMER ANALYSIS AND CHARACTERISATION Garbassi F EniChem SpA Analytical techniques, such as mass spectroscopy, atomic absorption spectroscopy and atomic emission spectroscopy, for the detection of trace elements, mainly metal trace elements, in polymers, used particularly in food, are briefly considered. The disadvantages and suitability of such techniques are summarised. 10 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.766702 Item 178 Adhesion ’99. Conference Proceedings. Cambridge, UK, 15th-17th Sept.1999, p.369-73 INTERPHASE CHEMISTRY OF CARBON FIBRE COMPOSITE MATERIALS Prickett A C; Vickers P E; Smith P A; Watts J F Surrey,University (IOM Communications Ltd.)

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The fibre-matrix interface in carbon fibre-reinforced epoxy resin composites was studied by time of flight secondary ion mass spectrometry (ToF-SIMS) using novel preparation techniques. The initial adsorption between uncured resin or amine curing agent and the fibre was investigated by the use of adsorption isotherms obtained by the analysis of fibre surfaces following immersion in liquid solutions of the resin. The intact interphase of a composite could be examined by ToF-SIMS following mode I or mode II failure within the spectrometer by the use of carefully designed in-situ fracture stages. 11 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.765326 Item 179 Adhesion ’99. Conference Proceedings. Cambridge, UK, 15th-17th Sept.1999, p.347-50 MICRO THERMAL ANALYSIS AT INTERPHASES Hassler R; zur Muhlen E Dresden,Institut fuer Polymerforschung; TA Instruments GmbH (IOM Communications Ltd.) Details are given of a thermal analysis technique, referred to as micro thermal analysis, which combines the high resolution positioning of scanning probe microscopy with some of the quantitative analysis capabilities of conventional thermal analysis. The application of this technique in characterising the thermal properties of interfaces in aluminium/epoxy resin adhesive joints and in glass fibrereinforced epoxy resin composites is described. 7 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; UK; WESTERN EUROPE

Accession no.765322 Item 180 Macromolecules 33, No.1, 11th Jan.2000, p.120-4 BRANCHING AND CROSSLINKING IN RADIATION-MODIFIED PTFE. A SOLID-STATE NMR INVESTIGATION Fuchs B; Scheler U Dresden,Institute of Polymer Research High-resolution fluorine 19 NMR was used to investigate the structural changes resulting from PTFE electron irradiation under vacuum. A quantitative analysis of the data was used to establish the density of side groups and branches. 20 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.764731 Item 181 Color and Appearance Retec 1999. Conference proceedings.

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References and Abstracts

Nashville, Tn., 27th-29th Sept.1999, p. 178-87 USING MICROSCOPY AS A PROBLEM SOLVING TOOL IN PLASTICS Compton C Sun Chemical Corp. (SPE,Color & Appearance Div.) Microscopy is a valuable tool for pigment evaluation and problem solving in plastics and other applications. The organic pigments used in plastic applications are typically sub-micron in size. Pigment performance is greatly affected by how well the pigment particles are incorporated in the polymer medium. Various microscopic evaluation techniques that can be used to investigate dispersion quality, strength development and thermal stability are reviewed. In addition, various microscopic techniques for identifying contaminants are discussed. 7 refs.

drinking water in contact with PP pipes was studied. Austrian, German and International Standard methods were used for water at 23C and 60C. The low molecular degradation product 2,4-di-tert-butylphenol, rather than the high molecular antioxidants, was detected in the aqueous extracts. In warm water extracts, the concentration of phenols, the total organic carbon content and the effect on odour and flavour were considerably higher than in cold. Alkaline water extracted higher amounts of phenols but acidic drinking water showed no effect. Thermal loading of PP during the extrusion process significantly increased the extractable phenols, total organic carbon content and flavour number/threshold odour. 7 refs. AUSTRIA; EUROPEAN UNION; WESTERN EUROPE

Accession no.763574

USA

Accession no.764247 Item 182 Composites Part A: Applied Science and Manufacturing 31A, No.2, 2000, p.165-71 FAILURE PHENOMENA IN TWODIMENSIONAL MULTI-FIBRE MICROCOMPOSITES. PART IV: A RAMAN SPECTRASCOPIC STUDY ON THE INFLUENCE OF THE MATRIX YIELD STRESS ON STRESS CONCENTRATIONS van den Heuval P W J; Peijs T; Young R J Eindhoven,University of Technology; UMIST; Queen Mary & Westfield College Raman spectroscopy is used to study the influence of shear yield stress of the matrix on stress situations in carbon fibre/epoxy resin composites containing a planar fibre array. A mixture of two curing agents, with different functionality and molecular weights, are used to cure the epoxy resin in order to obtain a matrix with varying crosslinked density. The carbon fibres are surface treated to give good fibre-matrix adhesion. Three matrix systems are investigated in the study, each with a different yield stress. The mechanical properties of each material are measured under tension and shear conditions. 35 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; UK; WESTERN EUROPE

Accession no.763633 Item 183 Journal of Macromolecular Science A A36, No.11, 1999, p.1751-8 POLYPROPYLENE PIPES FOR DRINKING WATER SUPPLY Hametner C Austrian Plastics Institute The migration of phenolic antioxidants (which are typically used for the stabilisation of PP pipes) into

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Item 184 West Conshohocken, PA, 1999, pp.6. NALOAN. ASTM D 2124-. METHOD FOR ANALYSIS OF COMPONENTS IN POLY (VINYL CHLORIDE) COMPOUNDS USING AN INFRARED SPECTROPHOTOMETRIC TECHNIQUE American Society for Testing & Materials ASTM D 2124Version 99. Photocopies and loans of this document are not available from Rapra. USA

Accession no.760789 Item 185 Journal of Coatings Technology 72, No.900, Jan.2000, p.69-74 ANALYSIS OF EXEMPT PAINT SOLVENTS BY GAS CHROMATOGRAPHY USING SOLIDPHASE MICROEXTRACTION Bodrian R R California,Polytechnic University Acetone, methyl acetate and parachlorobenzotrifluoride have been exempted as VOC solvents by the EPA. In measuring coating VOC content, separate methods for determining exempt solvents are required. One such method utilises solid-phase microextraction to sample the headspace of solvent-based coatings to which the surrogates acetone-d6, methyl acetate-d3 and/or metachlorbenzotrifluoride have been added. The sampled exempt coating solvents are thermally desorbed and analysed using gas chromatography with flame ionisation or mass spectral detection. This paper presents the results obtained for acetone and toluene in a large number of aerosol paints. Additionally, the results from a round-robin study for acetone, methyl acetate and parachlorobenzotrifluoride in commercial solvent-based coatings are reported. 17 refs. USA

Accession no.760572

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Item 186 Journal of Thermal Analysis and Calorimetry 57, No.3, 1999, p.847-51 IDENTIFICATION OF POLYETHYLENE BY DIFFERENTIAL SCANNING CALORIMETRY Tsukame T; Kutsuzawa M; Sekine H; Saitoh H; Shibasaki T Saitama,Criminal Investigation Laboratory; Saitama,University A forensic sample consisting of melt-recrystallised polymers recovered from the scene of a fire in a factory is identified by differential scanning calorimetry. The factory commonly used two kinds of film sheets, A and B, made by different manufacturers. It is necessary to decide whether the forensic sample related to material A or B. The forensic sample and reference samples of materials A and B are subjected to IR spectroscopy and pyrolysis gas chromatograph mass spectrometry measurements, which reveal their PE nature. The thermal behaviour of the samples is examined by differential scanning calorimetry (DSC) and they are found to be blends of two kinds of PEs, LDPE and LLDPE. The samples can be identified and distinguished from each other via the DSC measurements. 6 refs. JAPAN

Accession no.760331 Item 187 Journal of Thermal Analysis and Calorimetry 58, No.1, 1999, p.13-8 THERMAL CHARACTERISATION OF POLYURETHANE ACRYLATE RESINS Ledru J; Saiter J M; Grenet J; Yuossef B; Burel F; Bunel C Rouen,University; Rouen,Institut National des Sciences Appliquees Polyurethane acrylate resins cured by two different methods, thermally and photochemically, are investigated by means of differential scanning calorimetry and thermally stimulated depolarisation currents. Even if both curing methods lead to the same material from a chemical point of view, important differences exist between the thermocured resin and the photocured resin in terms of molecular relaxation behaviour. 8 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.760327 Item 188 Applied Spectroscopy 53, No.11, Nov.1999, p.1412-8 IN-LINE NEAR-INFRARED MONITORING OF POLYMER PROCESSING. I. PROCESS/ MONITOR INTERFACE DEVELOPMENT Reshadat R; Desa S; Joseph S; Mehra M; Stoev N; Balke S T

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Toronto,University Near-infrared inline monitoring of polymer processing means using an optical fibre-assisted spectrometer to obtain spectra of the polymer melt flowing through commonly used processing equipment (an extruder). Conditions in the extruder are typically 200 deg.C and 20 MPa. The design of interfaces between the spectrometer and the molten polymer is shown. Three designs are shown, each permitting monitoring at a different location in the process: a melt-at-die interface, a melt-in-barrel interface and a strand interface. These designs are for monitoring just before the extruder exit, in the main barrel of the extruder and after the product exits from the extruder as a strand, respectively. All these interfaces protect the inserted optical fibre probe from the harsh environment within the extruder while permitting easy replacement or a probe without interrupting the process. This latter characteristic is very important because it permits easy probe repair as well as the use of other types of probes (for monitoring colour or particles, for example) to be used during a run. Examples of near-infrared spectra obtained with each of the interfaces used with an immiscible blend of PE and PP are shown. Large differences in the spectra demonstrate that the design of the interface will affect multivariate analysis directed at composition prediction. Subsequent papers are directed at using the melt-at-die interface for composition prediction and accounting for nonlinear relationships between absorbance and concentration. 6 refs. CANADA

Accession no.760231 Item 189 Applied Spectroscopy 53, No.11, Nov.1999, p.1403-11 THERMAL VOLATILISATION ANALYSIS: A VERSATILE PLATFORM FOR SPECTROSCOPIC INVESTIGATION OF POLYMER DEGRADATION PROCESSES Guo X; Huang B; Dyakonov T; Chen Y; Padron L; Vickstrom T; Kuhn J; Hodkiewicz J; Stevenson W T K Wichita,State University; Harrick Scientific Co.; Oklahoma State University; Koch Industries Inc.; ATI Instruments Thermal volatilisation analysis (TVA) and sub-ambient thermal volatilisation analysis (SATVA) techniques are described. In addition to rate profiling of the volatile product flux of thermal degradation under high-vacuum conditions through measurement of pressure in the vacuum line as a function of sample temperature, the TVA technique is shown to afford a convenient method for an on the basis of volatility under high-vacuum conditions, of product fractions of thermal degradation for subsequent spectroscopic analysis. The capacity and flexibility of TVA as a platform for these analyses are illustrated in a case study format by degrading poly(bisphenol A, 2-

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References and Abstracts

hydroxy propylether). The overall degradation process is quantified, and most significant pathways of thermolysis are identified through subsequent spectroscopic analysis of products of decomposition. The design and construction of a modified vacuum-tight long-path gas IR cell, as an interface allowing for the application of Fourier transform infrared spectroscopy (FT-IR) for the online analysis of volatile products of polymer degradation, is described. Proof of concept and application of this new analytical technique, subsequently referred to as TVA/FT-IR, is illustrated through the examination of appropriate aspects of the thermal degradation of PMMA polymers. 49 refs. USA

Accession no.760230 Item 190 Analytical Chemistry 71, No.21, 1st Nov.1999, p.4793-9 GEL PERMEATION CHROMATOGRAPHY COUPLED TO FOURIER TRANSFORM MASS SPECTROMETRY FOR POLYMER CHARACTERIZATION Aaserud D J; Prokai L; Simonsick W J Florida,University On-line coupling of GPC to Fourier transform(FT) mass spectrometry(MS) using a modified commercial electrospray ionisation(ESI) interface was studied. Selected oligomer profiles for the sodiated oligomer ions of a narrow molec.wt. PMMA were generated and used for obtaining a calibration curve. Using the MS-generated calibration curve and the refractive index response for quantification, an accurate MWD was calculated and shown to be in good agreement with the value specified by the supplier. GPC/ESI/FT-MS also allowed for an unequivocal end group determination and characterisation of a secondary distribution due to the formation of cyclic reaction products. A glycidyl methacrylate/butyl methacrylate copolymer with a broad MWD was analysed, fractionation and high resolving power being required for adequate characterisation. MWD data showed the advantages of coupling high-resolution MS and GPC to overcome the difficulty of analysing polydisperse polymers with MS alone. 34 refs. USA

mode atomic force microscopy (AFM). The microfibrils feature is observed with an average width of 500 nm, composed of various types of periodical units of an average size 50 nm in a pleating appearance. At the less crystalline spot on the Kevlar fibre surface, the periodical organisations exhibit the skin core-like differentiation. In contrast, at the highly crystalline spot, the periodicity is more uniformly arranged by a rectangular network manner. Inverse gas chromatography (IGC) is used as a tool to investigate the surface structure heterogeneity by calculating the surface energy of different types of probes adsorbed on the Kevlar fibre surface. The energy sites distribution plot of n-hexylamine adsorption at finite dilution exhibits a two-adsorbing-peaks curve. At the higher energy site, a possible hydrogen bonding interaction is proposed between n-hexylamine and oxygen-containing groups formed at the less crystalline surface. According to the AFM and IGC results, a Kevlar fibre surface organisations model at the nanometer scale is proposed. 19 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; SWITZERLAND; WESTERN EUROPE

Accession no.758987 Item 192 Macromolecular Chemistry & Physics 200, No.10, Oct.1999, p.2345-55 THERMAL DEGRADATION MECHANISMS OF POLYETHERIMIDE INVESTIGATED BY DIRECT PYROLYSIS MASS SPECTROMETRY Carroccio S; Puglisi C; Montaudo G Istituto per la Chimica e la Tecnol.dei Mat.Pol.; Catania,University The thermal degradation of poly(2,2'-bis(3,4dicarboxyphenoxy)phenylpropane-2-phenylenediimide) was investigated by TGA and direct pyrolysis mass spectrometry and the pyrolysis of this polyimide compared with that of an aromatic polyamide (NOMEX). The structure of preformed oligomers from the purified polyetherimide and the structure of high temperature pyrolysis products obtained at 620C were examined and the thermal degradation pathways involved in the degradation elucidated. 32 refs.

Accession no.759794

EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Item 191 Polymer 40, No.26, 1999, p.7341-50 SURFACE STRUCTURE OF KEVLAR FIBRE STUDIED BY ATOMIC FORCE MICROSCOPY AND INVERSE GAS CHROMATOGRAPHY Rebouillat S; Peng J C M; Donnet J-B Du Pont de Nemours International SA; HauteAlsace,Universite

Accession no.757742

Kevlar fibre surface structure is primarily and directly observed in the filament configuration by the tapping

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Item 193 Macromolecular Chemistry & Physics 200, No.10, Oct.1999, p.2205-7 COLLECTION OF SOLID-STATE CARBON-13 CP/MAS NMR SPECTRA OF COMMON POLYMERS Wilhelm M; Neidhoefer M; Spiegel S; Spiess H W Max-Planck-Institut fuer Polymerforschung; WileyVCH Verlag GmbH

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A collection of high resolution solid-state Carbon-13 NMR spectra of a wide range of polymers is presented. It is useful for reference purposes in case of unknown or partly unknown samples, such as polymer blends, block copolymers or polymeric latices. 16 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.757725 Item 194 Polymer Degradation and Stability 66, No.1, 1999, p.107-25 VACUUM PYROLYSIS OF PVC. II: PRODUCT ANALYSIS Miranda R; Pakdel H; Roy C; Darmstadt H; Vasile C Quebec,Universite Laval; Institut Pyrovac Inc.; Petru Poni,Institute of Macromolecular Chemistry Vacuum pyrolysis of pure PVC was carried out at various temperatures between 220 and 520C and under a total pressure of 2 kPa. The main gaseous and liquid pyrolysis products obtained during the different stages of thermal degradation were identified and quantified by chromatographic methods. Global mass balance and chlorine mass balance were determined and different methods of capturing hydrogen chloride under vacuum conditions were tested. The elemental composition, surface properties and calorific value of the solid residue were determined. 43 refs.

Item 196 Polymer International 48, No.10, Oct.1999, p.1042-5 EFFECTS OF UV RADIATION ON SEVERAL HIGH-PERFORMANCE POLYIMIDE COMPOSITES Kiefer R L; Herring K; Wylie B J; Orwoll R A; Thibeault S A Williamsburg,College of William & Mary; NASA Langley Research Center Three carbon fibre-reinforced polyimides were exposed to UV radiation at 177C, at three different intensities for three different times, so that the product of intensity and time was a constant. Intensities of 1, 2 and 3 suns, where one sun is the power in space at one earth-sun distance, were used, for a time periods of 500, 250 and 167 h. The samples were characterised by X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis, thermomechanical analysis and dynamic mechanical analysis. Measurement of bulk properties showed no difference between samples exposed to heat and UV radiation, and control samples. Surface analysis by XPS showed an apparent decrease in carbonyl concentration on the surface of some exposed samples. This was correlated to surface contamination by a siliconecontaining material. 3 refs. USA

Accession no.756185

CANADA; EASTERN EUROPE; RUMANIA

Accession no.757340 Item 195 Polymer Recycling 4, No.1, 1999, p.13-25 COMPOSITIONAL ANALYSIS AND FEASIBILITY STUDY OF RECYCLED HDPE FOR DIRECT FOOD CONTACT APPLICATIONS Salafranca J; Cacho J; Nerin C Zaragoza,University Five HDPE samples, consisting of a virgin HDPE for food-contact applications, three samples of this polymer taken after each of the three sequential recycling cycles and a real post-consumer sample were analysed. Two different extraction methods were applied: a combination of maceration and sonication; and the total dissolution of the polymer. In order to evaluate both the feasibility of using these polymers in food-contact applications and the evolution of HDPE composition through the recycling process, samples were analysed by both qualitative and quantitative GC-MS. Furthermore, GC-FID was applied to the determination of alpha-alkenes, the most representative compounds as indicators of polymer matrix degradation. Finally, antioxidants were analysed by reversed phase HPLC. 34 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

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Item 197 Composites Part A: Applied Science and Manufacturing 30A, No.12, 1999, p.1401-13 USE OF XPS FOR CHARACTERISATION OF GLASS FIBRE COATINGS Thomason J L; Dwight D W Owens-Corning Science & Technology Center X-ray photoelectron spectroscopy was applied to a study of commercial and experimental glass fibres using three different instruments. A protocol for plotting ratios of appropriate atom concentrations was developed and the plots used to estimate the surface coverage of the coating on the glass fibres and provide data on the chemical composition of the coating. The relationships between the spectroscopic data and coated glass fibre parameters are demonstrated using an overlay model and data from the three instruments are compared. 22 refs. USA

Accession no.755993 Item 198 Analytical Chemistry 71, No.20, 15th Oct.1999, p.4776-80 COMPOSITION AND MICROSTRUCTURE DETERMINATION OF A LATEX SYSTEM BY PYROLYSIS GAS CHROMATOGRAPHY

© Copyright 2002 Rapra Technology Limited

References and Abstracts

Frank Cheng-Yu Wang Dow Chemical Co.

of branching and determination of refractive index increment. 19 refs.

The composition and microstructure of polymers in a latex system were studied by pyrolysis gas chromatography. The composition and microstructure of a polymer in the emulsion phase were identified by direct pyrolysis of the latex system, followed by comparing the trimer peak pattern with appropriate microstructure standards. The polymer in the aqueous phase was pre-pyrolysis derivatised with tetrabutylammonium hydroxide to convert the acid to its butyl ester. Similar procedures were then used to explore the composition and microstructure of the polymer in the aqueous phase. Polymers analysed included SCX-2660 (probably a styrene-methyl methacrylate-butyl acrylate terpolymer), styrene-butyl acrylate copolymer and styrene-alpha-methylstyrenebutyl acrylate terpolymer. 17 refs. JOHNSON S.C.,& SON INC.

CZECH REPUBLIC

USA

Accession no.755491

Accession no.755899 Item 199 Oxford, Butterworth-Heinemann Ltd., 1999, pp.xxvii,920. 24cms. 12/1/00. 011 PLASTICS MATERIALS. 7TH EDN. Brydson J A The latest edition, now the seventh, of this reputable text book, provides an overview of the scientific, technological and economic aspects of currently available plastics and related materials, and also focuses on new materials many based on metallocene catalyst technology. Developments with condensation polymers, including several new polyester-type materials of interest for bottle blowing and/or degradable plastics, are also covered. This edition also attempts to explain the basis of metallocene polymerisation. The commercial importance of the materials discussed is also noted. Accession no.755818 Item 200 Journal of Applied Polymer Science 74, No.10, 5th Dec.1999, p.2432-8 CHARACTERIZATION OF BISPHENOL ABASED EPOXY RESINS BY HPLC, GPC, GPCMALLS, VPO, VISCOMETRY, AND END GROUP ANALYSIS: ON THE IDENTIFICATION OF 2,3DIHYDROXYPROPYL-CONTAINING COMPOUNDS, DETERMINATION OF MOLAR MASS DISTRIBUTION, AND BRANCHING Podzimek S; Kastanek A SYNPO Results of the above characterisation are presented and discussed with particular reference to determination of alpha-glycol-containing compounds, determination of molar mass and molar mass distribution, determination

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Accession no.755647 Item 201 Journal of Vinyl and Additive Technology 5, No.3, Sept.1999, p.148-58 NMR SPECTRA OF LEAD STABILISERS Grossman R F Halstab Corp. High resolution proton and 13C NMR spectra of leadbased heat stabilisers and their reaction products, obtained using the magic angle spinning technique, support structural assignments inferred from IR spectra. These demonstrate that lead stabilisers are unique compounds, rather than the double salts of lead oxide found in textbooks. 8 refs. USA

Item 202 Polymers for Advanced Technologies 10, No.4, April 1999, p.237-43 CHARACTERISATION OF THE SURFACE OF BULK-MOULDED COMPOUNDS Vallat M F; Schultz J; Mauzac C; Jacquin M Institut de Chimie des Surfaces et Interfaces; PSA Etudes et Recherches Centre Technique de Belchamp The surface characterisation of bulk moulding compound (BMC) automotive parts using complementary techniques of surface analysis, i.e. SEM, X-ray photoelectron spectroscopy, time of flight secondary ion mass spectroscopy, glow discharge spectroscopy and contact angle is described. Similarities and differences between BMC surfaces and sheet moulding compound (SMC) surfaces are pointed out. Particular emphasis is placed on mould release agents (polymeric and stearate) on the surface which can influence future bonding behaviour. 14 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.754736 Item 203 Macromolecular Chemistry & Physics 200, No.9, 1999, p.2074-9 INVESTIGATION OF MOLECULAR DIMENSIONS OF POLYSTYRENE AS A FUNCTION OF SOLVENT COMPOSITION: APPLICATION TO LIQUID CHROMATOGRAPHY AT THE EXCLUSIONADSORPTION TRANSITION POINT Baran K; Laugier S; Cramail H ENSCPB Liquid chromatography was used to study PS standards at the exclusion-adsorption transition point using silica

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References and Abstracts

adsorbents having differing porosities in various eluents. The behaviour of model PS chains in solvent mixtures corresponding to the critical adsorption conditions was evaluated using viscometry and light scattering. It was found that critical adsorption conditions could be achieved if the polymer chains entered the pores of the stationary phase and that the characteristics of the elution mode could be defined with the aid of the polarity index of the eluent. 20 refs.

Item 206 LCGC International 12, No.9, Sept.1999, p.577/87 LC-MS ANALYSIS OF POLYMER ADDITIVES BY EL AND API: IDENTIFICATION AND QUANTIFICATION Yu K; Block E; Balogh M Waters Corp.

EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Mass spectrometry can be the ideal detector for liquid chromatography because it offers both universality and the required selectivity for complex analytical problems. The two most popular types of interface for the benchtop single quadrupole LC-mass spectrometer are the particle beam interface and the atmospheric pressure ionisation interface. The particle beam interface is used to generate electron ionisation spectra and the API interface is used to generate either electrospray or atmospheric pressure chemical ionisation. This comprehensive article supplies a detailed analysis of a study in which organic extractable from polypropylene was used as the model analyte to demonstrate how the information obtained separately from EI and API can be complementary. Seven compounds were separated and detected by both MS detectors. 35 refs.

Accession no.752269 Item 204 Macromolecular Symposia Vol.141, 1999, p.95-101 RECENT ADVANCES IN THE ANALYSIS OF POLYMERS AND COPOLYMERS BY MASS SPECTROMETRY Montaudo M S Istituto per la Chimica e la Tecnol.dei Mat.Pol. Progress which has been made in the use of MALDI mass spectroscopy to provide reliable molec.wt. and MWD values is reported. Molec.wt. averages and MWD of polydisperse samples (PMMA, siloxanes, polyesters and copolyesters) were obtained by off-line coupling of SEC equipment with the MALDI mass spectrometer. SEC traces of the samples were recorded, selected fractions were analysed by MALDI-TOF and the average molec.wts. of the fractions were determined from the mass spectrum. A method for analysing unknown copolymers, which involves the use of Markoffian statistics, is also presented. 26 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.752091 Item 205 Polimery 44, No.4, 1999, p.246-54 Polish USE OF PHOTOELECTRON SPECTROSCOPY IN STUDIES OF THE DEPTH PROFILE OF POLYPROPYLENE FILM Zenkiewicz M; Golebiewski J Metalchem Plastics Processing Institute

USA

Accession no.747567 Item 207 Macplas International No.10, Aug.1999, p.64-70 DIFFERENTIAL SCANNING COLORIMETRY AND INFRARED SPECTROSCOPY IN POLYMER ANALYSIS Panarotto A; Bertucci M Cesap Differential scanning calorimetry is one of the most commonly used methods for characterising the thermal properties of polymers. This method, particularly if complemented by IR spectroscopic analysis, also allows the nature of the materials under test to be determined. The principles involved in DSC and IR spectroscopy are discussed. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.745360

The physical fundamentals of photoelectron spectroscopy are reviewed and the range of applications is given. Three PP films were examined and the depth of oxidation was found to be in the nanometer range. The oxidation level of the external layer increases as the specific energy of corona discharges is increased. 27 refs. Articles from this journal can be requested for translation by subscribers to the Rapra produced International Polymer Science and Technology.

Item 208 Polimery Tworzywa Wielkoczasteczkowe 44, No.3, 1999, p.218-21 Polish DETERMINATION OF MIGRATION OF DIMETHYL TEREPHTHALATE AND DIMETHYL ISOPHTHALATE FROM PLASTICS Stareczek T; Kaminska G; Ermel J; Kortylewska Edited by: Gliwice,Institute of Plastics & Paint Industry

EASTERN EUROPE; POLAND

A gas chromatographic method is described for determining dimethyl terephthalate and dimethyl

Accession no.747688

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References and Abstracts

isophthalate in food simulants. The method consists in extracting DMT and DMIP from the food simulants with chloroform and analysing of the compounds by GC with the use of calibration curves and diethyl terephthalate as an internal standard. 3 refs. Articles from this journal can be requested for translation by subscribers to the Rapra produced International Polymer Science and Technology.

proposed and tested liquid chromatographic elution of homopolymers under limiting conditions of desorption and takes into account the simultaneous effect of adsorption and exclusion of macromolecules onto/from the column packing. 17 refs. SLOVAK REPUBLIC; SLOVAKIA

Accession no.743327

EASTERN EUROPE; POLAND

Accession no.745025 Item 209 Journal of Applied Polymer Science 73, No.2, 11th July 1999, p.221-6 EVALUATION OF EVA-PVAC BLEND BEHAVIOUR BY 1-D AND 2-D SOLID-STATE NMR De Souza C M G; Pacheco C R; Tavares M I B Rio de Janeiro,Universidade Federal; PETROBRAS Ethylene-co-vinyl acetate and poly(vinyl acetate) blends were prepared in different proportions by melting in a HAAKE Rheomix mixer. The blends were prepared at a fixed temperature, rotation rate, and processing time. High-resolution solid state NMR was used to characterise the blends with respect to structure-mobility-compatibility using magic angle spinning with cross-polarisation and high power hydrogen decoupling and measurements of the proton spin-lattice relaxation time in the rotating frame. Miscibility between polymer chains was also studied by two-dimensional hydrogen ion/carbon-13 shift correlation (HETCOR). 21 refs.

Item 211 Polymer Recycling 3, No.4, 1997/1998, p.263-7 PROCEDURES FOR THE COMPOSITIONAL ANALYSIS OF REINFORCED POLYESTER RECYCLATE Bream C E; Hornsby P R Brunel University In order to consider effective strategies for the recovery and reuse of plastics recyclates, a quantitative method is described for the characterisation of polyester-based moulding compounds. Analytical procedures are described for the quantification of fibre, filler and fire retardant contents in polyester moulding compounds containing calcium carbonate filler, glass fibre reinforcement, and aluminium hydroxide flame retardant. 3 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.742796

Accession no.743489

Item 212 High Performance Plastics Aug.1999, p.10 IDENTIFICATION OF PLASTICS IN WASTE

Item 210 Macromolecules 32, No.11, 1st June 1999, p.3671-3 LIQUID ADSORPTION CHROMATOGRAPHY OF COPOLYMERS: MOLAR MASS (IN)DEPENDENT RETENTION Berek D Slovak Academy of Sciences

A review is presented of the methods used in the identification of plastics waste prior to recycling operations, which was published in International Polymer Science and Technology, and translated from a Polish source. Rapid spectroscopic methods are indicated, and their use in packaging and automotive recycling are discussed.

BRAZIL

Liquid adsorption chromatography with a continuous solvent gradient elution was shown by several previous authors to be capable of separating random and graft copolymers according to their chemical composition, with their molar masses not playing an important role. A tentative explanation of this finding is presented. It is assumed that the copolymer species travel along the column with a velocity which exactly corresponds to that of the eluent composition, exhibiting a displacing power just necessary to prevent a fast progress of the macromolecules due to their exclusion. Under specific conditions, retention of macromolecules at this adsorption promoting ‘barrier’ depends almost exclusively on the copolymer composition and not on its molar mass. This hypothesis is based on the mechanism of the recently-

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EASTERN EUROPE; POLAND

Accession no.742675 Item 213 Journal of Polymer Science: Polymer Physics Edition 37, No.13, 1st July 1999, p.1485-94 GLASS TRANSITION AND MISCIBILITY IN BLENDS OF TWO SEMI-CRYSTALLINE POLYMERS: POLYARYL ETHER KETONE AND POLYETHER ETHER KETONE Woo E M; Tseng Y C Taiwan,National Cheng Kung University A study was made of the miscibility in the amorphous region of melt mixed blends composed of a novel polyaryl ether ketone (PK99) and PEEK using various methods,

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References and Abstracts

including optical microscopy, DSC, SEM, FTIR spectroscopy and wide-angle X-ray diffraction. Samples were physically aged in order to resolve any possible overlapping Tg’s but only one single Tg was detected over the entire composition range. No evidence for isomorphism was found and the crystal forms of the respective polymers remained distinct and unchanged by miscibility in the amorphous region. 14 refs. TAIWAN

Accession no.742306 Item 214 Applied Spectroscopy 53, No.6, June 1999, p.672-81 POST-CONSUMER PLASTIC IDENTIFICATION USING RAMAN SPECTROSCOPY Allen V; Kalivas J H; Rodriguez R G Idaho,State University The suitability of Raman spectroscopy, when used with K-nearest neighbours, library searching or cyclic subspace regression, for computerised classification of postconsumer plastics was evaluated. Plastics investigated were PETP, PP, PS, PVC, HDPE AND LDPE. Modifications were made to the original cyclic subspace regression algorithm for modelling multiple sample properties and the adapted algorithm employed to directly compare the mechanisms of principal component regression and the PLS2 form of partial least-squares. It was found that Raman spectroscopy could be used to identify both HDPE and LDPE. 33 refs. USA

Accession no.741260 Item 215 Applied Spectroscopy 53, No.5, May 1999, p.557-64 COMPARISON OF NEAR-INFRARED AND RAMAN SPECTROSCOPY FOR THE DETERMINATION OF CHEMICAL AND PHYSICAL PROPERTIES OF NAPHTHA Min-Sik Ku; Hoeil Chung SK Corp.

Sano K; Shimoyama M; Ohgane M; Higashiyama H; Watari M; Tomo M; Ninomiya T; Ozaki Y Kwansei-Gakuin,University; Hyogo,Prefectural Police Headquarters; Yokogawa Electric Co. FTIR spectra were measured for pellets of sixteen kinds of LLDPE with short branches and one kind of PE without any branch to explore the effects of the branches on the physical properties and the Raman spectrum. Partial least squares analysis regression was applied to the Raman spectra after multiplicative scatter correction to propose a calibration model that predicts the density of LLDPE. 38 refs. JAPAN

Accession no.740338 Item 217 Journal of Coatings Technology 71, No.893, June 1999, p.53-60 INVERSE GAS CHROMATOGRAPHY, SURFACE PROPERTIES, AND INTERACTIONS AMONG COMPONENTS OF PAINT FORMULATIONS Ziani A; Xu R; Schreiber H P; Kobayashi T Ecole Polytechnique de Montreal; Nippon Paint Co. Inverse gas chromatography analysis at very high dilution and at finite concentrations of probe injection was carried out on a series of polymers and pigments used in paint formulations. Values of dispersion surface energies, and of acid-base interaction parameters were obtained for the materials, and pair interaction parameters were calculated from the results. The dispersion stability of each pigment/ polymer combination was measured and correlated with the acid-base interaction parameters of the materials, and is shown to justify the availability of fundamental thermodynamic interaction data to optimise performance aspects of protective coatings. 23 refs. CANADA; JAPAN

Accession no.739845

Accession no.740339

Item 218 Analytical Chemistry 71, No.10. 15th May 1999, p.2037-45 ANALYSIS OF POLYMERIC FLAME RETARDANTS IN ENGINEERING THERMOPLASTICS BY PYROLYSIS GAS CHROMATOGRAPHY WITH AN ATOMIC EMISSION DETECTOR Wang F C Y Dow Chemical Co.

Item 216 Applied Spectroscopy 53, No.5, May 1999, p.551-6 FOURIER TRANSFORM RAMAN SPECTRA OF LINEAR LOW-DENSITY POLYETHYLENE AND PREDICTION OF THEIR DENSITY BY MULTIVARIATE DATA ANALYSIS

Halogen-containing polymeric flame retardants in engineering thermoplastics were analysed by pyrolysis gas chromatography(Py-GC) with an atomic emission detector(AED) and a mass selective detector(MSD). The AED was very effective in monitoring halogen-containing pyrolysates after Py-GC. The type of polymeric flame retardant used in thermoplastics could be identified by peak pattern recognition through an AED halogen element

Near-infrared and FTIR Raman spectroscopy were compared and evaluated for the quantitative analysis of naphtha using partial least-squares regression. 19 refs. SOUTH KOREA

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trace. A set of thermoplastic resins containing different brominated polymeric flame retardants was studied. After generation of the pyrogram by Py-GC/AED, those pyrolysates produced from polymeric flame retardants were identified by MSD analysis of a complex total ion chromatogram generated by the thermoplastic resins. The results demonstrated the effectiveness of the AED in the tasks of specific element monitoring and component pattern recognition. The advantages and disadvantages of using the AED are also discussed. 11 refs. USA

Accession no.738049 Item 219 ACS, Polymeric Materials Science and Engineering. Vol.76. Conference proceedings. San Francisco, Ca., Spring 1997, p.128-9. 012 ATOMIC FORCE MICROSCOPY STUDY OF INTRAOCULAR LENS IMPLANTS TOPOGRAPHY AND SURFACE PROPERTIES Kowalewski T; Ravi V N Washington,University; St.Louis,Veterans Affairs Medical Center (ACS,Div.of Polymeric Materials Science & Engng.) Cataracts are one of the most common causes of worldwide blindness. They are presently corrected by surgery in which the natural cataractous lens is replaced by a synthetic intraocular lens. Successful visual rehabilitation is not only a function of patients’ health and the surgical technique, but it also depends on the optical, mechanical and bioperformance of the intraocular lens. Visual deterioration after surgery has been attributed to cellular debris deposited on the lens surface and capsular opacification resulting from inflammation. Although the exact sequence of events that take place when an implant is exposed to the ocular environment in vivo is not known, protein adsorption, complement activation and cellular adhesion have been implicated and believed to be influenced by the surface properties of the implants. The surface characteristics (surface topography and viscoelasticity) of intraocular lenses are investigated using tapping-mode atomic force microscopy. 9 refs. USA

Accession no.737604 Item 220 Polymer 40, No.17, 1999, p.4763-7 MODULATED DIFFERENTIAL SCANNING CALORIMETRY: 14. EFFECT OF MOLECULAR INTERACTIONS ON GLASS TRANSITION BEHAVIOUR AND INCREMENT OF HEAT CAPACITY IN MISCIBLE POLYMER BLENDS Song M; Hourston D J; Pollock H M; Hammiche A Loughborough,University; Lancaster,University Modulated differential scanning calorimetry was used to study miscible polymer blends. The blends studied

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were poly(vinyl acetate)/poly(methyl acrylate), poly(phenylene oxide)/PS and two poly(styrene-coacrylonitrile)/PMMA blends, the last two containing different acrylonitrile contents. Specific molecular interactions determined whether the glass transition temperature and the increment of heat capacity versus composition showed positive or negative deviations from linearity for the blend systems. In the noninteracting system (poly(vinyl acetate)/poly(methyl acrylate)), the glass transition temperature and increment of heat capacity showed linear behaviour with composition. Thermodynamic theories for the observed results were discussed. 17 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.737361 Item 221 LCGC International 12, No.7, July 1999, p.432/6 QUANTITATIVE ANALYSIS OF POLY(METHYLMETHACRYLATE) IN DRUGS BY CURIE-POINT PYROLYSIS GAS CHROMATOGRAPHY Muguruma S; Uchino S; Oguri N; Kiji J Japan Analytical Industry Co.Ltd.; Tottori,University Curie-point pyrolysis gas chromatography was used for the quantitative analysis of residual synthetic adsorbent crosslinked PMMA used in drug purification. Levels of PMMA adsorbent below 0.15% in drug substances were successfully measured quantitatively by Py-GC using characteristic peaks that reflect the structure of the adsorbent, demonstrating that this analytical technique can be used to monitor compliance with the limit of 0.1% organic impurity in drug substances stipulated by ICH guidelines. 12 refs. JAPAN

Accession no.736647 Item 222 Journal of Applied Polymer Science 72, No.7, 16th May 1999, p.913-25 HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY OF EPOXY RESINS Fuchslueger U; Rissler K; Stephan H; Grether H J; Grasserbauer M Ciba Specialty Chemicals Inc.; Vienna,Technical University The application of liquid chromatography coupled to mass spectrometry for the analysis of epoxy resins was shown in two examples. Electrospray (ESI) and atmospheric pressure chemical ionisation (APCI) were compared with respect to the ionisation of diglycidyl ether of bisphenol A (DGEBA)-based epoxy resins. Byproducts in a typical modified solid DGEBA-based

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epoxy resin and in a new weatherable crosslinker for powder coating applications were characterised and discussed. 26 refs. AUSTRIA; SWITZERLAND; WESTERN EUROPE

Accession no.734831 Item 223 Journal of Adhesion Science and Technology 13, No.5, 1999, p.629-45 ADHESION CHARACTERISATION OF PROTECTIVE ORGANIC COATINGS BY ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY Deflorian F; Fedrizzi L Trento,University This review describes in detail the influences on adhesion of different pretreatments or organic coatings, considering aluminium, galvanised steel, and stainless steel substrates, and it was shown that the information obtained using an electrochemical approach can be used for adhesion evaluation, with particular attention to monitoring of adhesion in an aqueous environment, which is the most detrimental for protective organic coatings. 40 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.733531 Item 224 Macromolecular Chemistry & Physics 200, No.5, May 1999, p.1134-42 POSSIBILITIES AND LIMITS OF PHOTON CORRELATION SPECTROSCOPY IN DETERMINING POLYMER MOLECULAR WEIGHT DISTRIBUTIONS Faraone A; Magazu S; Maisano G; Villari V; Maschio G Messina,University The effect of concentration and polydispersity on the collective diffusion coefficient(Dc) evaluated using photon correlation spectroscopy was investigated on PMMA in acetone solutions. The concentration dependence of the Dc followed a linear regression law, the slope being fairly independent of polydispersity, molec.wt. and temp. The diffusion coefficient at infinite dilution obeyed a given scaling law. The inversion of the scattered intensity autocorrelation data by the regularisation method CONTIN permitted the evaluation of the MWD function of the polymeric samples. Although this algorithm gave valuable information on average amounts or on the widths of the distribution, it had limited resolution power. A comparison with the results obtained by size exclusion chromatography was therefore carried out for a set of samples having monomodal and bimodal distribution functions. 22 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

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Item 225 Coloring Technology for Plastics. New York, N.Y., Plastics Design Library, 1999, p.197207. 52 MEASURING STABILISERS IN PIGMENTED PLASTICS WITH NEAR-INFRARED SPECTROSCOPY Solera P; Nirsberger M; Castillo N Ciba Specialty Chemicals Corp. Edited by: Harris R M Near-infrared (NIR) spectroscopy has become a commonplace analytical tool in the plastics industry. NIR techniques have made quantification of many organic components in polymer processing easy and quick. The work presented outlines the methodology for using NIR to measure stabiliser levels in colour concentrates and natural polymer formulations. Advantages and limitations are considered as well as particle size and product form. 4 refs. USA

Accession no.732217 Item 226 Coloring Technology for Plastics. New York, N.Y., Plastics Design Library, 1999, p.1915. 52 PRACTICAL ANALYSIS TECHNIQUES OF POLYMER FILLERS BY FOURIER TRANSFORM INFRARED SPECTROSCOPY (FTIR) Coles B J; Hall C J Hauser Inc. Edited by: Harris R M The identification of polymers by FTIR is often complicated by the presence of fillers. However, for kaolin clay, FTIR analysis should be able to identify the filler and predict its concentration using a standard curve. The resulting percentage is more reliable than a simple ash, which may change the chemical composition of the filler. 2 refs. USA

Accession no.732216 Item 227 Pitture e Vernici 75, No.5, March 1999, p.7-8 English; Italian E.I.S. EVALUATION OF ATTACHED AND FREE POLYMER FILMS Castela A S; Simoes A M P Evaluation of the volume fraction of water in organic coatings in immersion is often made by electrochemical impedance spectroscopy, EIS, and based upon the evolution of the coating capacitance. Among the several models and equations proposed for this determination, the most frequently used is the Brasher equation. Most

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References and Abstracts

frequently these determinations are made with applied coatings, although studies can be found in the literature using free films. The behaviour of a commercial coating - PVC plastisol - is studied, both applied on a metallic substrate and as a free film. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.731759 Item 228 Journal of Thermal Analysis and Calorimetry 55, No.2, 1999, p.559-63 TG/FT-IR STUDIED OF POLY(VINYL CHLORIDE) BLENDS Pielichowski K Krakow,Technical University Thermogravimetry coupled with FTIR was used to investigate the stabilising action of 3-(2,4dibromophenylazo)-9-(2,3-epoxypropane)carbazole on the degradation of PVC. This secondary stabiliser increased the initial temperature of hydrogen chloride evolution (the main process responsible for PVC decomposition), thereby allowing its application for novel PVC systems with enhanced thermal stability. 10 refs. EASTERN EUROPE; POLAND

Accession no.731454 Item 229 Analytical Chemistry 71, No.9, 1st May 1999, p.1809-14 POLYMER ANALYSIS BY LIQUID CHROMATOGRAPHY/ELECTROSPRAY IONISATION TIME-OF-FLIGHT MASS SPECTROMETRY Nielen M W F; Buijtenhuijs F A Akzo Nobel Central Research Different liquid chromatography modes in polymer analysis were successfully interfaced with electrospray ionisation time-of-flight mass spectrometry in a single experimental set-up: the mass spectrometry data from size exclusion chromatography/mass spectrometry of PMMA were used as absolute calibration points in the size exclusion chromatography/refractive index chromatogram, and monomer mass and end groups were inferred from the isotopically resolved mass spectra. 44 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; WESTERN EUROPE

Accession no.731446 Item 230 Polymer Preprints. Volume 40. Number 1. March 1999. Conference proceedings. Boston, Ma., March 1999, p.226-7. 012 SURFACE MODIFICATION OF POLYSTYRENE STUDIED BY IR-VISIBLE SUM FREQUENCY

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GENERATION SPECTROSCOPY Zhang D; Dougal S; Yeganeh M S Exxon Research & Engineering Co. (ACS,Div.of Polymer Chemistry) The effects of UV light and oxygen plasma on PS surfaces is investigated using SFG spectroscopy. The observed spectral changes provide strong support for the photooxidation of the aromatic ring at the PS surface, as observed by the dramatic decrease in the aromatic C-H vibration during photo irradiation and plasma treatment. It is also found that the kinetics of the photooxidation of the PS surface, monitored by SFG, is much faster than similar process observed by other techniques, such as FTIR or SIMS. 13 refs. USA

Accession no.730043 Item 231 Polymer Composites 20, No.2, April 1999, p.314-20 CHARACTERISATION OF MIXED FIBRE NYLON COMPOSITES INCORPORATING COMPOSITE SCRAP Licea-Claverie A; Carrillo F J U; Alvarez-Castillo A; Castano V M Tijuana,Instituto Tecnologico; Zacatepec,Instituto Tecnologico; UNAM Recycling of engineering thermoplastics and their composites is discussed. A study on nylon-6,6 based composites with mixed glass fibre and carbon fibre reinforcement, including nylon composite scrap in their formulation, were reported. Several formulations were prepared by injection moulding and were characterised by stress-strain measurements, impact testing, simultaneous DTA and TGA, density measurements and SEM. Mechanical and thermal properties of the resulting composites are presented, discussed, and compared with a virgin standard composite. 26 refs. MEXICO

Accession no.729302 Item 232 Analytical Chemistry 71, No.7, 1st April 1999, p.1316-22 CHARACTERIZATION OF NATURAL RESIN SHELLAC BY REACTIVE PYROLYSIS-GAS CHROMATOGRAPHY IN THE PRESENCE OF ORGANIC ALKALI Wang L; Ishida Y; Ohtami H; Tsuge S; Nakayama T Nagoya,University; Gifu Shellac Manufacturing Co.Ltd. A method for determining the chemical composition of natural resin shellac was developed based on reactive pyrolysis-gas chromatography(Py-GC) in the presence of an organic alkali, tetramethylammonium hydroxide(TMAH). Py-GC using 25% TMAH aqueous

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solution permitted the highly sensitive determination of terpenic acids, aleuritic acid, several minor fatty acids and the wax components of shellac as their methyl derivatives on the resulting pyrograms with less than 2.0 % relative standard deviations without using any cumbersome pretreatment. The observed average distributions of each resin acid component determined by reactive Py-GC for shellac samples from India and Thailand showed that the average ratios among terpenic acids, aleuritic acid and the other fatty acids were about 53:24:14 for Indian shellac and 51:35:14 for Thailand shellac, respectively, suggesting a slightly significant difference. Clearer discrimination of the shellac samples from the two different countries was, however, achievable by applying principal component analysis for the mole percent distributions of all the acidic components determined by reactive Py-GC. 24 refs. INDIA; JAPAN; THAILAND

Accession no.727139 Item 233 ACS Polymeric Materials Science and Engineering. Fall Meeting 1997. Volume 77. Conference proceedings. Washington, D.C., 1997, p.594-5 .012 EFFECT OF SECOND DIMENSION SAMPLING RATE AND PARTICLE SIZE ON RESOLUTION AND RUN TIME IN TWO DIMENSIONAL LIQUID CHROMATOGRAPHY FOR THE ANALYSIS OF POLYMERS Murphy R E; Schure M R; Foley J P Rohm & Haas Co.; Villanova,University (ACS,Div.of Polymeric Materials Science & Engng.) The optimisation of a two dimensional high performance liquid chromatography (HPLC) (reverse phase liquid chromatography/gel permeation chromatography (GPC)) system for the analysis of low molecular weight polymers is described. A test mixture of polyethylene glycols and a commercial surfactant was used. The analysis time of the second dimension, GPC, was varied by using different columns. The columns had different particle sizes and lengths, and the two dimensional resolution was compared by varying the run time in the second dimension. Following the optimisation, it was possible to complete a two dimensional analysis in the time normally taken for a normal gradient HPLC run. It was established that conventional columns could be run with higher flow rates without a significant loss of resolution. The combination of shorter and smaller particle GPC columns resulted in lower sampling periods at lower flow rates than conventional columns. The highest sampling rate into the second dimension gave the best resolution. 7 refs. USA

Accession no.726180 Item 234 Shawbury, Rapra Technology Ltd., 1997, pp.315. 220.00. 30cms. 9922

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RAPRA COLLECTION OF INFRARED SPECTRA OF RUBBERS, PLASTICS AND THERMOPLASTIC ELASTOMERS. SECOND EDITION Sidwell J A This book provides a set of transmission and pyrolysate spectra of a comprehensive range of technically important rubber and plastics materials including copolymers and blends which are in current use. Materials are indexed under both polymer and trade name. Accession no.725345 Item 235 Polymer 40, No.12, 1999, p.3479-85 INVERSE GAS CHROMATOGRAPHIC CHARACTERIZATION OF POLY(ETHYLENE OXIDE) Al-Saigh Z Y Columbus,State University The inverse gas chromatography method was used to obtain the thermodynamic properties and the surface energy of a semicrystalline polymer, PEO. PEO was used as a stationary phase in the chromatographic column and 16 solutes with a different chemical nature were used as eluents. Alkanes showed endothermic interaction parameters and the molar heat of mixing in a temp. range of 70-130C. Acetates and alcohols showed better interactions with the PEO layer and butanol was found to be the best solvent for PEO among all solutes used. The variation in molec.wt. of PEO above 400 g/mol showed no apparent effect on the interaction coefficients. The dispersive contribution of the surface energy of PEO was measured as a function of temp., which ranged from 8.00 and 13.00 mJ/sq m, indicating a poor surface energy of PEO. 43 refs. USA

Accession no.721885 Item 236 Journal of Adhesion 68, Nos.1-2, 1998, p.117-42 QUANTIFICATION OF COATING ADHESION USING LASER INDUCED DECOHESION SPECTROSCOPY Meth J S; Sanderson D; Mutchler C; Bennison S J DuPont Co. A new technique, laser induced decohesion spectroscopy, is presented, which is capable of measuring the practical work of adhesion between a transparent polymer coating or substrate. A laser pulse directed onto the sample creates a blister at the transparent/opaque interface. The blister’s internal pressure depends on the laser pulse energy, and at a critical pressure the sample fractures, creating an annular debond similar to that obtained in the standard blister test. By measuring physical variables such as the

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References and Abstracts

curvature of the blister, and its radius and thickness, it is possible to deduce the practical work of adhesion. 19 refs. USA

Accession no.721348 Item 237 Journal of Adhesion Science and Technology 13, No.3, 1999, p.379-91 DETERMINATION OF THE ADHESION PROPERTIES OF AN ALKYD PIGMENTED COATING BY ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY Gonzalez J E G; Rosca J C M Gran Canaria,University Impedance measurements were performed in different frequency ranges at open circuit potential for an alkyd coating with titanium dioxide as a mineral pigment in 3% sodium chloride. The most probable impedance equivalent circuit method was considered for data analysis. The interpretation of the impedance spectra permitted the determination of water permeation, the formation of blisters, swelling of the coating, and the loss of adhesion. 17 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.721335 Item 238 ACS Polymeric Materials Science and Engineering.Fall Meeting 1997.Volume 77.Conference proceedings. Washington, D.C., 1997, p.48-9 012 QUANTITATION IN THE ANALYSIS OF OLIGOMERS BY HPLC WITH ELSD Trathnigg B; Kollroser M; Maier B; Berek D; Janco M Graz,Karl-Franzens-Universitat; Slovak Academy of Sciences (ACS,Div.of Polymeric Materials Science & Engng.) The influence of the operating parameters used when operating evaporative light scattering detectors in conjunction with high performance liquid chromatography for the characterisation of oligomers was investigated, using polyether samples. It was concluded that the instrument was useful because it provided gradient elution, however, very careful calibration was required to obtain reliable quantitative data. 16 refs. AUSTRIA; WESTERN EUROPE

Accession no.720839 Item 239 ACS Polymeric Materials Science and Engineering.Fall Meeting 1997.Volume 77.Conference proceedings. Washington, D.C., 1997, p.46-7 012 APPLICATION OF SEC AND HPLC TO THE CHARACTERIZATION OF POLYMERS, OLIGOMERS, AND SMALL MOLECULES USED IN COATINGS AND INKS

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Kuo C; Grieser M D; Robinson D Henkel Corp. (ACS,Div.of Polymeric Materials Science & Engng.) Applications are given of the use of size exclusion chromatography and high performance liquid chromatography for the characterisation of coatings systems which either use water as the major solvent or utilise low molecular weight polymers, oligomers, and reactive additives which are then reacted to produce high molecular weight and crosslinked films. 6 refs. USA

Accession no.720838 Item 240 ACS Polymeric Materials Science and Engineering.Fall Meeting 1997.Volume 77.Conference proceedings. Washington, D.C., 1997, p.35-6 012 LIQUID CHROMATOGRAPHY OF MACROMOLECULES UNDER LIMITING CONDITIONS OF SOLUBILITY: FIRST EXPERIMENTAL OBSERVATIONS Bartkowiak A; Hunkeler D; Murgasova R; Berek D Szczecin,Technical University; Swiss Federal Institute of Technology; Slovak Academy of Sciences (ACS,Div.of Polymeric Materials Science & Engng.) Liquid chromatography at the critical adsorption point (LC LCS) was investigated. The solubility of macromolecules, the sensitivity of LC LCS to such variables as the injection volume, concentration injected, mobile phase flow rate and mixing between the injection zone, were investigated, using polymethyl methacrylate (PMMA) and polyacrylamide standards. It is proposed that using tetrahydrofuran and n-hexane as eluents for PMMA, at the LC LCS, limited polymer insolubility or even local precipitation is combined with the size exclusion of macromolecules. 12 refs. EASTERN EUROPE; POLAND; SLOVAK REPUBLIC; SLOVAKIA; SWITZERLAND; WESTERN EUROPE

Accession no.720833 Item 241 ACS Polymeric Materials Science and Engineering.Fall Meeting 1997.Volume 77.Conference proceedings. Washington, D.C., 1997, p.31-2 012 LIQUID CHROMATOGRAPHY OF MACROMOLECULES AT THE CRITICAL ADSORPTION POINT: PROBLEMS AND PITFALLS Berek D; Janco M Slovak Academy of Sciences (ACS,Div.of Polymeric Materials Science & Engng.) The role of column packing pore size in liquid chromatography at the critical adsorption point was investigating using three silica gels and a series of polymethyl methacrylates (PMMA), using toluene, tetrahydrofuran (THF) or their mixtures as eluents.

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Toluene strongly promotes adsorption of PMMAs on the silica surface, whereas THF suppresses adsorption. It was established that the pore size of the column packings played an important role in liquid chromatography at the critical adsorption point. The column with the smallest pores largely determined the behaviour of the whole set. The feasibility of using silica gel as column packings for liquid chromatography at the critical adsorption point is questioned. 14 refs.

Dallas, Tx., Spring 1998, p.102-3. 012 COUPLED PROGRAMMED PYROPROBE-MASS SPECTROMETRY AND THERMOGRAVIMETRIC-MASS SPECTROMETRY Carraher C E; Molloy H M; Louda J W; Baker E Florida,Atlantic University; Florida,Center for Environmental Studies; Midwest Research Institute (ACS,Div.of Polymeric Materials Science & Engng.)

SLOVAK REPUBLIC; SLOVAKIA

In 1977, a thermogravimetric analysis unit was successfully coupled with a mass spectrophotometer, TGMS. More recently, a coupled programmed pyroprobemass spectrophotometry system, also utilising IR spectroscopy, was employed as a means of describing degradation sequences as a function of temperature. The application of these tools as a means to define polymer structure and degradation products is described. 9 refs.

Accession no.720831 Item 242 ACS Polymeric Materials Science and Engineering.Fall Meeting 1997.Volume 77.Conference proceedings. Washington, D.C., 1997, p.22-3 012 2D-LC OF FUNCTIONAL POLYETHERS Trathnigg B; Kollroser M; Parth M Graz,Karl-Franzens-Universitat (ACS,Div.of Polymeric Materials Science & Engng.) A combination of liquid chromatography under critical conditions using coupled density and RI detection in one dimension, and gradient high performance liquid chromatography in the second dimension, was used in the two-dimensional chromatographic analysis of the oligomers present in fatty alcohol ethoxylates. Full resolution was achieved. 6 refs. AUSTRIA; WESTERN EUROPE

Accession no.720827 Item 243 ACS Polymeric Materials Science and Engineering.Fall Meeting 1997.Volume 77.Conference proceedings. Washington, D.C., 1997, p.20-1 012 MOLECULAR CHARACTERIZATION OF COMPLEX POLYMERS BY COUPLED LIQUID CHROMATOGRAPHIC PROCEDURES Berek D Slovak Academy of Sciences (ACS,Div.of Polymeric Materials Science & Engng.) Size exclusion chromatography alone cannot characterise the constituents of complex polymer systems. Separation selectivity and characterisation of complex systems may be enhanced with liquid chromatographic (LC) methods utilising combinations of different separation mechanisms. These are termed coupled LC procedures. The applications of a variety of coupled LC procedures are discussed. 16 refs. SLOVAK REPUBLIC; SLOVAKIA

Accession no.720826 Item 244 ACS Polymeric Materials Science & Engineering, Spring Meeting 1998. Volume 78. Conference proceedings.

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Accession no.719193 Item 245 ACS Polymeric Materials Science & Engineering, Spring Meeting 1998. Volume 78. Conference proceedings. Dallas, Tx., Spring 1998, p.219-20. 012 SECONDARY TRANSITIONS IN POLYMERS PROBED BY DIFFERENTIAL SCANNING CALORIMETRY Bertolucci P R H; Harmon J P South Florida,University (ACS,Div.of Polymeric Materials Science & Engng.) The use of differential scanning calorimetry to identify secondary transitions in thermoplastics is studied. The temperature and breadth of the secondary transition are related to the those of the alpha transition in a variety of methacrylate, acrylate and styrene polymers, as well as polycarbonate. The effect of thermal history and the position and sharpness of these endothermic transitions is discussed. Some comparisons are made between this technique and results obtained via dielectric analysis and dynamic mechanical analysis obtained in the laboratory. 7 refs. USA

Accession no.718740 Item 246 Macromolecular Chemistry & Physics 200, No.2, Feb.1999, p.413-21 THERMAL PROPERTIES AND CRYSTALLISATION BEHAVIOUR OF POLYHYDROXYBUTYRIC ACID IN BLENDS WITH CHITIN AND CHITOSAN Ikejima T; Yagi K; Inoue Y Tokyo,Institute of Technology Films of blends of polyhydroxybutyric acid with chitin and chitosan were prepared as completely biodegradable

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References and Abstracts

polyester-polysaccharide composites. Crystallisation was examined using DSC. Data are given from FTIR and carbon 13 NMR. 31 refs. JAPAN

Accession no.716972 Item 247 Journal of Biomedical Materials Research (Applied Biomaterials) 48, No.1, 1999, p.5-8 EXTRACTABLE FREE MONOMERS FROM SELF-CURED DENTAL SEALANTS RESULTING FROM DISPENSING ERRORS Vaubert V M; Moon P C; Love B J Virginia,Polytechnic Institute HPLC experiments were performed on a series of selfcuring polybisglycidyl methacrylate dental sealants that were deliberately mismixed. The amount of extractable sealant under conditions of nonideal processing was measured. 13 refs. USA

Accession no.716163 Item 248 Macromolecular Rapid Communications 20, No.2, Feb. 1999, p.95-7 CURING OF MONOMER COMPOSITES. II. USE OF NMR TO MONITOR REAL TIME CURING DYNAMICS Martin S J; McBrierty V J; Dowling J; Douglass D C Dublin,Trinity College; Bausch & Lomb Inc. Details are given of a method for monitoring the realtime curing dynamics of composite monomers, exploiting site specific information provided by high resolution NMR. Data using polyvinylpyrrolidone, polyhydroxyethyl methacrylate and polybutylhydroxycyclohexyl methacrylate are compared with results from a computer simulation based on a multicomponent kinetic model. 7 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND; WESTERN EUROPE

Accession no.716161

systems under elongational interactions in polymer bilayer systems under elongational deformations and changes in potential energy, leading to determination of the work of adhesion. This research expands the scope of previous findings and provides a relationship between the C-H stretching vibrational energy changes for acrylic/PE, epoxy/PE, acrylic/PP, and epoxy/PP bilayer systems and the interfacial forces responsible for adhesion. 39 refs. USA

Accession no.715972 Item 250 Analytical Chemistry 71, No.2, 15th Jan.1999, p.468-75 IDENTIFICATION AND DETERMINATION OF CROSSLINKERS IN CROSSLINKED POLYVINYLPYRROLIDONE(PVP) BY PYROLYSIS-GAS CHROMATOGRAPHY(GC)/ MASS SPECTROMETRY(MS) Cheng T M H; Malawer E G International Specialty Products Pyrolysis-GC and pyrolysis-GC/MS were used to identify and quantify specific nitrogen-containing crosslinker compounds incorporated into the structures of crosslinked PVP polymers which appeared to be identical by FTIR spectroscopy. The pyrolyser regenerated and volatilised specific crosslinkers which could be distinguished from other pyrolysate compounds by either peak retention time or mass spectral release. Individual compounds studied included 3-ethylidene-1-vinyl-2-pyrrolidone, 3,3'ethylidenebis(1-vinyl-2-pyrrolidone) and N,N’divinylimidazolidone. In general, the level of specific crosslinkers in various commercial products ranged from 1.8 to 2.5% w/w. The effect of pyrolysis temp. on this level varied with the crosslinkers studied. The crosslinker content obtained by this technique correlated with the swell volume data for a specific series of crosslinked PVP samples made with a single crosslinker and having similar particle size distributions. The pyrolysis methodology could not distinguish the level of crosslinker which was incorporated as a pendant functionality from that portion which was incorporated through both vinyl groups. 26 refs. USA

Item 249 Journal of Adhesion Science and Technology 13, No.1, 1999, p.19-34 RHEO-PHOTOACOUSTIC (RPA) FTIR SPECTROSCOPIC STUDIES OF THE ADHESION OF THERMOSETS TO POLYOLEFINS Pennington B D; Urban M W North Dakota State University

Accession no.715578

Rheophotoacoustic FTIR analysis and previously developed theory were utilised in an attempt to correlate the molecular level interactions in polymer bilayer

Two EVA materials with distinct vinyl acetate ratios are studied by nuclear magnetic resonance using solution and solid techniques. These studies are made in order to obtain a

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Item 251 Polymer Testing 17, No.8, Dec.1998, p.533-41 NMR STUDY OF COMMERCIAL POLYETHYLENE-CO-VINYL ACETATE de Souza C M G; Tavares M I B Rio de Janeiro,Cidade Universitaria

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relation between the structure-properties-mobility and this response can be utilised in order to have precise information for new applications as well as better understanding of the material behaviour. The results show that these polymers present characteristic mobilities as a function of vinyl acetate in the copolymer. Thus, as the quantity of vinyl acetate increases the dyads and tryads distribution and the molecular mobility in the copolymer change, as a consequence of the different commercial applications. 13 refs. BRAZIL

Accession no.714141 Item 252 Journal of Thermal Analysis and Calorimetry 54, No.2, 1998, p.565-76 METHOD FOR ANALYSIS OF THE MEASURED CURVES OF TEMPERATURE-MODULATED DIFFERENTIAL SCANNING CALORIMETRY(TMDSC) INVESTIGATION IN THE MELTING REGION OF POLYMERS Schawe J E K; Bergmann E; Winter W Ulm,University; IFA GmbH The measured signal of the TMDSC was examined for the case of polymer melting. Fourier transform analysis was used to evaluate the data, the resulting information being the amplitude and the phase shift of the first harmonic of the periodic heat flow component. It was shown that this procedure was not sufficient for quantitative discussions if deviations from the symmetric curve shape occurred in the measured heat flow curves. For polymer melting, it was shown that asymmetric curves would be measured if the experimental temp. amplitude was too large. 15 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.713454 Item 253 Journal of Thermal Analysis and Calorimetry 54, No.2, 1998, p.477-99 APPLICABILITY OF TEMPERATUREMODULATED DIFFERENTIAL SCANNING CALORIMETRY(TMDSC) TO POLYMERIC SYSTEMS. GENERAL THEORETICAL DESCRIPTION BASED ON THE FULL HEAT CAPACITY FORMULATION Scherrenberg R; Mathot V; Steeman P DSM Research An overview is presented of the different aspects of TMDSC, using a general theoretical description based on the full heat capacity formulation. It is demonstrated that processes studied with the aid of TMDSC can be simply classified into three distinct regimes, depending on the time scale and the susceptibility of the process to the temp. modulation. 47 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; WESTERN EUROPE

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Item 254 Muanyag es Gumi 34, No.12, 1997, p.A12-4 Hungarian ASSESSMENT OF THE THERMAL HISTORY OF EXTRUDED UPVC Marossy K BorsodChem Rt. The paper deals with the investigation by differential scanning calorimetry of extruded rigid PVC formulations. The DSC traces of processed UPVC depend on the thermal history of the melt. The DSC tests can be used to estimate extrusion conditions e.g. of failed products. 16 refs. Articles from this journal can be requested for translation by subscribers to the Rapra produced International Polymer Science and Technology. EASTERN EUROPE; HUNGARY

Accession no.713264 Item 255 Surface Coatings International 82, No.1, Jan.1999, p.26-30 USE OF ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY FOR THE DETERMINATION OF THE PROTECTIVE PROPERTIES OF SOLVENT- AND WATER-BASED PAINT SYSTEMS Al-Hashem A; Carew J A; Hasan A Kuwait,Institute for Scientific Research In this work, electrochemical impedance spectroscopy was used to evaluate the corrosion protection properties of the solvent-based coatings and water-based coating systems currently being proposed for use in the industrial installations in the Arabian Gulf region. Evaluation of corrosion damage levels for three coating systems after 90 day immersion in 0.5M NaCl was performed using the EIS and visual observations. 22 refs. KUWAIT

Accession no.713236 Item 256 Journal of Materials Science 33, No.19, 1st Oct.1998, p.4721-5 RAMAN SPECTRA OF HIGH MODULUS POLYETHYLENE FIBRES BY RAMAN MICROSCOPY Lu S; Russell A E; Hendra P J Southampton,University Raman microscopy was used to analyse a series of high modulus PE fibres, relating the Raman scattering anisotropy to the mechanical performance of the filaments. Measurements of the band intensity ratio of the fibres were made and related to their Young’s modulus. This relationship is useful in morphological studies of PE fibres. 10 refs.

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References and Abstracts

EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.711133 Item 257 Applied Spectroscopy 52, No.12, Dec.1998, p.1498-504 MEASUREMENT OF ORIENTATION AND CRYSTALLINITY IN UNIAXIALLY DRAWN POLY(ETHYLENE TEREPHTHALATE) USING POLARISED CONFOCAL RAMAN MICROSCOPY Everall N J ICI Wilton Research Centre Polarised confocal Raman microscopy was used to measure molecular orientation in uniaxially drawn PETP films, prepared with draw ratios from 1 to 3.5. The orientation of both polarised Raman microscopy and polarised attenuated total reflection IR spectroscopy. Crystallinity profiles were measured through the thickness of the film samples and compared with the orientation gradients existing in the films. This procedure was to determine whether the intuitive assumption that orientation and crystallinity would be positively correlated actually holds true on the microscopic scale for these samples. 18 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Details are given of the range of physical and chemical properties of flame-sprayed ethylene-methacrylic acid copolymer following different processing conditions. Coatings were produced at a range of specific temperatures by varying the propane flow rate and gun traverse rate. Coatings were scanned using dielectric relaxation spectroscopy. 24 refs. AUSTRALIA; USA

Accession no.709520 Item 260 Polymer Journal (Japan) 30, No.10, 1998, p.771-4 CRYSTALLITE SIZES AND LATTICE DISTORTIONS OF GEL-SPUN ULTRA-HIGH MOLECULAR WEIGHT POLYETHYLENE FIBRES Xiao-Ping Hu; You-Lo Hsieh California,University A detailed method is reported for deriving the lattice distortions and crystallite sizes of UHMWPE fibres using a full wide angle X-ray diffraction patterns. The instrumental broadening and the background scattering is represented by a binomial. A discussion is included about the diffraction trace, peak assignments, and unit cell dimensions. 26 refs. USA

Accession no.711041

Accession no.709342

Item 258 Plasticheskie Massy (USSR) No.3, 1997, p.30-3 Russian BREAKDOWN OF AMMONIUM SALTS WITH REFERENCE TO THEIR INTRODUCTION INTO WOOD-BASED COMPOSITES Vigdorovich A I; Efremov V N

Item 261 Chinese Journal of Polymer Science 16, No.4, 1998, p.332-8 DETECTION OF TG BY MODULATED DIFFERENTIAL SCANNING CALORIMETRY Rui Song; Jing Chen; Jingui Gao; Xin Lin; Qingrong Fan Chinese Academy of Sciences

The possibility was studied of using ammonium salts as plasticisers for wood-based composites, and the breakdown of the ammonium salts during heating was studied by differential thermal gravimetry. 15 refs. Articles from this journal can be requested for translation by subscribers to the Rapra produced International Polymer Science and Technology.

The glass transition of PETP samples which were subjected to solvent induced crystallisation (SINC) was investigated by modulated differential scanning calorimetry (MDSC) and density measurements. The differential heat capacity signal from MDSC was used to monitor the SINC process. 16 refs. CHINA

Accession no.709335

RUSSIA

Accession no.710456 Item 259 Polymer Engineering and Science 38, No.11, Nov.1998, p.1873-81 PHYSICAL AND RELAXATION PROPERTIES OF FLAME-SPRAYED ETHYLENEMETHACRYLIC ACID COPOLYMER Brogan J A; Berndt C C; Simon G P; Hewitt D Stony Brook,University; Monash,University

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Item 262 Journal of Applied Polymer Science 71, No.1, 3rd Jan.1999, p.1-6 MICROWAVE PLASMA REACTIONS OF IMIDAZOLE ON POLY(VINYL CHLORIDE) SURFACES: A SPECTROSCOPIC STUDY Schmitt B R; Heung Kim; Urban M W North Dakota State University A closed-system microwave plasma reactor was used to react imidazole molecules to PVC surfaces. Newly created

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surfaces were analysed using ATR FTIR spectroscopy. Surface reactions on PVC were heavily dependent on a prior thermal history of the PVC substrate. A mechanism for the PVC-imidazole reactions was also presented. The PVC was useful as an implant for biomedical applications. 10 refs. USA

Accession no.709309 Item 263 Applied Spectroscopy 52, No.11, Nov.1998, p.1483-7 SAMPLING CONSIDERATIONS FOR FTRAMAN SPECTROSCOPY OF POLYMERS AND SOLUTIONS Barrerra B A; Sommer A J Miami,University Details are given of the determination of apparent absorption coefficients and optimal sample thickness of PE, PETP, cellulose, and cyclohexane by FT-Raman analysis. A relationship was developed that permits the optimal sample thickness for FT-Raman measurements to be determined by measuring the absorbance spectrum of a sample whose thickness is known. Results are discussed in the context of scattering theory, sampling considerations, and spectral artifacts. 9 refs. USA

Accession no.709038 Item 264 Journal of Applied Polymer Science 71, No.3, 18th Jan.1998, p.371-5 PROPYLENE OLIGOMERS: EXTRACTION METHODS AND CHARACTERISATION BY FTIR, HPLC, AND SEC El Mansouri H; Yagoubi N; Scholler D; Feigenbaum A; Ferrier D INRA Details are given of the isolation of propylene oligomers from polymer matrix by dissolution precipitation and Soxhlet methods. Characterisation was undertaken by FTIR, UV spectroscopy, HPLC, and GPC. Data were used to explain their behaviour toward packaged food products in PP packaging. 18 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.708984 Item 265 European Polymer Journal 34, No.12, Dec.1998, p.1817-28 CURING OF POLYMER COMPOSITES. I. NMR CHARACTERIZATION OF COMPONENT MONOMERS Martin S J; O’Brien J E; Dowling J; McBrierty V J Dublin,Trinity College; Bausch & Lomb Inc.

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The use of NMR to probe the in-situ curing of monomer mixtures commonly encountered in the manufacture of contact lenses was studied. Spectral lines were identified which monitored curing with time of individual components in the monomer mix. This information can aid in gaining an understanding of the overall curing dynamics and provide important guidance in establishing suitable protocols in the manufacturing process. As a precursor to this goal, several commonly-used component materials were characterised by high resolution proton and carbon-13 NMR spectroscopies. The efficacy of the overall procedure is demonstrated. 20 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND; WESTERN EUROPE

Accession no.706520 Item 266 Polimeros: Ciencia e Tecnologia 8, No.1, Jan./March 1998, p.46-53 Portuguese THERMAL STABILITY OF POLYETHYLENE TEREPHTHALATE PACKAGING: DETERMINATION OF OLIGOMERS Freire M T de A; Reyes F G R; Castle L Campinas,Universidade Estadual; UK,Min.of Agriculture,Fisheries & Food PETP food packaging materials were subjected to different heating conditions (50 minutes at 120-230C), and oligomers were identified by HPLC coupled with mass spectrometry and used as a parameter for evaluating the thermal stability of PETP. Small changes in oligomer distribution were observed only for samples heated at 230C, suggesting that PETP was thermally stable under the heating conditions employed. The results also suggested the suitability of PETP as a food packaging material for use in conventional and microwave ovens, and for secondary recycling under controlled conditions. 28 refs. BRAZIL; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.706082 Item 267 Journal of Thermal Analysis and Calorimetry 52, No.2, 1998, p.261-74 THERMAL ANALYSIS OF SOME ENVIRONMENTALLY DEGRADABLE POLYMERS Day M; Cooney J D; Shaw K; Watts J Canada,National Research Council The thermal characteristics of a series of degradable polymers for use in commercial composting facilities was investigated using TGA and DSC. Phase changes associated with some of the polymers investigated may cause problems in the interpretation of data from composting degradation studies. Several biodegradable

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References and Abstracts

polymers were observed to have melt transitions at temperatures similar to those found in a composting environment. 19 refs. CANADA

Accession no.705674 Item 268 Journal of Applied Polymer Science 70, No.12, 19th Dec.1998, p.2457-61 NUCLEAR MAGNETIC RESONANCE STUDY OF COMMERCIAL POLY(VINYL ACETATE) De Souza C M G; Tavares M I B Rio de Janeiro,Universidade Federal The commercial poly(vinyl acetate) bulk was studied by NMR at solution and solid state to understand the behaviour of this polymer to obtain information on structure, sample molecular mobility, and heterogeneity. To analyse the behaviour of this polymer, NMR techniques were chosen, such as carbon-13 solution, magic angle spinning, cross-polarisation/magic angle spinning, proton spin-relaxation time in the rotating frame parameter and dipolar dephasing experiment. 13 refs. BRAZIL

Accession no.705529 Item 269 Journal of Thermal Analysis and Calorimetry 52, No.1, 1998, p.145-55 German THERMOANALYTICAL CHARACTERISING UV-CURED POLYMER FILMS Hosselbarth B; Friese K; Geyer W Institut fuer Oberflaechenmodifizierung eV; LeipzigHalle Ltd.; Umweltforschungzentrum Thermooxidative and thermomechanical stabilities of radiation-cured acrylates and epoxides were examined by TGA, DMA and DSC. The polymeric trifunctional acrylates PETIA, TMPTA and THEIC displayed the highest temperatures of onset of degradation. The high crosslinking density of the films resulted in an almost temperature-independent complex E-modulus, as measured by DMA. With increasing degree of ethoxylation or propoxylation of the monomers, decreases in thermal stability and strength were found. For difunctional polymeric acrylates and epoxides, the TG temperature was measured. The average degree of curing of UV-cured epoxy films could be determined from the temperature of the maximum in the loss modulus. 13 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.705282 Item 270 Journal of Thermal Analysis and Calorimetry 52, No.1, 1998, p.131-43 German

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DETERMINATION OF VINYL ACETATE CONTENT IN EVA COPOLYMERS. FACILITIES AND LIMITS OF APPLICATIONS OF MASS SPECTROMETRY ANALYSIS METHODS Haussler L; Pompe G; Albrecht V; Voigt D Dresden,Institut fuer Polymerforschung Ethylene-vinyl acetate copolymers were investigated by simultaneous thermal analysis and pyrolysis gas chromatography. Both devices were coupled to a mass spectrometer. Calibration with polyvinyl acetate led to sufficient accuracy in relation to the vinyl acetate content, because of the linear calibration plot. Quantitative determination of vinyl acetate was carried out at both 500 and 700 C. The calibration plot was linear provided that the mass of vinyl acetate did not exceed a critical value. 18 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.705281 Item 271 Composites Science & Technology 58, No.10, 1998, p.1641-7 CHEMICAL ANALYSIS OF A FIELD-FAILED COMPOSITE SUSPENSION INSULATOR Chughtai A R; Smith D M; Kumosa M S Denver,University The type of corrosive environment responsible for brittle fracture of suspension composite insulators was established. A series of FTIR experiments was performed to identify chemical functionalities formed during the degradation process of composite insulators affected by brittle fracture. It was shown that the brittle fracture process was caused by the formation of nitric acid either outside or inside an insulator leading to stress corrosion cracking of the glass/polymer composite rod material. Nitrate was detected on the composite fracture surfaces inside a 115 kV suspension composite insulator which failed in service by brittle fracture. 17 refs. USA

Accession no.705241 Item 272 International Journal of Adhesion & Adhesives 18, No.5, 1998, p.319-31 LOW RESOLUTION PULSED NMR AND ULTRASOUND STUDY TO MONITOR THE CURE OF AN EPOXY RESIN ADHESIVE Cocker R P; Chadwick D L; Dare D J; Challis R E Keele,University; Manchester,Metropolitan University The cure of an epichlorohydrin-bisphenol A resin and curing agent containing a primary diamine and an amidopolyamine was studied using two complementary techniques, low resolution pulsed NMR spectroscopy and measurement of pulsed broad bandwidth ultrasound propagation velocity and absorption changes. The two

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techniques independently gave a similar picture of the cure process, predicting cure events at the same times. The results obtained indicated that the cure followed distinct phases, i.e. an initial liquid stage where short polymer chains were formed, followed by a second stage where longer molecules developed, a third stage where crosslinking between chains occurred and the adhesive began to solidify, and a final stage when solidification was completed. 19 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.704884 Item 273 Polymer Degradation and Stability 62, No. 1, Oct. 1998, p.41-8 MECHANISMS OF THERMAL DEGRADATION OF A POLYESTER FLAME-RETARDED WITH ANTIMONY OXIDE/BROMINATED POLYCARBONATE STUDIED BY TEMPERATURE-PROGRAMMED ANALYTICAL PYROLYSIS Sato H; Kondo K; Tsuge S; Ohtani H; Sato N Nagoya,University; Toray Research Center Inc. Thermal degradation of a flame-retarded PBTP consisting of PBTP and a synergistic flame-retardant system based on brominated polycarbonate (copolycarbonate containing units from bisphenol A and tetrabrominated bisphenol A plus tribromophenoxy end groups) and antimony trioxide was studied by means of various temperature-programmed analytical pyrolysis techniques such as temperature-programmed pyrolysis-mass spectrometry, temperature-programmed pyrolysis-atomic emission detection and temperature-programmed pyrolysis-gas chromatography. During the degradation of the flame-retarded PBTP, brominated phenols were first observed to evolve at temperatures slightly lower than those for the flammable product evolution from the substrate polymer PBTP, followed by the evolution of hydrogen bromide over the whole range of degradation temperatures for the substrate polymer. These degradation processes were closely related to the synergistic effects of antimony trioxide on the decomposition of brominated polycarbonate in the flame-retardant system to promote the thermal degradation of brominated polycarbonate at lower temperatures than those for pure brominated polycarbonate. Furthermore, the evolution of the flame poisoning antimony tribromide formed through the reaction between brominated polycarbonate and antimony trioxide could also be monitored directly by temperatureprogrammed pyrolysis techniques. On the basis of the data obtained by these temperature-programmed pyrolysis techniques, the thermal degradation of the flame-retarded PBTP and synergistic flame-retarding mechanisms are discussed. 10 refs. JAPAN

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Item 274 Revista de Plasticos Modernos 74, No.495, Sept.1997, p.255-61 Spanish FTIR SPECTROPHOTOMETRY FOR THE DETECTION OF MICROSTRUCTURAL CHANGES IN A POLYPROPYLENE/ POLYETHYLENE COPOLYMER CAUSED BY ARTIFICIAL AGEING Romeu J; Pages P; Carrasco F Cataluna,Universidad Politecnica; Girona,Universidad A study was made of microstructural changes occurring in blue and red samples of an ethylene-propylene copolymer exposed to artificial ageing in a Xenotest chamber for up to 5000 hours. The effects of ageing were quantified by Fourier transform IR spectrophotometry. By calculating the reduced absorption in selected spectral bands, it was possible to detect oxidation and chain scission reactions and variations in isotacticity which differed in the differently coloured specimens. 8 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.702522 Item 275 Journal of Applied Polymer Science 70, No.7, 14th Nov.1998, p.1307-10 MULTIDIMENSIONAL SPECTROMETRY AND MAPPING Fateley W G; Deverse R A; Hammaker R M Kansas State University A new inexpensive approach is described for mapping molecular structure in polymeric materials which includes the combination of interferometers and Hadamard transform techniques to perform multidimensional spectometry and mapping. 17 refs. USA

Accession no.702159 Item 276 Journal of Materials Science.Materials in Medicine 9, No.9, Sept.1998, p.529-33 INVESTIGATION OF GLASS-IONOMER CEMENTS USING DIFFERENTIAL SCANNING CALORIMETRY Khalil S K H; Atkins E D T Bristol,University Six commercial glass-ionomer cements commonly used for various dental applications were investigated using DSC. Heat flow behaviour and heat capacity of the cements were measured during isothermal (at 37 C) setting reactions. All materials underwent an exothermic setting process, but with different enthalpies of reactions and different heat capacities; there were no remaining endoor exothermic reactions after the setting of the cement.

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References and Abstracts

All materials examined were effective thermal insulators. 18 refs.

Popovici D; Sacher E; Meunier M Montreal,Ecole Polytechnique

EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Teflon, type AF1600, which contains perfluorinated dioxole rings, was found to suffer significant degradation when exposed to X-rays whilst undergoing investigation by X-ray photoelectron spectroscopy. The degradation mechanism was significantly different to that of fluoropolymers which contain only carbon and fluorine. It was established that oxygen was at least as twice as susceptible as fluorine, and that the amounts of oxygen loss were equal to those of fluorine. Oxygen could be degraded by the breaking of only one bond, the oxygen then forming a free radical. The free radicals produced by scission of carbon-carbon bonds participated in reactions leading to degradation and crosslinking. 9 refs.

Accession no.702142 Item 277 Journal of Materials Science 33, No.14, 15th July 1998, p.3511-7 MOLECULAR ORGANISATION IN STRUCTURAL PVDF Glennon D; Cox P A; Nevell R T; Nevell T G; Smith J R; Tsibouklis J; Ewen R J Portsmouth,University; West of England,University Poly(vinylidene fluoride) containing 10% dibutyl sebacate plasticiser, as used in the construction of flexible oil and gas pipelines, was exposed to raised temperatures for prolonged periods of time, to acid etching and to various tensile deformation regimes. The effects of these treatments on crystallinity and surface properties of this material were examined in the light of analytical data obtained by FTIR, DSC, X-ray diffraction, X-ray photoelectron spectroscopy, goniometry and a variety of microscopy techniques. 36 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.701984 Item 278 Food Additives and Contaminants 15, No.3, 1st April 1998, p.346-54 PARTS-PER-TRILLION DETERMINATION OF STYRENE IN YOGHURT BY PURGE-AND-TRAP GAS CHROMATOGRAPHY WITH MASS SPECTROMETRY DETECTION Nerin C; Rubio C; Cacho J; Salafranca J Zaragoza,University Headspace sampling methods prior to capillary gas chromatography are widely used for the determination of volatile compounds present in very different types of samples. An automated and rapid system for determination of volatiles from yoghurt was developed. Thirty-five volatile organic compounds(VOCs) were identified in PS cups used for yoghurt packaging and 42 VOCs from yoghurt samples. Quantitative analysis of styrene in several samples from the Spanish retail market was carried out. 16 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.700270 Item 279 Journal of Applied Polymer Science 70, No.6, 7th Nov.1998, p.1201-7 PHOTODEGRADATION OF TEFLON AF1600 DURING XPS ANALYSIS

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CANADA

Accession no.700200 Item 280 Polymer International 47, No.1, Sept.1998, p.72-5 TEMPERATURE-MODULATED DIFFERENTIAL SCANNING CALORIMETRY. II. DETERMINATION OF ACTIVATION ENERGIES Zhong Jiang; Hutchinson J M; Imrie C T Aberdeen,University Alternating differential scanning calorimetry (ADSC), a commercial development of temperature-modulated differential scanning calorimetry, was used to determine the activation energy associated with the relaxation processes in polycarbonate in the region of the glass transition. In this procedure the frequency of the temperature modulation is varied over a range of approximately one decade, and the mid-point of the step change in the complex heat capacity is evaluated. In these experiments, two different amplitudes of temperature modulation were employed. The results were in agreement with each other, and in good agreement with published values. Ripples seen on the Fourier-transformed signals are attributed to the mode of the data analysis, and not to noise on the data. 7 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.700165 Item 281 Materials World 6, No.10, Oct.1998, p.617-9 THROWING LIGHT ON FIBRES AND COMPOSITES Young B Manchester,University The use is discussed of Raman spectroscopy to monitor the stresses and strains on individual fibres in composite materials. New instrumentation has caused rapid growth in the use of Raman spectroscopy for materials characterisation, including the introduction of charged-

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coupled device cameras which offer significant improvements in sensitivity and very low noise, and also holographic notch filters which are used to remove the laser line and allow single monochromators to be used. Both these developments are incorporated in the Raman imaging microscope developed by Renishaw in collaboration with Leeds University Physics Department. Its use is described with reference to aramid fibre reinforced PP. 5 refs. RENISHAW PLC EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.699334 Item 282 Farbe und Lack 104, No.10, 1998, p.93/8 German MODULATED DIFFERENTIAL SCANNING CALORIMETRY Haessler R Dresden,Institut fuer Polymerforschung The use of modulated DSC for improved interpretation of product characteristics under thermal effects was investigated. Tgs, for example, which are masked by postcuring or enthalpy relaxation, could be detected in a single measurement and compared. The separation of complex transitions in multicomponent systems into individual parts such as melts, transition temps. and relaxations was shown to be feasible. The potential for use of modulated DSC in the field of epoxy resins was demonstrated using examples of the determination of Tg near the regions of enthalpy relaxation, melt and post-curing. 7 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.699054 Item 283 Structure and properties of Oriented Polymers. Second Edition. London, Chapman & Hall, 1997, p.234-68. 9 NUCLEAR MAGNETIC RESONANCE Speiss H W Max-Planck-Institut fuer Polymerforschung Edited by: Ward I M (Leeds,University) The basics of solid state NMR are outlined and the siteselective information available from multi-dimensional NMR spectra about molecular order and dynamics in oriented polymers is illustrated with specific experimental examples. 55 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.697739 Item 284 Structure and properties of Oriented Polymers. Second Edition.

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London, Chapman & Hall, 1997, p.181-233. 9 INFRARED DICHROISM, POLARISED FLUORESCENCE AND RAMAN SPECTROSCOPY Bower D I Leeds,University Edited by: Ward I M (Leeds,University) The three spectroscopic techniques for studying molecular orientation in polymers described in detail use polarised electromagnetic radiation. The principles of the techniques are outlined, relevant theory and experimental details described, and a selection of results presented. 79 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.697738 Item 285 Polymer 39, No.20, 1998, p.4973-6 EFFECTS OF SUBSTRATE INTERACTIONS IN THE LIQUID CHROMATOGRAPHY OF POLYMERS Kosmas M K; Bokaris E P; Georgaka E G Ioannina,University The elution behaviour of PMMA samples was studied through two liquid chromatographic columns, one containing a substrate of silica covered with trimethylsilyl groups and the other a substrate of pure silica. Both substrates had the same pore size and the solvent was the same for both columns. The results were discussed and they showed that the polymer-surface interactions changed when the nature of the substrate was changed. 14 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; WESTERN EUROPE

Accession no.696588 Item 286 Food Additives and Contaminants 15, No.1, 1st Jan.1998, p.93-9 SYSTEMATIC STUDY ON THE STABILITY OF SELECTED POLYMER ANTIOXIDANTS IN EU OFFICIAL AQUEOUS AND ALTERNATIVE FOOD SIMULANTS USING HPLC Demertzis P G; Franz R Fraunhofer Institute for Food Technol. & Packag. Details are given of the stability of five commercial antioxidants in food simulants and in an alternative fat simulant. Analysis was performed using a rapid HPLC method with UV detection. 23 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.695963

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References and Abstracts

Item 287 Colloid & Polymer Science 276, No.7, July 1998, p.565-9 DESCRIPTION OF THE GLASS TRANSITION MEASURED BY TEMPERATURE MODULATED DIFFERENTIAL SCANNING CALORIMETRY Schawe J E K Ulm,University

discussed include the use of SEM in studying fracture in mineral filled thermoplastics, secondary electron imaging in obtaining information on sample topography, backscattered electron imaging in studying filler dispersion in polymer matrices, and energy dispersive Xray spectroscopy in determining the chemical composition of the fillers or contaminants responsible for fracture initiation. 5 refs.

The temp. modulated DSC (TMDSC) technique could be used for heat capacity spectroscopy in the low frequency range. The measured property was the complex heat capacity. The frequency-dependent relaxation transition measured by TMDSC occurred in the temp. range of the thermal Tg. The non-equilibrium of the glassy state thus influenced the TMDSC curves. Experimental evidence was the dependence of the shape of the heat capacity curve on the thermal history. A theoretical description of the influence of the non-equilibrium state on the spectroscopic curves, based on the Tool-Narayanaswamy-Moynihan model, is presented. 23 refs.

BRAZIL

EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.695591 Item 288 Composites Plastiques Renforces Fibres de Verre Textile No.21, May/June 1997, p.48-54 French DURABILITY OF COMPOSITES: HOW TO ACHIEVE RELIABLE ACCELERATED AGEING Siampiringue N; Gaumet S; Lemaire J Centre National d’Evaluation de Photoprotection The use of accelerated ageing tests and spectrophotometric techniques in studying the photooxidative degradation of unsaturated polyester resins and glass fibre-reinforced composites is examined. Results of accelerated and natural ageing tests are compared, and criteria to be taken into account in achieving accelerated test results representative of reality are discussed. 5 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.695308 Item 289 Polimeros: Ciencia e Tecnologia 7, No.3, July/Sept.1997, p.19-23 Portuguese FAILURE ANALYSIS OF MATERIALS BY ADVANCED MICROSCOPIC TECHNIQUES Chinaglia C R; Correa C A Sao Carlos,Universidade Federal Failure analysis techniques allowing the determination of the chemical composition of a sample and its correlation with the observed fracture mode are examined. Topics

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Accession no.695299 Item 290 Journal of Polymer Science : Polymer Physics Edition 36, No.12, 15th Sept.1998, p.2165-75 DESCRIPTION OF THERMAL RELAXATION OF POLYSTYRENE CLOSE TO THE THERMAL GLASS TRANSITION Schawe J E K Ulm,University Using spectroscopic methods at relatively high frequency, the alpha-relaxation was measured in the thermodynamic equilibrium. In the caloric case this phenomenon is called thermal relaxation transition. Using a conventional differential scanning calorimeter, the transition of the equilibrium (the melt) into a nonequilibrium (the glassy state) was measured. This effect is called thermal glass transition. Temperature-modulated DSC curves in the glass transition region were described using the ToolNarayanaswamy-Moynihan model. 54 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.694872 Item 291 Journal of Polymer Science : Polymer Physics Edition 36, No.12, 15th Sept.1998, p.2103-9 RAPID DETERMINATION OF COMONOMER CONTENT, CRYSTALLINITY, AND LONG SPACING BY MULTIPLE-PULSE PROTON NMR IN ETHYLENE-VINYL ALCOHOL COPOLYMERS Perez E; Cerrada M L; Vanderhart D L Instituto de Ciencia y Tecnologia de Polimeros; US,National Institute of Standards & Technology Capitalising on the superior sensitivity of proton NMR, relatively rapid estimates of three parameters, namely, comonomer content, crystallinity, and long spacing, were determined for three ethylene-vinyl alcohol copolymers using solid state proton NMR measurements. Multiple-pulse techniques were utilised (a) in conjunction with magic angle spinning for measuring comonomer content, (b) in conjunction with a relaxation time measurement for determining crystallinity, and (c) in conjunction with a relaxation time-based spin diffusion measurement for determining the long spacing. These three parameters, extracted from data collected in a total spectrometer time of

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about 20 min., and were compared with similar parameters obtained using more conventional DSC, small angle X-ray scattering (including synchrotron), and solution-state NMR measurements, with good agreement. 23 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; USA; WESTERN EUROPE

Accession no.694867 Item 292 Smart Materials & Structures 7, No.4, Aug. 1998, p.557-68 IN SITU CURE MONITORING USING OPTICAL FIBRE SENSORS. A COMPARATIVE STUDY Powell G R; Crosby P A; Waters D N; France C M; Spooncer R C; Fernando G F Brunel University; Cranfield,University A comparative study is presented for different types of optical fibre sensor developed to monitor the cure of an epoxy resin system. The sensors were based on transmission spectroscopy, evanescent wave spectroscopy and refractive index monitoring. 19 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.694840 Item 293 Polymer Testing ’97. Day 3: Chemical Analysis. Conference proceedings. Shawbury, 7th-11th April 1997, Paper 4. 9T RAMAN SPECTROSCOPY OF POLYMERS Williams K P J; Wilcock I C Renishaw plc (Rapra Technology Ltd.; Plastics & Rubber Weekly; European Plastics News) Raman spectroscopy is now coming of age as a routine analytical method. Advances in Raman technology have meant that robust, user-friendly equipment can be manufactured at a reasonable cost. These advances are described, together with applications of Raman imaging microscope systems to polymer analysis. 11 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.694712 Item 294 International Polymer Processing 13, No.2, July 1998, p.142-8 PEROXIDE INDUCED CROSSLINKING AND DEGRADATION OF POLYAMIDE Yu Q; Zhu S McMaster University Peroxide-induced crosslinking and degradation of nylon 12 were investigated using ESR. Various reaction mechanisms are proposed. 20 refs. CANADA

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Item 295 Macromolecular Chemistry & Physics 199, No.8, 1998, p.1623-9 THERMAL STABILITY AND CRYSTALLISATION KINETICS OF PEEK Chen J-Y; Chen M; Chao S-C Taiwan,National Sun Yat-Sen University TGA, dynamic rheological analysis and polarised light microscopy were used to assess thermal stability of PEEK. Emphasis is given to the effect of melting temperature on thermal stability. 23 refs. CHINA

Accession no.694246 Item 296 Injection Molding 6, No.8, Aug. 1998, p.56/9 MATERIALS ANALYST: PART 13. PERFORMANCE PROBLEMS: WHEN THE PELLETS DON’T MATCH THE PARTS Sepe M Dickten & Masch Mfg. The use of differential scanning calorimetry and thermogravimetric analysis as analytical tools in part failure determination is applied. Problems are examined in part performance of moulded 30% glass-reinforced, low-viscosity PEI and a second part moulded from PPS with proprietary additives to improve wear resistance. The importance of checking the composition of the basic material is stressed. USA

Accession no.693205 Item 297 Journal of Applied Polymer Science 69, No.11, 12th Sept.1998, p.2175-85 IR SPECTROSCOPY AS A QUANTITATIVE AND PREDICTIVE ANALYSIS METHOD OF PHENOL-FORMALDEHYDE RESOL RESINS Holopainen T; Alvila L; Rainio J; Pakkanen T T Joensuu,University; Dynoresin Oy A set of resin samples was characterised by IR and carbon13 NMR spectroscopy. The suitability of IR spectroscopy for the quantitative analysis of resins was evaluated by statistical methods using the NMR reference data as calibration. The values of interesting properties, e.g. the amount of free phenol and the formaldehyde-to-phenol molar ratio, of the resins being similar to the calibration resins were predicted from the IR spectra. The predicted results were compared with those observed by carbon-13 NMR spectroscopy. 15 refs. FINLAND; SCANDINAVIA; WESTERN EUROPE

Accession no.692990 Item 298 Journal of Materials Science 33, No.13, 1st July 1998, p.3245-9

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References and Abstracts

XPS MONITORING OF THE REMOVAL OF AN AGED POLYMER COATING FROM A METAL SUBSTRATE BY TEA-CARBON DIOXIDE LASER ABLATION Cottam C A; Emmony D C; Cuesta A; Bradley R H Loughborough,University; Aberdeen,Robert Gordon University

transform-Raman spectroscopy was proposed as a qualitative tool to follow the degree of crosslinking in this high-ortho novolac. 54 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; WESTERN EUROPE

Accession no.689414

X-ray photoelectron spectrometry was used to observe the changes in surface chemistry during the removal of paint from a zinc coated steel substrate using TEA-carbon dioxide laser ablation. Laser ablation at both plasma and sub-plasma fluences were investigated and their relative merits discussed. The laser was shown to be effective in paint removal and was not impaired by ageing in the paint. 32 refs.

Item 301 Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.1415-7. 012 IN SITU SPECTROSCOPY OF CO2-INDUCED PLASTICISATION OF GLASSY POLYMERS Kazarian S G; Brantley N H; Eckert C A Georgia,Institute of Technology (SPE)

EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

In situ spectroscopy is used to study the plasticisation of glassy polymers by high-pressure and supercritical CO2. The methodology for in situ spectroscopic analysis of the interactions between CO2 and polymers is described. The changes in IR spectra of CO2 incorporated into various polymers indicate a specific interaction between CO2 and polymer functional groups. Increased polymer segmental mobility is also observed, indicative of the plasticisation phenomenon. Implications of these discovered molecular interactions are discussed. 25 refs.

Accession no.692055 Item 299 Analytical Chemistry 70, No.15, 1st Aug.1998, p.3298-303 IMPROVEMENTS IN POLYMER CHARACTERIZATION BY SIZE-EXCLUSION CHROMATOGRAPHY AND LIQUID CHROMATOGRAPHY AT THE CRITICAL CONDITION BY USING ENHANCED-FLUIDITY LIQUID MOBILE PHASES WITH PACKED CAPILLARY COLUMNS Hao Yun; Olesik S V; Marti E H Ohio,State University; Ashland Chemical Co. The use of the above combination of techniques is described and results obtained for samples of PS, PMMA, styrene-methyl acrylate copolymers and functionalised PS are presented and discussed. 32 refs. USA

Accession no.691471 Item 300 Polymer 39, No.22, 1998, p.5293-300 QUANTITATIVE CARBON-13 SOLID-STATE NMR AND FT-RAMAN SPECTROSCOPY IN NOVOLAC RESINS Ottenbourgs B; Adriaensens P; Carleer R; Vanderzande D; Gelan J Limburg,University A qualitative and quantitative study of the curing behaviour of a high-ortho novolac resin with paraformaldehyde under different conditions was conducted. The degree of cure as a function of the formaldehyde/phenol ratio, the degree of conversion and the final structure after curing were determined on the basis of a quantitative carbon-13 solid state NMR with cross-polarisation and magic angle spinning. The spin-lattice relaxation time was measured as a probe to follow the evolution of cure. Fourier

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USA

Accession no.687565 Item 302 Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.1860-4. 012 QUANTITATIVE ANALYSIS OF CHEMICAL BLOWING AGENTS BY DSC Prasad A; Shanker M Millennium Petrochemicals Inc. (SPE) It is shown that differential scanning calorimetery (DSC) can be used to determine quantitatively the level and composition of chemical blowing agents such as azodicarbonamide (azo) in commercial formulations. DSC can also be used to obtain the onset of decomposition temperature and the rate of decomposition of azo in the presence of group II and group IV metal salt activators. DSC has the potential to detect the level of undecomposed blowing agents present in processed foam products and to qualitatively determine the degree of dispersion of the blowing agent and the activators in commercial formulations. Advantages of DSC over the currently used EGA technique are ease of operation, shorter analysis time and detection of azo concentrations as low as 1%. 12 refs. USA

Accession no.687551 Item 303 Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.2114-8. 012

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APPLICATION OF GC/MS IN THERMOPLASTICS PROBLEM SOLVING Shaker D C; Kim H C LNP Engineering Plastics (SPE) The use of GC/MS (gas chromatography/mass spectrometry) in the thermoplastics problem solving area is outlined. GC/ MS is a hyphenated technique; i.e. it combines the two techniques, chromatography and spectroscopy. In this procedure, a material is introduced into the GC, components are separated and sent to the MS where they are ionised, and the resulting particles are separated by mass. The applications of GC/MS to solving complex problems are discussed through positive identification of base resins, contamination, odours and solvents. USA

Accession no.687499 Item 304 Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.2101-5. 012 TEMPERATURE GRADIENT INTERACTION CHROMATOGRAPHY OF POLYMERS Chang T; Lee W; Lee H C; Mays J W; Harville S; Frater D J Pohang,University of Science & Technology; Alabama,University at Birmingham (SPE) Temperature gradient interaction chromatography (TGIC) is a conventional reversed phase BPLC technique, but the column temperature is varied during elution. A very fine and reproducible control of interaction between polymer chains and the stationary phase can be achieved by changing the column temperature. Under a suitable temperature programming, this method provides a far superior resolution to conventional size exclusion chromatography. In addition, elution in TGIC is more sensitive to molecular weight alone. Thus it provides an excellent route to separating branched polymer molecules of similar hydrodynamic volume but differing molecular weight. 8 refs. KOREA; USA

Accession no.687496 Item 305 Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.2037-41. 012 MODULATED DIFFERENTIAL SCANNING CALORIMETRY TO STUDY REACTING POLYMER SYSTEMS Van Mele B; Van Assche G; Van Hemelrijck A Brussels,Free University (SPE) Modulated (temperature) differential scanning calorimetry (MTDSC or MDSC) is used to simultaneously study the evolution of heat flow and heat capacity for the isothermal and non-isothermal reactions of polymer systems. An

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epoxy-anhydride thermosetting system is used as an example. Vitrification and devitrification steps are observed. The heat flow phase during isothermal and nonisothermal cure is always small, but its evolution contains information on relaxation phenomena, vitrification and devitrification, in the course of the chemical reaction. Modelling of the (heat flow related) chemical kinetics and the (heat capacity related) mobility restrictions contributes to a better understanding of the reaction mechanism and reaction kinetics up to a high degree of chemical conversion. The use of MTDSC as a tool for a quantitative construction of the vitrification curve in Temperature-TimeTransformation and Continuous-Heating-Transformation diagrams is illustrated. 20 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; WESTERN EUROPE

Accession no.687483 Item 306 Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.2215-8. 012 PRACTICAL ANALYSIS TECHNIQUES OF POLYMER FILLERS BY FOURIER TRANSFORM INFRARED SPECTROSCOPY (FTIR) Coles B J; Hall C J Hauser Inc. (SPE) The identification of polymers by FTIR is often complicated by the presence of fillers. However for kaolin clay, an FTIR analysis should be able to identify the filler and predict its concentration using a standard curve. The resulting percentage is more reliable than a simple ash, which may change the chemical composition of the filler. 2 refs. USA

Accession no.687418 Item 307 Polymer Engineering and Science 38, No.6, June 1998, p.922-5 IDENTIFICATION OF OFF-FLAVOUR COMPOUNDS IN HDPE WITH DIFFERENT AMOUNTS OF ABSCENTS Villberg K; Veijanen A; Gustafsson I Jyvaskyla,University; Borealis AB Details are given of the addition of zeolite to HDPE drinking water pipes in an attempt to eliminate odours and to remove odour-causing compounds. The system used for analysis of volatile organic compounds was a gas chromatographic/mass spectrometric sniffing system. Purge and trap techniques were used to introduce the volatile, off-flavour components into the gas chromatograph. 16 refs. FINLAND; SCANDINAVIA; SWEDEN; WESTERN EUROPE

Accession no.686400

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References and Abstracts

Item 308 Polymer 39, No.19, 1998, p.4665-73 SURFACE GLASS TRANSITION BEHAVIOUR OF AMORPHOUS POLYMER FILM BY SCANNING FORCE MICROSCOPY AND SURFACE SPECTROSCOPY Kakiyama T; Tanaka K; Takahara A Kyushu,University The surface molecular motion of amorphous polymeric solids was measured by lateral force microscopy, scanning viscoelasticity microscopy, and differential X-ray photoelectron spectroscopy. Data are given for PS and styrene-methyl methacrylate copolymers. 35 refs. JAPAN

Accession no.686392 Item 309 Revista de Plasticos Modernos 73, No.487, Jan.1997, p.26-31 Spanish TEMPERATURE MODULATED DIFFERENTIAL SCANNING CALORIMETRY: A STEP FORWARD IN STUDYING THE THERMAL PROPERTIES OF POLYMERS Perena J M Instituto de Ciencia y Tecnologia de Polimeros The principles of temperature modulated DSC are described, and a number of examples are presented of its application to studies of the thermal properties of plastics. Some limitations of the technique are also examined. 6 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.686251 Item 310 Analytical Chemistry 70, No.13, 1st July 1998, p.456A-61A CHARACTERISING SYNTHETIC POLYMERS BY MALDI MS Kuang Jen Wu; Odom R W Evans C.,& Associates An review is given of the use of matrix-assisted laser desorption/ionisation time-of flight (MALDI TOF) mass spectroscopy to determine MWDs and structures of synthetic organic polymers, including the ion desorption mechanism, synthetic polymer analysis, molecular weight analysis, and its use in calibration of GPC profiles. 30 refs. USA

Accession no.686157 Item 311 Food Additives and Contaminants

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15, No.2, 1998, p.217-28 EFFECTS OF PACKAGING AND STORAGE CONDITIONS ON VOLATILE COMPOUNDS IN GAS-PACKED POULTRY MEAT Eilamo M; Kinnunen A; Latva-Kala K; Ahvenainen R VTT Biotechnology & Food Research; Finland,Technical Research Centre Volatile compounds released by raw chicken legs packed in modified atmosphere packages were determined to develop a spoilage indicator for monitoring the shelf life of raw chicken. The effects of four packaging factors (headspace volume, oxygen transmission rate of the package, residual oxygen and carbon dioxide concentration) and three storage factors (temperature, illumination and storage time) on the amounts of volatile compounds in the headspace of gas packages containing two chicken legs were studied. Statistical experimental design was applied and a linear screening design comprising 18 experiments (fractional factorial) was utilised. Volatile compounds in package headspace were determined by gas chromatography/mass spectrometry. The results were compared with the results of sensory evaluation and microbial determinations. 8 refs. FINLAND; SCANDINAVIA; WESTERN EUROPE

Accession no.686119 Item 312 International Journal of Adhesion & Adhesives 18, No.3, 1998, p.193-8 USE OF XPS AND TOF-SIMS TO INVESTIGATE ADHESION FAILURE OF A CATIONIC RADIATION CURED COATING ON GALVANISED STEEL Leadley S R; Watts J F; Rodriguez A; Lowe C Surrey,University; Becker Industrial Coatings Details are given of coating delamination in a hot, humid environment for a cationic radiation cured coating of cycloaliphatic epoxy resin. X-ray photoelectron spectroscopy and time-of-flight mass spectroscopy of the delaminated surface showed that the phosphorus hexafluoride anion of the photoinitiator segregates to the interface. The durability of the coating was improved by reformulation with a reduced concentration of photoinitiator. 7 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.684932 Item 313 Antec ’98. Volume I. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.816-20. 012 METHODS FOR THE MEASUREMENT OF CRYSTALLINITY OF PREFORMS AND BOTTLES MADE FROM PETP Bashir Z; Al-Alouish I; Al-Raqibah I; Ibrahim M SABIC Corp.

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References and Abstracts

(SPE) PETP has established itself as a material for making lightweight, clear and tough bottles. Ideally, a preform with zero or very low crystallinity (for purposes of clarity) is sought, while the final bottle should have high crystallinity (for enhancing gas barrier and mechanical properties). Monitoring crystallinity is thus important. An attempt is made to evaluate methods of crystallinity measurement using density, differential scanning calorimetry and modulated differential scanning calorimetry to study the crystallinity of preforms and bottles. The applicability and appropriateness of each technique for different PETP sample types, and interpretation problems are also discussed. 20 refs. SAUDI ARABIA

Accession no.684627 Item 314 Polymer Journal (Japan) 30, No.5, 1998, p.439-43 DIRECT DETERMINATION OF MOLECULAR WEIGHT DISTRIBUTION BY SIZE EXCLUSION CHROMATOGRAPHY(SEC) WITH 750 MHZ PROTON NMR DETECTION (ON-LINE SECNMR) Ute K; Niimi R; Hongo S; Hatada K Osaka,University The above on-line SEC-NMR technique was used to analyse MWDs of isotactic PMMAs with Mn ranging from 3270 to 22,200. The molec.wt. of the polymer in flowing eluate was determined directly (without a conventional calibration procedure) from he relative intensity of NMR signals due to the end group and repeating units. The MWD determined in this manner was proved to be accurate by SEC-NMR experiments on uniform isotactic PMMAs consisting of exactly 23, 40 and 80 repeating units. Investigation was also undertaken to optimise flow rate and NMR parameters for quantitative SEC-NMR measurements. The signal-to-noise ratio of 750 MHz SEC-NMR spectra was 9.2 times that obtained previously with 500 MHz SEC-NMR operated under similar conditions. 17 refs. JAPAN

Accession no.684613 Item 315 Shawbury, Rapra Technology Ltd., 1996, pp.150. 95.00. 30cms. 9511 ENVIRONMENTAL STRESS CRACKING OF PLASTICS Wright D C Rapra Technology Ltd. This book reviews the factors which influence environmental stress cracking, and examines the current state of knowledge regarding specific categories of plastics. The book is divided into three main sections

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focusing on the prediction of ESC and assessment by testing, factors that influence ESC and data on specific plastics. Methods for the experimental evaluation of environmental stress are described. This book is available for purchase from Publication Sales, Rapra Technology Ltd. Accession no.683806 Item 316 Journal of Adhesion Science and Technology 12, No.5, 1998, p.507-21 EFFECT OF CURING TEMPERATURE ON THE ADHESION STRENGTH OF POLYAMIDEIMIDE/ COPPER JOINTS Cho J H; Kong D I; Park C E; Jin M Y Pohang,University of Science & Technology; Korea,Research Institute of Chemical Technology The adhesion strength of polyamideimide/copper joints was investigated as a function of the curing temperature and time. The effects of copper oxide formed by thermal treatment and alkaline treatment on the adhesive strength of the joints were examined. The locus of failure of the joints was also studied by SEM and X-ray photoelectron spectroscopy. 21 refs. KOREA

Accession no.682955 Item 317 Polymer Engineering and Science 38, No.4, April 1998, p.566-72 DYNAMIC AND ISOTHERMAL THERMOGRAVIMETRIC ANALYSIS OF A POLYCYANURATE THERMOSETTING SYSTEM Zacharia R E; Simon S L Pittsburgh,University Isothermal and dynamic thermogravimetric analysis (TGA) were performed on a polycyanurate thermosetting material. The effects on thermal stability of the copper naphthenate catalyst were studied by comparing two systems with different amounts of catalyst. Tests were performed isothermally at temperatures ranging from 200240C for times up to one week. Dynamic tests were also performed at rates of 0.1 C/min to 40 C/min at temperatures ranging from 180 to 600C. Results demonstrate the difficulties of extrapolating dynamic TGA data to use conditions to predict long-term thermal stability. 14 refs. USA

Accession no.681689 Item 318 European Polymer Journal 34, No.2, Feb.1998, p.163-70 STUDY OF TALC-ADDITIVE INTERACTIONS BY COMBINED TGA-FTIR SYSTEM Bertin D; Boutevin B; Rigal G; Fourty G

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References and Abstracts

Montpellier,Ecole Nationale Superieure de Chimie; Talcs de Luzenac SA By using combined TGA/FTIR thermogravimetric analysis, accurate real time qualitative and quantitative data can be obtained for thermal decomposition of polymers. It was used to study interactions between an additive and a filler (talc), highlighting a degradation phenomenon of additive by talc, and this phenomenon depended on the structure and chemical composition of talc. This procedure also applied to analysis of degradation of other additives by talc. Thus, polymer formulations will rapidly be optimised in various areas of filled polymers. 12 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.681630 Item 319 Journal of Polymer Science : Polymer Chemistry Edition 36, No.9, 15th July 1998, p.1363-71 LIQUID CHROMATOGRAPHY OF MACROMOLECULES AT THE CRITICAL ADSORPTION POINT. II. ROLE OF COLUMN PACKING: BARE SILICA GEL Berek D; Janco M; Meira G R Slovak,Academy of Sciences; INTEC CONICET Data are presented manifesting the role of column packings from the point of view of both their pore size and surface chemistry. Bare silica gels that are the most commonly used LC CAP column packings and model macromolecules, viz. narrow PMMA, were investigated. 20 refs. ARGENTINA; SLOVAK REPUBLIC; SLOVAKIA

Accession no.681599 Item 320 20th Annual Anniversary Meeting of the Adhesion Society. Conference proceedings. Hilton Head Island, S.C., 23rd-26th Feb.1997, p.51921. 8(10) USING XPS TO INVESTIGATE FIBRE/MATRIX CHEMICAL INTERACTIONS AT THE INTERFACE IN CARBON FIBRE REINFORCED COMPOSITES Weitzsacker C L; Xie M; Drzal L T Michigan,State University Edited by: Drzal L T; Schreiber H P (US,Adhesion Society) With composites expanding into areas from aerospace to recreation, different matrices are being investigated to tailor composites to specific uses. The degree of adhesion between the fibre and matrix, influenced by chemical reactions, mechanical interactions and topography at the fibre/matrix interface, has been recognised as a critical factor in determining the performance of fibre-reinforced

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composites. The interaction and chemical reaction of functional groups in the matrix with functional groups at the fibrer surface contribute to the adhesion. Direct analysis of the fibre/matrix interface by surface analytical methods such as X-ray photoelectron spectroscopy is not trivial due to the thickness of a matrix layer over fibres and the complexity of the matrix system. Indirect analysis of the matrix/fibre interface is possible using model compounds which represent functional groups where differences in results are indicative of reaction between fibre and matrix. The matrix functional groups that may chemically react with the fibre surface can be separated and investigated individually. Mixtures of model compounds can be used to investigate functional groups reactions between the components, and with the fibre surface. Model compounds based on epoxy, polyimide, polyphenylene sulphide and vinyl ester matrices are investigated to characterise the chemical reactions at the fibre/matrix interface. XPS is used to characterise both the carbon fibre surfaces and the reacted carbon fibre surfaces. The model compounds representative of each of these matrices demonstrate the range of possible reactions and interactions possible between the fibre and matrix, ranging from no reaction to distinct chemical reactions. 4 refs. USA

Accession no.681439 Item 321 Cleanrooms 12, No.5, Suppl. May 1998, p.S13/20 APPLICATION OF FTIR FOR MONITORING CLEANROOM AIR AND PROCESS EMISSIONS Zazzera L; Reagen W 3M Co. The use of FTIR monitoring methods for HAP, VOC, PFC and HFC emissions for identification and quantification in process exhaust and in clean room air, is discussed. A summary is included of the various protocols, test methods and references for the use of FTIR spectroscopy to generate verifiable data. Results of field trials and laboratory study trials are presented, which demonstrate its value as a monitoring method in the semiconductor industry USA

Accession no.679498 Item 322 Analytical Chemistry 70, No.8, 15th April 1998, p.1563-8 POLYMER ANALYSIS BY MICRO-SCALE SIZEEXCLUSION CHROMATOGRAPHY(SEC)/ MALDI TIME-OF-FLIGHT MASS SPECTROMETRY WITH A ROBOTIC INTERFACE Nielen M W F Akzo Nobel Central Research

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A report is presented on the development of a micro-scale SEC system in which the MALDI matrix solution is coaxially added to the column effluent and directly spotted onto the MALDI targets in a robotic interface. Each spot corresponds to the 10-s elution window from the microSEC column, thus yielding a narrow polymer distribution which is amenable to characterisation by MALDI mass spectroscopy. The performance of the system is demonstrated by the characterisation of a polybisphenol A carbonate and a complex dipropoxylated bisphenol A/ adipic acid/isophthalic acid copolyester resin. 29 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; WESTERN EUROPE

Accession no.679150 Item 323 Polymer Engineering and Science 38, No.2, Feb.1998, p.265-73 DSC STUDIES ON THE CRYSTALLISATION CHARACTERISTICS OF POLY(ETHYLENE TEREPHTHALATE) FOR BLOW MOULDING APPLICATIONS Daw-Ming Fann; Huang S K; Jiunn-Yih Lee Taiwan,National University of Science & Technology The crystallisation behaviour of blow moulded PETP bottles, which helps determine the product’s transparency, was investigated by DSC dynamic cooling experiments that simulated the cooling that occurs in the injection blow moulding manufacturing process. DSC measurements were used to obtain information on related aspects, such as the ease of crystallisation from glassy and molten states and crystallinity in the products. An Avrami equation was used for calculation of the crystallisation kinetic parameters. 40 refs. TAIWAN

Accession no.678858 Item 324 TAPPI 1997 Polymers, Laminations and Coatings Conference. Conference Proceedings. Book 1. Toronto, Ontario, 24th-28th Aug.1997, p.173-82. 012 INFLUENCE OF MINERAL FILLERS ON THE PROCESSING OF LLDPE FILMS Ansari D M; Higgs R P ECC International Ltd. (TAPPI) A study was made of the thermal properties and melt rheology of linear LDPE masterbatches filled with calcium carbonate, talc and calcined clay. Films were prepared by extrusion blowing and temperature changes were monitored along the bubble. Filler distribution within the films was assessed by optical and electron microscopy. Rheological properties of the diluted masterbatches were evaluated over four decades of shear rate. The mineral fillers increased cooling rates and improved bubble stability. Coarser calcium carbonate grades gave the

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greatest improvement, while fine grades and talc had little effect. Micrographs revealed the level of interparticle contact and alignment of anisotropic particles which gave rise to the observed differences. Filler type and content did not significantly influence shear rheology at the shear rates associated with film extrusion. 17 refs. CANADA; EUROPEAN COMMUNITY; EUROPEAN UNION; UK; USA; WESTERN EUROPE

Accession no.677503 Item 325 TAPPI 1997 Polymers, Laminations and Coatings Conference. Conference Proceedings. Book 1. Toronto, Ontario, 24th-28th Aug.1997, p.35-44. 012 EFFECT OF TITANIUM DIOXIDE ON EXTRUSION STABILITY Merkley J H Eastman Chemical Co. (TAPPI) Rheological techniques for following the degradation and changes in molecular weight and MWD of titanium dioxide-filled polyolefins during extrusion coating are examined. These include measurements of the crossover point between loss modulus and storage modulus and the variation in complex viscosity versus frequency curves seen in the rotational mechanical spectrometer curves, variations in viscosity versus shear rate seen in the capillary extrusion rheometer curves, and shifts in the DMTA curves. CANADA; USA

Accession no.677489 Item 326 Journal of Polymer Science : Polymer Chemistry Edition 36, No.5, 15th April 1998, p.851-60 PEROXIDE INDUCED CROSSLINKING AND DEGRADATION OF PVC Yu Q; Zhu S; Zhou W McMaster University Peroxide induced crosslinking and degradation of PVC were investigated using an on-line ESR technique. The reaction variables included temperature, peroxide type and concentration. The mechanism involved in the reaction was determined base on the radical information. The gel content and swelling ratio were also measured. 38 refs. CANADA

Accession no.674965 Item 327 Journal of Materials Science Letters 17, No.6, 15th March 1998, p.511-3 EVIDENCE OF MOLECULAR ORIENTATION IN POLY(3-BUTYLTHIOPHENE) FILMS BY ELECTRON SPIN RESONANCE MEASUREMENTS

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References and Abstracts

Pawlicka A; Walmsley L; Faria R M; Nascimento O R Sao Paulo,University; Paulista,Universidade Estadual It was demonstrated that ESR could show evidence of molecular orientation in films of poly(3-butyl thiophene), making ESR useful to study orientation in conjugated polymers when it is wished to avoid radiation damage or for a non-destructive investigation before X-ray measurements. 11 refs. BRAZIL

Accession no.674766 Item 328 Macromolecules 30, No.25, 15th Dec.1997, p.7970-6 DSC, FT-IR, AND ENERGY DISPERSIVE X-RAY DIFFRACTION APPLIED TO THE STUDY OF THE GLASS TRANSITION OF POLY(PPHENYLENE SULPHIDE) Caminiti R; D’Ilario L; Martinelli A; Piozzi A; Sadun C Roma,Universita La Sapienza; Roma,Istituto Nazionale per la Fisica della Materia The glass transition of PPS was studied by means of DSC, FTIR spectroscopy and energy dispersive X-ray diffraction. All of the techniques showed the alpha-transition of the polymer. The results of the different techniques were consistent if the onset temperature for the DSC experiments was taken as representative of the glass transition. The glass transition temperature was found to vary as a function of the heating rate. The activation energy of the glass transition process was calculated by means of a theoretical model. The results were discussed. 47 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.672088 Item 329 Kunststoffe Plast Europe 88, No.2, Feb.1998, p.34-5 WHAT HAS GONE WRONG? Sass A NRW GmbH Practical case studies are used to demonstrate how useful differential scanning microscopy analysis can be for material testing and damage analysis on plastics and plastic parts. It measures the physical and chemical properties of the plastic as a function of temperature. Information gained by use of the analytical tool is examined, and case studies relating to fluctuating material quality through the use of recyclate, and the oxidation of PP water pipes are discussed. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

SHEATH-CORE DIFFERENCES CAUSED BY RAPID THERMOOXIDATION DURING MELT BLOWING OF FIBRES Kelley S L; Shambaugh R L Oklahoma,University A technique based on intrinsic viscosity measurements was developed for measuring sheath and core molecular weights during melt blowing of fibres. A mathematical model is described which accounts for rapid diffusion and thermooxidation. Experimental molecular weight measurements for PP fibres were compared with theoretical predictions. 29 refs. USA

Accession no.670584 Item 331 Polymer Bulletin 40, No.2-3, Feb./March 1998, p.227-34 COMPATIBILISATION OF POLYSULPHONE/ POLYAMIDE BLENDS BY REACTIVE POLYSULPHONES. EVIDENCE FOR COPOLYMER FORMATION Weber M; Heckmann W BASF AG Melt blending studies using polysulphone with different functional groups and polyamide were performed in a batch type mixer. Blends were investigated by solvent extraction and TEM. Model experiments revealed the possibility to compatibilise these blends by reactive blending techniques using functionalised polysulphones. 14 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.670478 Item 332 Journal of Polymer Science : Polymer Physics Edition 36, No.1, 15th Jan.1998, p.133-41 NEW APPROACH FOR ESTIMATING THE RECRYSTALLISATION RATE AND EQUILIBRIUM MELTING TEMPERATURE Hong Gyun Kim; Robertson R E Michigan,University A method was described for measuring the heat and rate of crystallisation following partial melting. The method uses a specific sequence of temperatures with a differential scanning calorimeter, and the melting and recrystallisation processes were confirmed by optical observations. The method was applied to poly(butylene terephthalate). The melting temperatures obtained from recrystallisation were used in the Hoffman-Weeks equation to deduce 236 C as the equilibrium melting temperature for PBTP. 22 refs. USA

Accession no.671875

Accession no.669994

Item 330 Industrial & Engineering Chemistry Research 37, No.3, March 1998, p.1140-53

Item 333 Composites Science & Technology 57, No.8, Aug.1997, p.975-83

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References and Abstracts

EFFECTS OF SILANE COUPLING AGENTS ON THE INTERPHASE AND PERFORMANCE OF GLASS-FIBRE REINFORCED POLYMER COMPOSITES Wu H F; Dwight D W; Huff N T Owens-Corning Science & Technology Center A single filament model of a commercial glass fibrereinforcement manufacturing process was used to apply methacryloxy and amino silanes with one, two and three silanols to two different glass fibres in a molecular model. Surface analyses by angular-dependent X-ray photoelectron spectroscopy, electric-kinetic analysis, and contact-angle measurements were used to characterise the surface coatings. The micro-indentation technique was used to evaluate fibre-matrix interfacial adhesion. Changes observed in surface chemistry, micromechanics, and composite properties as functions of silanol type are correlated. Data includes molecular models of coupling agent on E-glass surface, chemisorption of coupling agent into glass surface, isoelectric point values for each treatment, composite flexural strength, composite TS, and composite interfacial shear strength before and after 3days in boiling water. Matrix was polyester resin (E-701 from Owens Corning). 22 refs. (Presented at 6th Int. Conf. on Composite Interfaces, Microphenomena in Advanced Interfaces, Zichron Yaacov, Israel, 5th-8th May 1996). USA

Accession no.669950 Item 334 Polymer Bulletin 39, No.6, Dec.1997, p.721-7 COMPARISON OF CALIBRATION WITH PPG AND PS STANDARDS IN SIZE EXCLUSION CHROMATOGRAPHY MEASUREMENTS FOR CHARACTERISATION OF OLIGOLACTONE MACROMONOMERS Schoch M; Gopp U; Steurich S; Sandner B Halle,Martin-Luther-Universitat The calibration of size exclusion chromatography measurements for the determination of the molecular weights of oligolactone macromonomers was carried out using PPG and PS as standards. Results are compared with those obtained by end-group analysis with proton NMR14 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.669429 Item 335 Analytical Chemistry 70, No.1, 1st Jan.1998, p.131-5 USE OF MALDI-TOF TO MEASURE MOLECULAR WEIGHT DISTRIBUTIONS OF POLYDISPERSE POLYMETHYL METHACRYLATE

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Rashidzadeh H; Baochuan Guo Cleveland,State University Using PMMA samples, some of the causes of mass discrimination encountered in the MALDI-TOF analysis of polydisperse polymers were investigated. It was found that detector saturation could be a major instrumental factor causing mass discrimination. This was due to the strong signals of matrix-related ions and low-mass oligomer ions. The matrix effect as another source of mass discrimination was analysed quantitatively. 34 refs. USA

Accession no.666829 Item 336 Polymer 39, Nos.6-7, 1998, p.1439-43 TEMPERATURE MODULATED DSC STUDY OF POLYETHYLENE TEREPHTHALATE CRYSTALLIZATION. II. APPLICABILITY TO NON-ISOTHERMAL PROCESS Toda A; Tomita C; Hikosaka M; Saruyama Y Hiroshima,University; Kyoto,Institute of Technology The non-isothermal crystallisation of PETP was examined by temp. modulated DSC(TMDSC). A new analytical model of TMDSC was applied to the process, taking account of the response of exothermic heat flow to temp. modulation in an apparent heat capacity of complex quantity. By examining the frequency dependence of the apparent heat capacity, the applicability was successfully examined for the non-isothermal process. The method was capable of determining the temp. dependence of crystal growth rate from TMDSC data analysis. The results were in good agreement with the dependence determined from literature values of spherulite growth rate measured by optical microscopy. 12 refs. JAPAN

Accession no.666765 Item 337 Polymer Journal (Japan) 29, No.11, 1997, p.910-3 FRACTIONATION OF PEO STAR SAMPLES BY SUPERCRITICAL FLUIDS Cansell F; Botella P; Six J-L; Garrabos Y; Tufeu R; Gnanou Y CNRS Details are given of the use of supercritical fluids for the fractionation of PEO. The fractionation of a binary mixture of star and linear chains of PEO was studied. 25 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.666545 Item 338 Polymer 39, No.2, 1998, p.255-66

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References and Abstracts

INVESTIGATION OF PHYSICAL AGEING IN POLYMETHYLMETHACRYLATE USING POSITRON ANNIHILATION, DIELECTRIC RELAXATION AND DYNAMIC MECHANICAL THERMAL ANALYSIS Davis W J; Pethrick R A Strathclyde,University Physical ageing of PMMA was studied using positron annihilation lifetime spectroscopy (PALS), dielectric relaxation spectroscopy (DRS) and dynamic mechanical thermal analysis (DMTA) and the results obtained from these techniques were compared. A correlation existed between the free volume as measured by PALS and the changes which occurred in the DRS and DMTA data. It was concluded that “thermorheologically simplicity” was probably an oversimplification for this system and that physical ageing was associated with a redistribution, not just a shift, of molecular relaxation processes. The relaxation distribution changed as the glass transition temperature was approached. The free volume distribution probably changed during ageing, but it was not possible to quantify these changes from the PALS study. 43 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.665913 Item 339 Journal of Applied Polymer Science 67, No.3, 18th Jan.1998, p.487-500 SURFACE ENERGY MAPPING OF KEVLAR FIBRES BY INVERSE GAS CHROMATOGRAPHY Rebouillat S; Donnet J B; Guo H; Wang T K Du Pont (UK) Ltd.; Ecole Nationale Superieure de Chimie de Mulhouse The surface energy characteristics of three Kevlar fibres were systematically studied using two inverse gas chromatography (IGC) techniques, i.e. at an infinite probe dilution and at a finite probe concentration, with the latter allowing a unique mapping of the surface energy levels, which complements greatly the more traditional characterisation of the highest energy sites. The standard thermodynamic parameters, such as the free energy and the adsorption enthalpy and entropy, as well as the dispersive and the specific component of the fibre surface energy, were determined from the retention behaviour at zero coverage of selected molecules of various polarity. Using the second IGC approach, i.e. at finite concentration, the isotherms for the adsorption of n-octane and n-hexylamine on the three selected Kevlar fibres were constructed by the one peak method. 29 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.665736 Item 340 Journal of Applied Polymer Science

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67, No.3, 18th Jan.1998, p.449-53 COMPATIBILITY STUDY OF POLYCARBONATE-POLYVINYL PYRROLIDONE BLEND USING HIGH RESOLUTION SOLID STATE NUCLEAR MAGNETIC RESONANCE da Silva E P; Tavares M I B Rio de Janeiro,Universidade Estadual do Norte Fluminense; Rio de Janeiro,Universidade Federal The combining NMR techniques in the solid state permit the evaluation of the polymeric systems homogeneity. In polycarbonate-polyvinyl pyrrolidone blends, the response of proton spin-lattice relaxation time in the rotating frame was the determinant to obtain information on the transition when the quantity of polyvinyl pyrrolidone is close to 40 wt% and a better organisation of amorphous phase was detected. 13 refs. BRAZIL

Accession no.665732 Item 341 Applied Spectroscopy 51, No.12, Dec.1997, p.1823-5 INVESTIGATION OF CHEMICAL INTERACTIONS AT THE STEEL/POLYMER INTERFACE BY FT-IR DIFFUSE REFLECTANCE SPECTROSCOPY Bistac S; Vallat M F; Schultz J Institut de Chimie des Surfaces et Interfaces Interactions between a steel surface and an ethylene-vinyl acetate copolymer grafted with maleic anhydride were investigated by FTIR diffuse reflectance spectroscopy. The failed surfaces obtained after a mechanical separation of the polymer/steel assemblies were analysed. A twostep mechanism was proposed: the opening of the anhydride cycle by a hydrolysis reaction, leading to the formation of a carboxylic diacid, followed by the reaction of the acid with some oxidised metallic elements present at the metal surface. This study underlines the contribution of FTIR reflectance techniques to the understanding of adhesion mechanisms. 7 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.665698 Item 342 Applied Spectroscopy 51, No.12, Dec.1997, p.1784-90 DEPTH PROFILING STUDY OF EFFECT OF ANNEALING TEMPERATURE ON POLYMER/ POLYMER INTERFACES IN LAMINATES USING CONFOCAL RAMAN MICROSPECTROSCOPY Hajatdoost S; Olsthoorn M; Yarwood J Sheffield,Hallam University; Utrecht,University The effect of annealing temperature on molecular interactions at the interface of polymer laminates was

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reported. Depth profiling was carried out using confocal Raman microspectroscopy to study polyacrylonitrile/ polyvinyl alcohol and polyacrylonitrile/polyacrylic acid laminates. The laminates were annealed at 65, 75 and 90C. It was demonstrated that the degree of hydrogen bonding interaction between the nitrile and alcohol groups near the interfacial region changes between laminates annealed at different temperatures. For comparison, Raman mapping of a polyacrylonitrile-polyvinyl alcohol blend was used to study the interactions between the polymers in this (disordered) system. 29 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; UK; WESTERN EUROPE

Accession no.665697 Item 343 Applied Spectroscopy 51, No.11, Nov.1997, p.1741-4 CHARACTERISATION OF DENTURE ACRYLIC RESIN SURFACES MODIFIED BY GLOW DISCHARGES Suzer S; Ozden N; Akaltan F; Akovali G Bilkent,University; Ankara,University; Middle East,Technical University Resin samples prepared by compression moulding using a PMMA denture base material were exposed to radio frequency glow discharges to improve the wettability of the material. FTIR reflectance, X-ray photoelectron spectroscopy and contact angle measurements were used to characterise the changes introduced by the glow discharge plasma. 18 refs. TURKEY

Accession no.665695

Item 345 Applied Spectroscopy 51, No.11, Nov.1997, p.1668-77 RAPID-SCAN TWO-DIMENSIONAL FT-IR: AN EFFICIENT APPROACH TO DYNAMIC INFRARED SPECTROSCOPY Steeman P A M DSM Research A new and efficient mode of operation is presented that involves a continuous rapid-scan FTIR spectrometer, the measurement technique relying completely on the utilisation of the digital signal processor for data acquisition and manipulation. Experimental and mathematical details were discussed. Application of the rapid-scan technique was illustrated with some results for a styrene-acrylonitrile/butadiene copolymer. 17 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; WESTERN EUROPE

Accession no.665692 Item 346 Applied Spectroscopy 51, No.11, Nov.1997, p.1593-6 RAMAN IMAGING OF DENTAL ADHESIVE DIFFUSION Wieliczka D M; Kruger M B; Spencer P Missouri,University Using micro-Raman spectroscopy, chemical and morphological information on the dentin/adhesive interface was collected with minimal sample preparation. Results provided direct evidence of an adhesive preparation and demineralisation depth for two adhesive systems. 17 refs. USA

Item 344 Applied Spectroscopy 51, No.11, Nov.1997, p.1736-40 GENERALISED TWO-DIMENSIONAL FOURIER TRANSFORM INFRARED PHOTOACOUSTIC SPECTRAL DEPTH-PROFILING ANALYSIS Jiang E Y; McCarthy W J; Drapcho D L; Crocombe R A Bio-Rad Laboratories Inc. A new application of generalised two-dimensional correlation spectroscopy in photoacoustic depth-profiling analysis. Both rapid-scan and step-scan photoacoustic spectroscopy (obtained by using the software-based digital signal processing technique) of multilayer samples were used to calculate generalised two-dimensional correlation maps. Advantages of this unambiguous analysis method in enhancing spectral as well as depth resolutions, over conventional two-dimensional correlation and other spectral depth-profiling methods, were discussed. 31 refs. USA

Accession no.665694

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Accession no.665691 Item 347 Injection Molding 5, No.12, Dec. 1997, p.44-5 MATERIALS ANALYST: PART 3. LOT-TO-LOT VARIATION Sepe M Dickten & Masch Mfg.Co. The use is examined of thermogravimetric analysis as an analytical tool for the diagnosis of part failure in injection moulding. The consistent performance of an ethylene vinyl acetate copolymer was evaluated and the need to separate the component parts of the material to test for the amount of vinyl acetate in the compound is discussed in order to develop a thermal history. Once this history is established, a customer can institute an incoming QC test on the material’s composition rather than by adjusting the process for each new lot and performing product testing after the parts have been produced. USA

Accession no.664180

© Copyright 2002 Rapra Technology Limited

References and Abstracts

Item 348 Polymer Degradation and Stability 57, No.3, 1997, p.313-24 THERMOANALYTICAL STUDY OF THE EFFECT OF EAA AND STARCH ON THE THERMOOXIDATIVE DEGRADATION OF LDPE Bikiaris D; Prinos J; Perrier C; Panayiotou C Thessaloniki,University The effect of ethylene-acrylic acid copolymer (EAA) and plasticised starch (PLST) on the thermooxidative degradation of LDPE was examined. The course of oxidation was followed using TGA to monitor the weight changes during heating and DSC to study the heat changes taking place during oxidation. Three types of blend were examined: LDPE-plasticised starch, LDPE-EAA and LDPE-starch-EAA blends. All blends contained cobalt stearate as prooxidant. 36 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; WESTERN EUROPE

Accession no.664073 Item 349 Pitture e Vernici 73, No.17, 1997, p.38-43 English; Italian RELEASE OF VOLATILE DERIVATIVES FROM INITIATORS IN RADIATION CURING Visconti M; Cattaneo M; Li Bassi G Lamberti SpA Details are given of the development of a technique for the direct evaluation of volatile organic compounds during the radiation curing process. This method was used to evaluate the release of benzaldehyde from commercially available alpha-hydroxyketones during curing. 8 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.663242 Item 350 Iranian Journal of Polymer Science & Technology 10, No.2, Summer 1997, p.35-46 Persian APPLICATIONS OF HIGH-RESOLUTION SOLID-STATE CARBON 13 NMR SPECTROSCOPY TO POLYMERS Farahmand F G; Morshedian J Iran,Polymer Research Centre A brief review is given of the theory and applications of carbon 13 NMR to polymer analysis. Mention is made of conformational analysis, polymer reactions in solid state, analysis of crosslinked systems, homogeneity of polymeric blends, analysis of surface species, and variable temperature carbon 13 NMR solid state spectroscopy. 37 refs. IRAN

Accession no.663219

© Copyright 2002 Rapra Technology Limited

Item 351 Analytical Chemistry 69, No.23, 1st Dec.1997. p.4872-7 SAMPLE PRECONCENTRATION USING IONEXCHANGE POLYMER FILM FOR LASER ABLATION SAMPLING INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY Wing Tat Chan; Yip H H G Hong Kong,University An efficient sample pretreatment/introduction technique for the inductively coupled plasma atomic emission spectrometry (ICP-AES) using ion exchange for analyte preconcentration and matrix separation and laser ablation sampling for sample introduction was developed. Ammonium pyrrolidone dithiocarbamate-PS films were coated on glass plates for analyte preconcentration. 32 refs. HONG KONG

Accession no.662915 Item 352 Pigment & Resin Technology 26, No.6, 1997, p.370-7 FTIR SPECTROSCOPY OF LAC RESIN AND ITS DERIVATIVES Sarkar P C; Shrivastava A K Indian Council of Agricultural Research; Ranchi College Fourier transform infrared spectroscopy was applied to the study of lac resin, a complex natural resin of insect origin, and some of its derivatives. The results obtained by this method are compared with those from earlier studies that used classical methods of chemical analysis. Experiments include the preparation of hard and soft resins, dewaxed lac, ammoniated lac, lac acetal, halogenated lac, hydrolysed lac, rebuilt lac (rebulac), and the preparation of lac metal salts. It is found that FTIR has several advantages over classical methods, but that FTIR data requires supplementing by other instrumental techniques such as FT-Raman spectroscopy and solid state nuclear magnetic resonance. 21 refs. INDIA

Accession no.662758 Item 353 Journal of Vinyl and Additive Technology 3, No.3, Sept.1997, p.249-55 PRACTICAL GUIDE TO THE IDENTIFICATION OF MONOMERIC PLASTICIZERS IN FLEXIBLE PVC COMPOUNDS Kozlowski R R; Gallagher T K Aristech Chemical The performance of a flexible PVC compound is often defined by its plasticiser content and composition and a simple, accurate and fast method of plasticiser identification could, therefore, be an effective quality

121

References and Abstracts

control and benchmark performance test in new product development studies. Gas chromatography was shown to provide the most effective identification method and it was demonstrated that it could be complemented by IR spectroscopy, liquid chromatography and physical observations to confirm identity. 4 refs. USA

Accession no.661993 Item 354 Macromolecules 30, No.21, 20th Oct.1997, p.6674-6 HIGH-RESOLUTION CALORIMETRY STUDY OF THE ORDER-DISORDER TRANSITION IN A DIBLOCK COPOLYMER MELT Voronov V P; Buleiko V M; Podneks V E; Hamley I W; Fairclough J P A; Ryan A J; Mai S M; Liao B X; Booth C Russian Academy of Sciences; Leeds,University; UMIST; Manchester,University A new method is reported for locating the order-disorder transition in a diblock copolymer, namely high-resolution calorimetry, and the result compared with determinations by small-angle X-ray spectroscopy and rheology. 13 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; RUSSIA; UK; WESTERN EUROPE

Accession no.658801 Item 355 Polymer Science Series A 39, No.8, Aug.1997, p.953-7 STUDY OF SOLUBLE POLYAMIC ACIDS AND POLYESTER IMIDES BY METHODS OF EXCLUSION LIQUID CHROMATOGRAPHY Nesterov V V; Kudrysvtsev V V; Svetlichnyi V M; Gazdina N V; Bel’nikevich N G; Kurenbin O I; Zhukova T I St.Petersburg,Institute of Macromol.Compounds The molecular and conformation characteristics of a series of polyamic acids and polyester imides, obtained by hightemp. imidisation of polyamic acids in Nmethylpyrrolidinone or m-cresol, were studied by viscometry and exclusion liquid chromatography. The differences in the molec.wts. of the products of polyamic acid imidisation in N-methylpyrrolidinone and m-cresol were explained by the different characters of inactivation of the anhydride groups. 20 refs. (Full translation of Vys.Soed.A, 39, No.8, 1997, p.1387-91)

MEASUREMENT OF POLYDISPERSE POLYMERS FROM THEIR MATRIX-ASSISTED LASER DESORPTION/IONISATION TIME-OFFLIGHT MASS SPECTRA Vitalini D; Mineo P; Scamporrino E Istituto per la Chimica e la Tecnol.dei Mat.Pol.; Catania,Universita A recently reported off-line procedure to estimate molecular weight averages and MWD index, also for polydisperse polymers, directly from their matrix-assisted laser desorption/ionisation time-of-flight mass spectra (MALDI-TOF) was applied to poly(bisphenol Acarbonate), a poly(ether-sulphone resin) and poly(dimethylphenylene oxide), all having a wide polydispersity index. The molecular weight and MWD obtained values were compared with those determined by GPC or supplied by makers. A structural characterisation of these polymers was also performed by examining their MALDI-TOF mass spectra. 29 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.657168 Item 357 Injection Molding 5, No.10, Oct. 1997, p.60/2 MATERIALS ANALYST: PART 2. BRITTLE PPO Sepe M Dickten & Masch Mfg. The use is described of differential scanning spectroscopy (DSC) as an analytical tool in the diagnosis of part failure. Degradation of the polymer during processing is examined, and the example is investigated of a 30% glass reinforced PPO which showed brittleness and for which the causes of failure were revealed by means of DSC analysis. USA

Accession no.655661

Accession no.658622

Item 358 Macromolecular Symposia Vol.119, July 1997, p.317-24 CHEMICAL ANALYSIS OF POLYMERS USING TRANSMISSION ELECTRON MICROSCOPY/ ELECTRON ENERGY-LOSS SPECTROSCOPY: THE EXAMPLE OF POLY(ETHYLENE TEREPHTHALATE) Varlot K; Martin J M; Quet C; Kihn Y Lyon,Ecole Centrale; CEMES-LOE

Item 356 Macromolecules 30, No.18, 8th Sept.1997, p.5285-9 FURTHER APPLICATION OF A PROCEDURE FOR MOLECULAR WEIGHT AND MOLECULAR WEIGHT DISTRIBUTION

Electron energy-loss spectroscopy analysis of PETP was performed in the analytical TEM to evaluate the possibility of chemical analysis of the polymer at submicrometre scale. Due to irradiation damage, it was necessary to work at the lowest possible electron dose, and with the specimen cooled to liquid nitrogen temperature. In the acquired spectra, an identification of

RUSSIA

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References and Abstracts

the different chemical bondings in agreement with X-ray absorption near-edge spectroscopy experiments is proposed. 14 refs.

OF POLYETHYLENE AND N-ALKANES Parker S F Rutherford Appleton Laboratory

EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

High quality inelastic neutron scattering (INS) spectra of randomly oriented polycrystalline PE, polydeuteropolyethylene and highly oriented polyethylene are presented and a number of new features described. 9 refs.

Accession no.653745 Item 359 Macromolecular Symposia Vol.119, July 1997, p.309-15 CARBON-13, MAGNESIUM-25 AND BORON-11 SOLID STATE NMR STUDY OF A FIRE RETARDED ETHYLENE-VINYL ACETATE COPOLYMER Pecoul N; Bourbigot S; Revel B Ecole Nationale Superieure de Chimie de Lille; Centre Commun de Mesures RMN Flame retardance of ethylene-vinyl acetate copolymer can be achieved using magnesium hydroxide incorporated in the polymeric matrix. The adduct of a small amount of zinc borate as synergistic agent in the formulation increases the fire-proofing properties. Multinuclei solidstate NMR appears as a means to characterise materials before and after combustion. It was shown that endothermic dehydration, water vapour evolved and formation of a glassy coating provided the flame retardancy of interest to the polymer matrix. 12 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.653744 Item 360 Macromolecular Symposia Vol.119, July 1997, p.269-76 QUANTITATIVE ATR-FTIR SPECTROSCOPY AT POLYMER SURFACES: SORPTION AND MOLECULAR CONFORMATION Mueller M; Schmitt F J Dresden,Institute of Polymer Research Adsorption and diffusion phenomena at or within polymer systems were investigated by surface sensitive ATR-FTIR spectroscopy. For a systematic description, a study was made of (1) the competitive adsorption and desorption behaviour of proteins on polymer surfaces, (2) swelling of hydrophilic polymers by water molecules, which can be accompanied by conformational changes, and (3) induced orientational changes of hydrophobically modified polypeptides by apolar solvents. 10 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; WESTERN EUROPE

Accession no.653740 Item 361 Macromolecular Symposia Vol.119, July 1997, p.227-34 INELASTIC NEUTRON SCATTERING STUDIES

© Copyright 2002 Rapra Technology Limited

EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.653736 Item 362 Macromolecular Symposia Vol.119, July 1997, p.157-64 INFRARED ABSORPTION SPECTRA OF POLYMERS FROM CLASSICAL MOLECULAR SIMULATION Soldera A; Dognon J P CEA/Le Ripault A method is proposed to predict the IR spectra of amorphous polymers. Based on classical molecular simulation and Kramers-Kronig relations, it allows the computations of absorption and transmittance spectra of polymer films in near and middle infra-red domains with good agreement with experimental data. 22 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; WESTERN EUROPE

Accession no.653730 Item 363 Macromolecular Symposia Vol.119, July 1997, p.79-87 CREEP RATE SPECTROSCOPY USING A LASER INTERFEROMETER AS ULTRA-HIGH RESOLUTION TECHNIQUE FOR STUDY OF RELAXATIONS Peschanskaya N N; Yakushev P N; Sinani A B; Bershtein V A Russian Academy of Sciences An original laser interferometry creep rate spectroscopy (CRS) method was developed and used as the lowfrequency and high-resolution technique for studying microplasticity and relaxations in different materials including brittle ones. New possibilities for CRS for polymers are demonstrated. 13 refs. RUSSIA

Accession no.653722 Item 364 Macromolecular Symposia Vol.119, July 1997, p.49-63 POTENTIAL OF TWO-DIMENSIONAL NEARINFRARED CORRELATION SPECTROSCOPY IN STUDIES OF PRE-MELTING BEHAVIOUR OF NYLON 12

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References and Abstracts

Ozaki Y; Yongliang Liu; Noda I Kwansei-Gakuin,University; Procter & Gamble Co.

g PE; and 0.125 mg dioctadecyl-beta,beta’-thiodipropionate (Irganox PS 802) /1 g PE. 23 refs.

This review paper discusses the potential of generalised two-dimensional near-infrared correlation spectroscopy in studies of pre-melting behaviour and hydrogen bonds of nylon 12. A study on dissociation and hydrogen bonds of N-methylacetamide is also reviewed as a model compound study of nylon 12. FTIR spectra were measured over a temperature range of 30-150C where gradual weakening of inter- or intramolecular associative interactions and decrease of local order leading to the eventual fusion of nylon 12 crystals are observed. 24 refs.

AUSTRIA; WESTERN EUROPE

JAPAN; USA

Accession no.653720 Item 365 Macromolecular Symposia Vol.119, July 1997, p.25-48 UNDERSTANDING POLYMERS BY VIBRATIONAL SPECTROSCOPY: SOME RECENT ADVANCES IN THEORY AND EXPERIMENT Meier R J DSM Research A rapid scan version of two-dimensional spectroscopy is introduced and applied to study the phases of an acrylonitrile-butadiene-styrene polymer system. Some recent advances in the application of computational chemistry to the evaluation of vibrational spectra are presented. Some specific applications are discussed. 31 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; NETHERLANDS; WESTERN EUROPE

Accession no.653719 Item 366 International Journal of Polymer Analysis and Characterization 3, No.4, 1997, p.369-79 HPLC QUANTIFICATION OF THIOETHER ANTIOXIDANTS IN POLYETHYLENE AFTER DISSOLUTION OF POLYMER UNDER PRESSURE IN ALIPHATIC SOLVENT Macko T; Furtner B; Lederer K Leoben,Montan-Universitat A new method is described for the quantitative determination of some sulphur-containing antioxidants in PE. The polymer matrix is dissolved in hot n-heptane/ isopropyl alcohol, 97/3 v/v at 160 deg.C under elevated pressure (0.33 MPa) and precipitated by cooling. The solution is injected directly into a normal-phase silica gel column flushed with the same solvent as used for the dissolution of the polymer. This method gives high recovery of the antioxidants, good repeatability of the analysis and a low detection limit of 0.011 mg 4,4'-thiobis(3-methyl-6tert-butylphenol) (Santonox R) /1 g PE; 0.074 mg ditetradecyl-beta,beta’-thiodipropionate (Chimox 14) / 1

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Accession no.653220 Item 367 Macromolecular Symposia Vol.118, June 1997, p.383-8 FREE VOLUME STUDIES IN MISCIBLE POLYMER BLEND SYSTEMS Campbell J A; Goodwin A A; Ardi M S; Simon G P; Landry-Coltrain C J T Monash,University; Eastman Kodak Co. A brief review is presented of the published literature relating to the use of positron annihilation lifetime spectroscopy in studying the effects of miscibility on the free volume of miscible, amorphous polymer blends. Studies of a fully miscible polyvinyl phenol/PVAC blend, a partially miscible polyphenyl methacrylate/ polycarbonate blend and a largely immiscible PS/PVAC blend are reported. The results indicate that miscible blends tend to show a negative deviation of free volume size, and to a lesser degree free volume fraction, on mixing due to the intimacy of packing of the blend component macromolecules. The largely immiscible blend shows positive deviation of free volume size which is ascribed to additional free volume at the interface. 13 refs. AUSTRALIA; USA

Accession no.652994 Item 368 Journal of Polymer Science : Polymer Chemistry Edition 35, No.12, 15th Sept.1997, p.2431-9 ESR STUDY ON CHEMICAL CROSSLINKING REACTION MECHANISMS OF PE USING A CHEMICAL AGENT. II. EFFECT OF PHENOLIC ANTIOXIDANTS Yamazaki T; Seguchi T Hitachi Cable Ltd.; Japan,Atomic Energy Research Institute The effect of antioxidant on the reaction mechanism of chemical crosslinking of PE with dicumyl peroxide at high temperatures was investigated by ESR. The antioxidant reacted with the alkyl radicals in PE formed by the thermal decomposition of dicumyl peroxide above 120C and disturbed the crosslinking. 10 refs. JAPAN

Accession no.652659 Item 369 Applied Spectroscopy 51, No.8, Aug.1997, p.1176-8 QUANTITATION OF POLYETHYLENE GLYCOL CONCENTRATION USING RAMAN

© Copyright 2002 Rapra Technology Limited

References and Abstracts

SPECTROSCOPY Melendez Y; Schrum K F; Ben-Amotz D Purdue,University; Maryville College Raman spectroscopy is used to quantitate the amount of polymer in solution, in particular polyethylene glycol dissolved in chloroform. For various chain lengths and polymer weight fraction ranges, it is shown that the ratios of peak intensifies in the C-H stretching region may be used to quantitate polymer weight fraction with about 1% uncertainty. For low polymer weight fraction ranges (010%), the relationship between Raman intensity and polymer weight fraction is essentially linear, while at higher ranges (0-50%) the intensity follows a nonlinear function derived from basic concentration relationships and indicates a universal scaling with polymer chain length. 10 refs. USA

Accession no.652414 Item 370 Polymer 38, No.17, 1997, p.4381-5 SEPARATION AND IDENTIFICATION OF ETHYLENE-PROPYLENE BLOCK COPOLYMER Junting Xu; Linxian Feng; Shilin Yang; Yinan Wu; Yiqing Yang; Xiangming Kong Zhejiang,University; Shanghai,Research Institute of Petrochemical Technology A commercial impact resistant PP alloy was fractionated using the temperature rising elution fractionation technique and several ethylene-propylene block copolymers with different ethylene contents were obtained. The block structure of the fractions was identified by combining the fractionation results with carbon-13 NMR spectroscopy and DSC results. Some transition segments were found between PE and PP segments in the block copolymers. With increasing elution temperature, the number and kind of transition segments decreased, together with the length and melting temperature of the PE segment in the block copolymer fractions. 18 refs. CHINA

Accession no.651909 Item 371 Analyst 122, No.8, Aug.1997, p.777-81 DETERMINATION OF FINISHING OILS IN ACRYLIC FIBRES BY NEAR-INFRARED REFLECTANCE SPECTROMETRY Blanco M; Coello J; Fraga J M G; Iturriaga H; Maspoch S; Pages J Barcelona,Universidad Autonoma The potential of near-infrared diffuse reflectance spectrometry for quality control analyses in the textile

© Copyright 2002 Rapra Technology Limited

industry is explored with a view to the quantification of finishing oils in acrylic fibres by partial least-squares regression, using a rotary cuvette system for recording spectra. Calibration is performed with a set of samples that encompasses every source of variability, and the wavelength region where absorption is mostly due to the oil is used to construct several models from which that leading to the minimum relative standard error for a sample test set is selected. The results provided by various mathematical treatments used to minimise scattering resulting from the differential linear density of the samples reveal no significant differences between prediction errors. The model is used to quantify levels of finishing oil in routinely manufactured samples for a period of six months, during which time two batches show poor predictions due to a new component appearing in the product. Modification of the calibration model to account for this component substantially increases robustness and allows the accurate quantification of all batches manufactured after the model is developed. 28 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.651451 Item 372 Analyst 122, No.9, Sept.1997, p.101R-15R ANALYTICAL EXTRACTION OF ADDITIVES FROM POLYMERS Vandenberg H J; Clifford A A; Bartle K D; Carroll J; Newton I; Garden L M; Dean J R; Costley C T Leeds,University; ICI; Newcastle,University of Northumbria Plastics contain many other small molecules as well as the polymer itself. These include additives to alter the polymer properties or prolong the life of the polymer, such as plasticisers, antioxidants and UV light absorbers. There may also be processing aids, residual monomers, low molecular weight oligomers and inadvertent contaminants present. It is important for the manufacturer and regulators to know the level of these materials in the polymer to ensure the product is fit for its intended purpose. Food contact plastics are regulated by maximum concentrations allowable in the plastic, which applies to residual monomers and processing aids as well as additives. There are some methods for determining concentrations of additives without extraction from the polymer, such as nuclear magnetic resonance spectrometry, UV spectrometry and UV desorption-mass spectrometry. However, in order to determine the levels in the polymer, it is usually necessary to extract the compounds quantitatively from the plastic before analysis. A review is presented of the available extraction techniques. 102 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.651430

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References and Abstracts

Item 373 Analytical Chemistry 69, No.16, 15th Aug.1997, p.3304-13 QUANTITATIVE ANALYSIS OF PESTICIDES IN POST-CONSUMER RECYCLED PLASTICS USING OFF-LINE SUPERCRITICAL FLUID EXTRACTION(SFE)/GAS CHROMATOGRAPHY-ECD Nerin C; Batlle R; Cacho J Zaragoza,University

chromatography, is described. Fine and reproducible control of interaction between polymer chains and the alkyl chain bonded silica packing material can be achieved by varying the column temperature. The method can be used to characterise binary polymer mixtures, where one component is separated by the size exclusion mechanism and the other is simultaneously separated by the interaction mechanism in a single isocratic elution. The application of this technique to the characterisation of PS and PS/PMMA mixtures is examined. 12 refs.

The SFE of several organochlorine and organophosphorus pesticides and two metabolites from recycled plastics was studied. The recycled plastics, used as agricultural soil covers, were a mixture of LDPE and EVA. The SFE was optimised and compared with the classical sonication and total dissolution extraction methods. The plastic was extracted with supercritical carbon dioxide under different extraction conditions, depending on the physical matrix characteristics. Average recoveries of the eleven chemicals studied ranged from values greater than 90% with an overall relative standard deviation of 4.3% for plastics films to values lower than 40% with an overall standard deviation of 7.2% for plastics pellets. The variables affecting the whole extraction process and the results obtained in the comparison between the three extraction methods are discussed. 45 refs.

KOREA

EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.650545 Item 374 European Polymer Journal 33, No.7, July 1997, p.1135-42 FOURIER TRANSFORM INFRARED SPECTROSCOPY APPLIED TO THE STUDY OF PVC DECOMPOSITION Beltran M; Marcilla A Alicante,Universidad The process of PVC decomposition was studied by FTIR under dynamic conditions. The IR spectra were directly obtained from PVC films pyrolysed in-situ in a specially designed infra red cell. A qualitative description of the changes observed in the spectra was presented. 35 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; WESTERN EUROPE

Accession no.650382 Item 375 Macromolecular Symposia Vol.118, June 1997, p.261-5 HIGH PERFORMANCE LIQUID CHROMATOGRAPHY CHARACTERIZATION OF MACROMOLECULES Chang T; Lee H C; Lee W Pohang,University of Science & Technology A new chromatographic method for polymer molecular weight characterisation, temperature gradient interaction

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Accession no.649987 Item 376 Macromolecules 30, No.13, 30th June 1997, p.3781-7 CHARACTERISATION OF POLYESTERS BY MATRIX-ASSISTED LASER DESORPTION IONISATION MASS SPECTROMETRY Williams J B; Gusev A I; Hercules D M Pittsburgh,University A series of aliphatic polyesters, characterised by asymmetric oligomer distributions, heteroterminated linear chains, and cyclic oligomers, were studied using MALDI. Structural characterisation results were compared with those from fast atom bombardment mass spectrometry, electrospray ionisation mass spectrometry, NMR and endgroup titration. MALDI molecular weight determination was contrasted with those from GPC and NMR. 23 refs. USA

Accession no.649761 Item 377 Shawbury, Rapra Technology Ltd., 1997, pp.120. 12 ins. 15/4/97. Rapra Review Rept. No.95, vol.8, No. 11 1997, THERMAL ANALYSIS OF POLYMERS Sepe M P Dickten & Masch Mfg.Co. Edited by: Dolbey R (Rapra Technology Ltd.) Rapra Review Report No.95 A review is presented of the techniques involved in the thermal analysis of polymers. Techniques discussed include differential scanning calorimetry, differential photocalorimetry, thermogravimetric analysis, thermomechanical analysis, dynamic mechanical analysis, dielectric, thermally stimulated current/relaxation map analysis analysis, and thermal conductivity analysis. 381 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.647258 Item 378 Journal of Applied Polymer Science 65, No.3, 18th July 1997, p.595-600

© Copyright 2002 Rapra Technology Limited

References and Abstracts

MOLECULAR WEIGHT OF POLYETHYLENE GLYCOLS BY VAPOR PRESSURE OSMOMETRY: AN ALTERNATIVE DATA TREATMENT Sabadini E; Assano E M; Atvars T D Z Campinas,Universidade Estadual The number-average molec.wt. of some polyethylene glycols was analysed using vapour pressure osmometry. This technique generally worked with a plot of the difference in electrical resistance/concentration versus concentration and the molec.wt. was determined by the calibration constant obtained from the curve intercept. It was demonstrated that this method induced a high dispersion of the data, which could be minimised using a plot of difference in electrical resistance versus concentration.. More precise values of molec.wt. could thus be obtained and the number-average molec.wt. of several polyethylene glycols could be directly obtained from the ratio between the curve slopes obtained for a standard and the polymer sample. 10 refs. BRAZIL

Accession no.645677 Item 379 Speciality Chemicals 17, No.5, June/July 1997, p.165/70 MAKING LIQUID CHROMATOGRAPHY MORE ACCESSIBLE Kuehler T C; Sellen M; Lavold T; Batt J; Langridge J; Raso R; Rontree J A Astra Hassle AB; Micromass AB; Micromass UK Ltd. Until recently, mass spectrometry was regarded as a highly sophisticated technique requiring careful use of the instrument by a sole operator, and demanding meticulous sample preparation by the chemist. However, moves towards open-access, chemist-operated systems have been reported on mass spectrometers equipped with a variety of ionisation modes. The reliability and robustness of atmospheric pressure ionisation, the ease and speed of source tuning, the fact that it is unnecessary to optimise the source conditions for each sample individually and the reproducibility of results have made API techniques the ionisation methods of choice. Details are given. 5 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; SCANDINAVIA; SWEDEN; UK; WESTERN EUROPE

Accession no.645281 Item 380 Polymer Degradation and Stability 57, No.2, 1997, p.135-49 THERMAL DEGRADATION KINETICS OF POLYPROPYLENE. III. THERMOGRAVIMETRIC ANALYSIS Chan J H; Balke S T Toronto,University Thermogravimetric data were obtained for the pyrolysis of polypropylene, and several previously published

© Copyright 2002 Rapra Technology Limited

interpretation methods were applied to the data. The wide temperature range used in this work (45-580C) encompassed a change in the decomposition mechanism and this greatly limited the utility of the methods. To accommodate this mechanism change, the data were treated as a pseudo-first order reaction. The lower activation energy occurring at lower degradation temperatures was attributed to scission of the ‘weak links’ in the polymer. The higher activation energy was similar to the carbon-carbon dissociation energy and was associated with random scission throughout the polymer. 47 refs. CANADA

Accession no.645116 Item 381 Polymer Degradation and Stability 57, No.2, 1997, p.113-25 THERMAL DEGRADATION KINETICS OF POLYPROPYLENE. I. MOLECULAR WEIGHT DISTRIBUTION Chan J H; Balke S T Toronto,University A kinetic model for the thermal degradation of PP was developed and fitted to MWD data obtained by high temperature size exclusion chromatography. In a series of ampoule experiments, reaction temperatures of 275315C were examined with reaction times of up to 48 h. A single-parameter version of the model, containing an apparent rate constant, was found to provide excellent fits of all MWDs. Values of the parameter varied with both temperature and reaction time. 35 refs. CANADA

Accession no.645114 Item 382 Analytical Chemistry 69, No.13, 1st July 1997, p.2485-95 MASS SPECTROMETRIC INVERSE GAS CHROMATOGRAPHY: INVESTIGATION OF POLYMERIC PHASE TRANSITIONS Panda S; Bu Q; Huang B; Edwards R R; Liao Q; Yun K S; Parcher J F Mississippi,University An improved inverse gas chromatographic method involving the use of a mass-specific detector for determination of the Tg of polymeric materials is described. This new method allows the use of several probe solutes simultaneously with an automated, closedloop injector and stepped temperature programming. The result is a single continuous chromatogram for each probe solute over a range of temperatures encompassing the Tg. Several different methods for the exact determination of Tg from the chromatogram were investigated. Two new methods were also proposed for the evaluation of Tg from either the temperature dependence of the second moments

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References and Abstracts

of the elution peaks for probe solutes or simple inspection of the variation of elution peak height (width) with temperature. 51 refs. USA

Accession no.645093 Item 383 Analytical Chemistry 69, No.12, 15th June 1997, p.15R-28R COATINGS Anderson D G Witco Corp. A review is presented of analytical techniques applicable to the examination of coatings, raw materials and substrates since 1995. The most highly referenced areas were found to be IR spectroscopy, NMR, HPLC, thermal analysis and gas chromatography. 704 refs. USA

Accession no.640310 Item 384 Polymer Bulletin 38, No.6, June 1997, p.681-8 SEPARATION OF BLOCK COPOLYMERS FROM PARENT HOMOPOLYMERS BY MEANS OF LIQUID CHROMATOGRAPHY AT THE CRITICAL ADSORPTION POINT Janco M; Berek D; Onen A; Fischer C H; Yagci Y; Schnabel W Slovak Academy of Sciences; Istanbul,Technical University; Hahn-Meitner-Institut Berlin GmbH The principle underlying the above method is described and results of its application to block copolymers consisting of methyl methacrylate and tetrahydrofuran blocks are presented and discussed. The technique is shown to be suitable for characterisation of block copolymers with regard to the presence of homopolymer and multiblock (triblock) fractions. 5 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; SLOVAK REPUBLIC; SLOVAKIA; TURKEY; WESTERN EUROPE

Accession no.640169 Item 385 Antec 97. Volume III. Conference proceedings. Toronto,27th April-2nd May 1997,p.3588-92. 012 FOURIER TRANSFORM INFRARED MICRO SPECTROSCOPY MAPPING. APPLICATIONS TO VINYL SIDING INDUSTRY Garcia D; Black J Elf Atochem North America Inc. (SPE) Fourier transform IR (FTIR) spectroscopy is a powerful analytical technique capable of yielding high quality information with a spacial resolution as low as 10 microns.

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When coupled with an automated mapping stage, it can offer unique evaluation capabilities. A number of applications of FTIR spectroscopy mapping to the vinyl siding industry are described. Examples focus on determining, in single sample mapping experiments, the compositional changes associated with capstock to substrate transition and evaluating the degradation species and level observed during weathering exposure throughout the thickness of the siding panel. 4 refs. USA

Accession no.639927 Item 386 Antec 97. Volume II. Conference proceedings. Toronto, 27th April-2nd May 1997, p.2310-4. 012 QUANTITATIVE ANALYSIS OF LDPE/LLDPE BLEND USING DSC AND FTIR METHODS Prasad A; Mowery D Quantum Chemical Co. (SPE) A blend of LDPE and LLDPE is widely used for blown film applications. For quality control an accurate and rapid method is required to identify the type and composition of alpha-olefin in an LDPE/LLDPE blend. A rapid, accurate and new test method is developed which utilises DSC and FTIR techniques. The melting point of LDPE varies with density and usually is in the range of 106 deg.C to 112 deg.C for film grade resins. The DSC thermogram of LLDPE is characterised by a broad range of melting with a lower melting peak around 106 deg.C to 110 deg.C and a higher one in the range of 120 deg.C to 124 deg.C. In the blend with LDPE, the ratio of the two endothermic peak heights changes. At a given weight percent of LDPE, this ratio depends on the type of LLDPE. The separate calibrations for butene-1, hexene-1, and octene-1 LLDPEs are developed to quantify the blend composition from DSC thermograms provided the alpha-olefin type is identified by a rapid method such as FTIR. 17 refs. USA

Accession no.638387 Item 387 Shawbury, Rapra Technology Ltd., 1992, pp.112. 12ins. 30/6/97. Rapra Review Rept. No.61, Vol.6, No.1, 1992. FOOD CONTACT POLYMERIC MATERIALS Sidwell J Rapra Technology Ltd. Edited by: Dolbey R (Rapra Technology Ltd.) Rapra Review Report No.61 A review is presented of the current and proposed European legislation on materials in contact with food, as well as the latest technological advances. With reference to legislation, details are given of EC directives issued, their implementation, FDA regulations, recycling and waste management legislation. Technical

© Copyright 2002 Rapra Technology Limited

References and Abstracts

developments in food contact materials cover barrier polymers in multilayer packaging films, migration of species from food contact materials, and methods of analysis of multilayer food contact materials. 485 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.637749 Item 388 Polymer 38, No.12, 1997, p.3035-43 CHARACTERIZATION OF POLYETHYLENE TEREPHTHALATE AND POLYETHYLENE TEREPHTHALATE BLENDS Fox B; Moad G; van Diepen G; Willing I; Cook W D CSIRO,Div.of Chemicals & Polymers; Monash,University A method was developed for direct determination of the molec.wt. of the PETP component in PETP/ABS blends by GPC. The technique was used to demonstrate that an observed deterioration in the mechanical properties, e.g. Izod impact strength, of PETP/ABS blends on processing could be correlated with a decrease in the molec.wt. of the PETP component. Various methods for evaluating the molec.wt. and the chemical microstructure of PETP were examined. The use of NMR spectroscopy as a means of quantitatively identifying end groups and comonomers that were present at the 1-4% level in commercial PETP was critically evaluated with reference to the stability of PETP and PETP end groups in various NMR solvents. New proton NMR chemical shift assignments for cyclohexanedimethanol units are presented and the reactivity of hydroxy end groups in trifluoroacetic acid mixtures is examined. 34 refs. AUSTRALIA

Accession no.636573 Item 389 Polymer Testing 16, No.2, 1997, p.193-8 NMR CARBON-13 HIGH RESOLUTION STUDY OF POLY(ETHYLENE-CO-VINYL ACETATE) Stael G C; Tavares M I B CCT/UENF EVA was analysed by carbon-13 high-resolution using NMR employing solution and solid state techniques. The analyses of this copolymer by solution NMR permitted the copolymer composition to be obtained, and using solid-state NMR, a study of molecular mobility was carried out. Both studies were made to correlate the structure and properties. 9 refs. BRAZIL

5, No.3, March 1997, p.97-102 CHARACTERISATION OF POLYMER BLENDS BY INVERSE GAS CHROMATOGRAPHY Al-Saigh Z Y Ohio,State University A brief review is presented of the use of inverse gas chromatography to characterise polymer blends. Comparisons between data from inverse gas chromatography and DSC are discussed. 23 refs. USA

Accession no.632110 Item 391 Polymer News 22, No.1, Jan.1997, p.15 POLYMER ANALYSIS AND CHARACTERISATION. SOLID STATE NMR: IS IT BECOME TRULY POPULAR? Garbassi F EniChem SpA A very brief review is presented of specific areas where solid state NMR can contribute to polymer analysis. Mention is made of polymer morphology, interactions, dynamics and polymer reactions. 10 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; WESTERN EUROPE

Accession no.632071 Item 392 Analytical Chemistry 69, No.4, 15th Feb.1997, p.618-22 COMPOSITION AND MICROSTRUCTURE ANALYSIS OF CHLORINATED POLYETHYLENE BY PYROLYSIS GAS CHROMATOGRAPHY AND PYROLYSIS GAS CHROMATOGRAPHY/MASS SPECTROMETRY Cheng-Yu Wang F; Smith P B Dow Chemical Co. A pyrolysis gas chromatography method was developed to determine the composition and microstructure of chlorinated PE (CPE). The method used specific aromatic compounds which were formed through dehydrochlorination of trimers after pyrolysis of CPE polymers at elevated temperatures. The composition and microstructure calculation was based on the difference between the levels of ethylene and vinyl chloride trimers formed. The composition of CPE polymers used in this study was corroborated with carbon-13 NMR results and the manufacturers product specification. 23 refs. USA

Accession no.629089

Accession no.634101 Item 390 Trends in Polymer Science

© Copyright 2002 Rapra Technology Limited

Item 393 Biomaterials 18, No.5, March 1997, p.415-9

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References and Abstracts

DETECTION OF PEROXY SPECIES IN ULTRAHIGH MOLECULAR WEIGHT POLYETHYLENE BY RAMAN SPECTROSCOPY Chenery D H Smith & Nephew Group Research Centre Samples of gamma-sterilised UHMWPE were examined using infra-red and Raman spectroscopies. The purpose of this study was to detect the peroxy intermediates by the novel use of Raman spectroscopy to confirm that oxidation proceeded by this mechanism. 16 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.625483 Item 394 Polymer 38, No.1, 1997, p.1-7 MODULATED DIFFERENTIAL SCANNING CALORIMETRY: 6. THERMAL CHARACTERISATION OF MULTICOMPONENT POLYMERS AND INTERFACES Hourston D J; Song M; Hammiche A; Pollock H M; Reading M Loughborough,University of Technology; Lancaster,University; ICI Paints A quantitative thermal method, based on the differential of heat capacity signal from modulated temperature differential scanning calorimetry, was described for determining the weight fraction of interface and the extent of phase separation in polymer materials. The interface was modelled as discrete fractions, each with its own characteristic increment of heat capacity. The materials used to demonstrate the range of the method were PS blended with poly(phenylene oxide) (PPO), pure PS, pure PPO, a styrene-isoprene-styrene triblock copolymer (SIS), SIS blended with PPO, PMMA/poly(vinyl acetate) blends and PVC sandwiched with poly(n-butyl acrylate). Twophase and four-phase systems were used. The calculated results agreed well with experimental results for two- and four-phase systems. 20 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.621625 Item 395 Analytical Chemistry 69, No.1, 1st Jan.1997, p.66-71 LIQUID CHROMATOGRAPHY AT THE CRITICAL CONDITION USING ENHANCEDFLUIDITY LIQUID MOBILE PHASES Souvignet I; Olesik S V Ohio,State University The use of enhanced-fluidity liquid mixtures of THF and carbon dioxide for liquid chromatography at the critical condition was examined. For PS polymers, the molec.wt. range that could be analysed at the critical condition was

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compared for THF/carbon dioxide and other common liquid mixtures. As enhanced-fluid liquids were highly compressible, it was possible to reach the critical condition by changing the pressure of the THF/carbon dioxide mixture. Approaching the critical condition by pressure variation was compared with that possible with temp. changes. Pressure variation was a more accurate and reproducible means of reaching the critical condition than temp. variation. Finally, THF/carbon dioxide mixtures were used as mobile phases at the critical condition for PS to characterise styrene-methyl acrylate copolymers. 25 refs. USA

Accession no.620015 Item 396 Shawbury, Rapra Technology Ltd., 1995, pp.108. 12ins. 18/7/95. Rapra Review Rept. Vol.7, No.11, 1995, MOLECULAR WEIGHT CHARACTERISATION OF SYNTHETIC POLYMERS Holding S R; Meeham E Rapra Technology Ltd.; Polymer Laboratories Ltd. Edited by: Dolbey R (Rapra Technology Ltd.) Rapra Review Report No. 83 Techniques are examined for the determination of the molecular weight distribution and molecular weight averages of synthetic polymers. The use is discussed of gel permeation chromatography in combination with other techniques such as light scattering and viscometry to provide information about the molec.wt. of a polymer and potentially significant information on the composition of copolymers and blends. The use of solution viscosity is also examined as a valuable quality control technique. 411 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; UK; WESTERN EUROPE

Accession no.556661 Item 397 Analytical Chemistry 60,No.9,1st May 1988,p.932-7 IDENTIFICATION OF DYES IN SOLID POLYMETHYL METHACRYLATE BY MEANS OF LASER DESORPTION FOURIER TRANSFORM ION CYCLOTRON RESONANCE MASS SPECTROMETRY Hsu A T;Marshall A G OHIO STATE,UNIVERSITY It is demonstrated that the above technique can detect and identify (by chemical formulae) dyes in solid PMMA commercial plastics at concentrations at least on order of magnitude lower (0.1% vs 1-2wt%) than those obtained by the best currently-available alternative method (ATR Fourier transform IR spectrometry). Both untreated and redissolved PMMA can be characterised, in the presence and absence of up to three dyes in a single sample. 44 refs. USA

Accession no.357996

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References and Abstracts

Item 398 Oxford, Pergamon Press Ltd., 1984, pp.ix,445. LS.24.50. 9ins. 2copies. 12/7/85. Analytical Chemistry Vol.8. 91T ANALYSIS OF PLASTICS Crompton T R This book covers all aspects of the analysis of plastics by chemical and physical methods. It is divided into eight chapters which each deal with a particular polymer or group of polymers:- polyolefins, polypropylene, higher alkene polymers, styrene polymers, chlorine-containing polymers, methacrylates, polybutadienes, polyesters and polyethers. The techniques discussed include spectroscopy, chromatography, fractionation,, X-ray diffraction, autoradiography, DTA, TGA and DSC. UK

Accession no.280400 Item 399 Weinheim, Verlag Chemie GmbH, 1981, pp.XV,687. 12ins. 22/3/82. R.ROOM. 91T ATLAS OF POLYMER AND PLASTICS ANALYSIS. VOL.3....ADDITIVES AND PROCESSING AIDS: SPECTRA AND METHODS OF IDENTIFICATION. 2ND REV.EDN. Scholl F

processing aids are presented. Over 1300 IR spectra and 60 UV spectra are included. The functions and compositions as well as the physical and chemical methods of identification of the following materials are discussed: plasticisers, fillers, pigments, antioxidants, UV stabilisers, optical brighteners, antistatic agents, biostabilisers, flame retardants, lubricants, accelerators, hardeners and blowing agents. 608 refs. Accession no.211056 Item 400 Members Rept.49 Shawbury, 1980, pp.12. 12ins. 2copies. 26/6/80. 91T HIGH PERFORMANCE LIQUID CHROMATOGRAPHY - ANALYTICAL APPLICATIONS IN THE RUBBER AND PLASTICS INDUSTRIES Sidwell J A Rubber & Plastics Research Assn.of Gt.Britain RUBBER & PLASTICS RA.MEMBERS REPT.049 This report details some of the high-performance liquid chromatography work carried out at RAPRA and reviews reported in the literature. 11 refs. RUBBER & PLASTICS RESEARCH ASSN.OF GT.BRITAIN Accession no.154074

The spectroscopic and chromatographic data that are required for the identification of plastics additives and

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References and Abstracts

132

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Subject Index

Subject Index A ABS, 160 164 207 225 345 365 388 398 ABSORPTION, 56 226 297 306 374 382 ABSORPTION SPECTRA, 274 ABSORPTION SPECTROSCOPY, 358 362 ACCELERATOR, 399 ACCURACY, 131 ACETIC ACID, 76 266 ACETONE, 185 224 266 311 ACETONITRILE, 21 266 ACID, 277 288 ACOUSTIC MICROSCOPY, 126 ACRYLATE, 269 ACRYLIC, 199 ACRYLIC ACID COPOLYMER, 172 217 348 ACRYLIC POLYMER, 33 172 255 299 314 335 371 384 397 ACRYLIC-MELAMINE RESIN, 44 175 ACRYLONITRILE, 119 ACRYLONITRILE COPOLYMER, 57 ACRYLONITRILE-STYRENE COPOLYMER, 72 110 220 345 ACTIVATION ENERGIES, 49 75 146 169 280 288 317 328 380 381 ADDITIVE, 29 36 71 89 99 107 108 112 124 128 132 151 161 171 178 181 199 201 206 225 226 250 272 288 289 302 306 318 324 325 353 366 372 377 387 391 397 399 ADHESION, 32 61 62 145 157 167 176 202 223 231 236 237 247 249 312 316 341 346 ADHESIVE, 9 20 62 167 168 179 272 346 ADSORPTION, 46 56 65 93 103 178 203 210 221 241 285 319 339 360 384 ADSORPTION CHROMATOGRAPHY, 105 210 AEROPLANE, 36 62 121 AFFINITY CHROMATOGRAPHY, 50 97 AGEING, 66 80 86 88 112 148 152 274 288 298 309 338 377 ALCOHOL, 56 235 288 ALCOHOLYSIS, 39

ALKYD RESIN, 237 ALPHA TRANSITION, 245 290 328 ALUMINIUM, 126 168 179 223 266 ALUMINIUM HYDROXIDE, 211 ALUMINIUM OXIDE, 6 AMINE, 36 48 130 151 161 178 272 AMMONIUM PYRROLIDONE DITHIOCARBAMATE, 351 AMMONIUM SALT, 258 AMORPHOUS, 14 54 74 78 99 117 141 170 207 213 274 283 340 362 367 ANISOTROPY, 13 256 324 ANNEALING, 24 54 74 101 135 136 277 308 338 342 ANTI-STICK AGENT, 6 ANTIMONY, 95 ANTIOXIDANT, 65 86 93 107 132 171 183 195 286 288 366 368 372 387 399 ANTISTATIC AGENT, 399 AQUEOUS, 46 198 223 232 ARAMID FIBRE, 281 AROMA, 56 57 AROMATIC, 48 125 192 278 288 299 392 ATMOSPHERIC PRESSURE, 50 206 222 ATOMIC ABSORPTION SPECTROSCOPY, 177 ATOMIC EMISSION SPECTROSCOPY, 95 177 218 273 351 ATOMIC FORCE MICROSCOPY, 30 38 44 58 59 62 108 115 118 142 145 154 167 179 191 219 277 ATTENUATED TOTAL REFLECTANCE SPECTROSCOPY, 43 61 69 126 257 262 301 360 AUGER ELECTRON SPECTROSCOPY, 13 AUTOMATION, 46 50 212 278 382 AUTOMOTIVE APPLICATION, 44 56 62 67 175 202 212 236 329 AUTOOXIDATION, 169

B BACKSCATTERED ELECTRON IMAGING, 289 BAG, 266 BAGASSE, 100

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BAND STRUCTURE, 262 BARIUM SULPHATE, 40 BARRIER PROPERTIES, 56 57 86 94 168 387 BENZENE, 382 BETA RELAXATION, 325 BIAXIALLY ORIENTED, 104 BIOCOMPATIBLE, 42 BIODEGRADABLE, 37 112 267 387 BIODETERIORATION, 5 37 112 246 267 387 BIOMATERIAL, 42 46 246 262 BIOMEDICAL APPLICATION, 262 BIREFRINGENCE, 257 284 BISPENTAMETHYLPIPERIDYL SEBACATE, 66 BISPHENOL A, 200 222 272 356 BISPHENOL A COPOLYMER, 189 BISPHENOL A DIGLYCIDYL ETHER, 178 BISPHENOL A EPOXY RESIN, 11 BISPHENOL A POLYCARBONATE, 4 29 78 135 159 322 367 BISPHENOL DIGLYCIDYL ETHER, 178 BLEND, 11 12 15 25 47 58 60 63 64 69 72 77 91 98 107 110 112 125 137 139 146 147 151 156 186 188 193 209 213 220 228 234 246 309 331 340 347 348 363 367 375 377 386 388 390 391 394 BLOCK COPOLYMER, 127 193 274 354 370 384 394 BLOW MOULDING, 313 323 BLOWING AGENT, 302 399 BLOWN FILM, 324 386 BODY ARMOUR, 281 BOILING POINT, 120 185 266 BONDING, 32 168 202 BONDING AGENT, 168 179 BONNET, 329 BOTTLE, 57 131 212 266 313 323 BOUND WATER, 51 BOUNDARY LAYER, 81 BRANCHING, 18 35 60 102 200 216 BRITTLE, 41 62 271 289 357 363 BROMINE CONTAINING COPOLYMER, 273

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Subject Index

BUCKET, 67 BUILDING APPLICATION, 7 385 BULK MOULDING COMPOUND, 202 BUMPER, 67 BUTYL ACRYLATE COPOLYMER, 28 198 BUTYL METHACRYLATE COPOLYMER, 166 190 BUTYLENE COPOLYMER, 102 113

C CALCINED CLAY, 324 CALCIUM CARBONATE, 65 211 289 324 CALCULATION, 8 14 77 98 114 149 162 172 190 227 276 277 285 290 310 323 328 330 337 344 362 382 390 392 394 CALIBRATION, 6 47 173 190 208 216 229 238 270 297 309 310 319 334 378 392 CALORIMETRY, 9 61 64 65 74 88 133 150 154 186 290 302 305 313 354 359 CAPILLARY ELECTROPHORESIS, 46 50 97 CAPILLARY GAS CHROMATOGRAPHY, 76 CAPILLARY RHEOMETRY, 324 325 CAR, 56 67 CARBON 13, 130 193 209 265 268 297 359 370 389 392 CARBON BLACK, 40 93 CARBON DIOXIDE, 57 298 301 311 373 395 CARBON DISULPHIDE, 311 CARBON FIBRE-REINFORCED PLASTIC, 36 178 182 196 231 320 CARBONYL GROUP, 274 288 CARBOXYLIC ACID, 288 341 CASTING, 94 262 367 CELLULAR MATERIAL, 80 84 85 97 302 CELLULOSE, 43 82 263 CELLULOSE ACETATE, 79 CELLULOSE NITRATE, 46 79 185 CEMENT, 276 CHAIN LENGTH, 272 274 CHAIN SCISSION, 274 380 CHAR, 194 CHEMICAL BONDING, 358

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CHEMICAL COMPOSITION, 25 72 80 89 103 107 146 159 172 197 198 211 213 229 232 289 318 CHEMICAL FORCE MICROSCOPY, 58 CHEMICAL IONISATION MASS SPECTROSCOPY, 222 CHEMICAL REAGENT, 53 334 CHEMICAL RECYCLING, 39 CHEMICAL RESISTANCE, 57 175 CHEMICAL STRUCTURE, 1 8 12 16 25 31 47 49 51 53 56 66 68 73 77 83 89 93 98 102 103 114 130 133 140 152 158 159 164 166 168 180 200 222 228 229 243 264 268 269 274 275 277 283 284 286 291 300 301 308 310 317 318 328 331 334 337 355 356 364 365 368 370 376 382 391 CHEMILUMINESCENCE, 88 CHEMOMETRIC ANALYSIS, 140 216 CHINA CLAY, 226 306 CHITIN, 246 CHLORINATED POLYETHYLENE, 146 392 CHLORINE, 17 194 373 CHLORODIFLUOROETHANE, 337 CHLOROFORM, 3 208 369 382 CHROMATOGRAPHIC ANALYSIS, 66 81 86 89 96 97 105 112 119 137 141 152 171 191 194 229 235 303 304 366 375 382 384 CHROMATOGRAPHY, 3 21 25 28 29 30 34 35 39 40 46 50 52 53 55 56 60 66 71 72 75 80 81 84 86 87 89 96 97 102 103 105 107 108 112 113 114 116 119 120 124 128 137 141 152 158 159 160 166 169 171 172 174 183 185 186 190 191 194 195 200 203 204 206 208 210 218 222 229 233 235 239 240 241 242 243 259 264 273 278 285 295 299 303 304 307 310 311 314 319 322 325 334 349 353 355 356 366 372 373 375 376 379 381 382 383 384 388 395 398 399 CHROMIC ACID, 61 CHROMOGEN, 16 288 CLAY, 324 CLEARCOAT, 27 44 175

CLOUD POINT, 12 98 125 COATED FIBRE, 179 COATED METAL, 157 227 COATING, 19 27 44 62 66 121 126 138 163 168 174 175 185 217 222 223 227 236 237 239 255 259 266 298 312 325 359 383 COBALT STEARATE, 348 COHESION, 94 145 167 COLOUR, 274 288 COLOURANT, 181 COLUMN CHROMATOGRAPHY, 233 375 COLUMN PACKING, 50 203 235 241 319 375 COMBUSTION, 359 COMPATIBILITY, 63 90 209 331 340 COMPLEX VISCOSITY, 325 COMPOSITE, 10 13 17 36 62 79 81 82 90 100 134 141 176 178 179 182 196 197 199 202 211 231 234 258 265 271 281 288 289 296 318 320 333 339 357 377 COMPOSITION, 72 73 100 122 123 130 220 241 243 389 392 394 COMPUTER AIDED ANALYSIS, 46 67 108 173 174 214 309 COMPUTER MODEL, 144 152 174 338 COMPUTER SIMULATION, 248 367 CONCENTRATION, 55 102 105 129 130 183 197 215 224 250 262 283 300 311 317 339 353 378 CONE CALORIMETER, 150 359 CONFOCAL RAMAN MICROSPECTROSCOPY, 168 342 CONFORMATIONAL ANALYSIS, 360 CONTACT ANGLE, 37 61 202 217 277 333 343 CONTACT LENS, 265 CONTAINER, 57 266 278 CONTAMINATION, 17 128 160 181 289 357 COOLING, 57 67 139 309 323 324 358 COOLING RATE, 57 126 207 309 323 324 COPOLYESTER, 204 322 COPOLYETHERSULPHONE, 47 COPOLYMER COMPOSITION, 28 57 70 94 198 210 220 370

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Subject Index

COPPER, 61 316 317 CORONA TREATMENT, 205 CORRELATION SPECTROSCOPY, 344 364 CORROSION, 255 271 CREEP RATE SPECTROSCOPY, 363 CRESOL, 355 CRITICAL CONCENTRATION, 241 CRITICAL POINT, 103 395 CRITICAL SOLUTION TEMPERATURE, 125 CROSS-POLARISATION, 193 209 268 300 CROSSLINK, 83 279 CROSSLINK DENSITY, 179 269 CROSSLINKED, 110 179 221 250 CROSSLINKING, 9 10 20 24 27 36 46 48 49 73 85 115 134 161 180 187 265 272 279 288 294 300 309 326 368 377 CROSSLINKING AGENT, 222 288 CRYSTALLINE, 2 59 143 147 283 313 CRYSTALLINITY, 2 13 24 42 54 57 62 63 64 69 94 102 113 114 117 122 126 131 139 143 147 168 257 260 274 277 281 291 309 313 323 357 364 367 377 391 CRYSTALLISATION, 2 9 12 13 22 24 26 52 54 57 59 74 78 107 117 122 131 136 139 147 148 155 170 246 261 295 309 323 329 332 336 386 CRYSTALLISATION TEMPERATURE, 136 309 CRYSTALLITE, 57 139 260 CURE TEMPERATURE, 2 48 161 CURE TIME, 36 265 309 CUREMETER, 134 CURING, 8 20 27 36 68 73 83 89 138 144 149 161 163 178 182 187 247 248 265 269 272 300 305 309 312 316 349 377 CURING AGENT, 36 151 161 178 182 222 250 272 288 317 CYCLOHEXANE, 21 263 285

D DATA ANALYSIS, 13 216 237 267 291 319 DATA COLLECTION, 291 345 DEBONDING, 236 DECANE, 382

DEFECT, 67 88 126 289 329 DEFORMATION, 41 59 67 249 277 283 DEGRADABLE, 37 112 267 387 DEGRADATION, 4 16 39 44 58 65 66 80 85 86 87 88 92 94 101 112 119 135 148 152 164 175 183 189 194 195 213 228 244 258 266 267 274 279 288 294 298 302 309 311 318 325 326 330 338 347 357 374 377 380 385 DEGRADATION PRODUCT, 4 17 34 75 87 112 128 152 175 183 194 274 279 288 DEGRADATION TEMPERATURE, 194 269 380 DEGREE OF BRANCHING, 18 35 DEGREE OF CROSSLINKING, 9 27 300 377 DEGREE OF CRYSTALLINITY, 143 313 DEGREE OF CURE, 10 36 269 DEHYDROCHLORINATION, 146 392 DELAMINATION, 255 312 DENSITY, 18 52 56 106 131 168 179 216 231 261 289 313 367 DENTAL APPLICATION, 172 247 276 343 346 DEPOLYMERISATION, 39 165 266 DEPTH PROFILING, 205 333 342 344 DERIVATIVE THERMOGRAVIMETRY, 380 DESORPTION, 71 93 104 210 310 360 DETECTION LIMIT, 56 174 289 DIACID, 288 341 DIBUTYL PHTHALATE, 76 DIBUTYL SEBACATE, 277 DICHLOROXYLENE, 48 DICHROISM, 284 DICUMYL PEROXIDE, 368 DICYANATE POLYMER, 11 DIELECTRIC ANALYSIS, 9 377 DIELECTRIC CONSTANT, 46 237 338 DIELECTRIC PROPERTIES, 46 245 338 DIELECTRIC RELAXATION SPECTROSCOPY, 49 110 259 338 DIELECTROMETRY, 9 DIETHYLENE GLYCOL, 26 121 266 DIFFERENTIAL

© Copyright 2002 Rapra Technology Limited

INTERFERENCE MICROSCOPY, 324 DIFFERENTIAL PHOTOCALORIMETRY, 377 DIFFERENTIAL SCANNING CALORIMETRY, 2 6 7 8 10 11 12 15 17 18 20 22 24 29 36 41 51 54 56 63 64 65 74 77 78 83 85 88 94 95 98 101 110 113 114 122 125 126 131 133 134 135 136 139 144 146 147 149 154 155 161 163 164 170 186 187 207 211 213 220 245 246 252 253 254 258 261 267 269 276 277 280 282 287 290 291 296 302 305 309 313 323 324 328 329 332 336 348 357 367 370 377 382 386 387 390 394 398 DIFFERENTIAL THERMAL ANALYSIS, 2 6 7 8 10 12 15 17 18 20 22 24 29 36 41 54 56 63 64 65 74 77 78 83 88 94 95 98 101 110 113 114 122 125 126 131 133 134 136 139 144 146 147 149 154 155 161 163 164 170 186 187 207 211 213 231 245 246 252 253 254 258 267 269 276 277 280 287 290 291 296 302 309 313 323 324 328 329 332 336 348 357 367 370 377 382 386 387 390 398 DIFFUSE REFLECTANCE SPECTROSCOPY, 341 DIFFUSION, 9 56 80 99 124 125 264 274 346 351 360 372 387 394 DIFFUSION COEFFICIENT, 56 99 111 224 DIGITAL ANALYSIS, 10 DIGLYCIDYL ETHER BISPHENOL A, 200 DIMETHYL FORMAMIDE, 21 77 DIMETHYL ISOPHTHALATE, 208 DIMETHYL SULPHOXIDE, 342 DIMETHYL TEREPHTHALATE, 39 208 DIPHENYLMETHANE DIISOCYANATE, 9 DISCOLOURATION, 288 DISPERSION, 181 217 289 361 DISTILLED WATER, 56 DISTORTION, 20 260 DISTRIBUTION, 60 102 338 DOMESTIC APPLIANCE, 80 DOUGH MOULDING COMPOUND, 211 DRAW RATIO, 117 257 283 284

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Subject Index

DRINKING WATER, 183 307 DUCTILE FAILURE, 289 DYE, 16 397 DYNAMIC, 71 144 317 323 374 DYNAMIC DIFFERENTIAL SCANNING CALORIMETRY, 11 DYNAMIC INFRARED SPECTROSCOPY, 345 DYNAMIC LIGHT SCATTERING, 111 DYNAMIC MECHANICAL ANALYSIS, 36 56 73 83 92 114 134 161 196 245 269 309 377 DYNAMIC MECHANICAL THERMAL ANALYSIS, 325 338 367 DYNAMIC PROPERTIES, 179 317 325 DYNAMIC SPECTROSCOPY, 345 DYNAMIC VISCOELASTIC PROPERTIES, 101

E ELECTRICAL CONDUCTIVITY, 38 ELECTRICAL INSULATOR, 271 ELECTRICAL PROPERTIES, 38 46 338 378 ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY, 5 223 227 237 255 ELECTRODIALYSIS, 97 ELECTROKINETIC CHROMATOGRAPHY, 46 ELECTROKINETIC POTENTIAL, 333 ELECTRON DISPERSIVE X-RAY ANALYSIS, 6 ELECTRON ENERGY LOSS SPECTROSCOPY, 13 358 ELECTRON IONISATION MASS SPECTROMETRY, 206 ELECTRON MICROSCOPY, 2 5 13 63 82 108 129 181 289 324 ELECTRON SCANNING MICROSCOPY, 2 5 13 63 82 108 129 181 ELECTRON SPECTROSCOPY FOR CHEMICAL ANALYSIS, 61 ELECTRON SPIN RESONANCE SPECTROSCOPY, 45 66 294 326 327 368

136

ELECTRONIC APPLICATION, 5 ELECTROPHORESIS, 46 50 97 ELECTROSPRAY IONISATION, 190 222 229 376 ELEMENTAL ANALYSIS, 15 115 160 194 351 ELUENT, 203 235 375 ELUTION, 35 46 203 210 266 285 370 375 382 ELUTION CHROMATOGRAPHY, 50 ELUTION FRACTIONATION, 52 ELUTION VOLUME, 35 285 310 356 EMISSION, 56 87 174 321 END GROUP, 36 102 130 151 229 274 314 END-GROUP ANALYSIS, 190 200 334 376 388 ENDOTHERM, 54 56 74 78 94 125 136 139 ENDOTHERMIC, 235 245 276 309 329 359 ENERGY ABSORPTION, 207 ENERGY CONTENT, 357 ENERGY DISPERSIVE X-RAY ANALYSIS, 108 129 289 328 ENGINEERING APPLICATION, 309 367 ENTHALPY, 36 64 74 125 179 187 276 282 309 339 354 375 ENTROPY, 339 375 ENVIRONMENTAL SCANNING ELECTRON MICROSCOPY, 324 ENVIRONMENTAL STRESS CRACKING, 315 EPICHLOROHYDRIN, 272 EPOXY NOVOLAC RESIN, 11 EPOXY RESIN, 10 11 20 32 36 47 62 68 144 145 149 151 157 161 178 179 182 199 200 222 249 255 269 272 282 292 305 309 312 320 EQUIPMENT, 6 46 138 194 197 218 309 335 379 ERROR ANALYSIS, 13 ETHANOL, 56 311 ETHERSULPHONE COPOLYMER, 47 ETHYLENE ACRYLIC ACID COPOLYMER, 51 348 ETHYLENE-BUTYLENE COPOLYMER, 52 ETHYLENE CONTENT, 370 392 ETHYLENE COPOLYMER, 22 60 63 102 113 154 209 259 348 359 389

ETHYLENE GLYCOL, 39 266 ETHYLENE-HEXENE COPOLYMER, 52 ETHYLENE-PROPYLENE COPOLYMER, 69 274 370 ETHYLENE TEREPHTHALATE COPOLYMER, 131 ETHYLENE-VINYL ACETATE COPOLYMER, 57 70 100 209 226 251 270 306 341 347 359 373 389 ETHYLENE-VINYL ALCOHOL COPOLYMER, 56 57 94 291 387 ETHYLIDENE VINYL PYRROLIDONE, 250 EVANESCENT WAVE SPECTROSCOPY, 111 292 EXCLUSION CHROMATOGRAPHY, 28 29 34 35 40 41 50 52 55 60 97 102 103 108 112 114 116 158 166 204 210 229 239 240 243 299 314 322 334 355 375 381 EXOTHERM, 85 323 EXOTHERMIC, 54 276 309 329 336 EXTENDER, 121 EXTRACTION, 71 97 128 171 185 195 266 331 372 373 EXTRACTION CHROMATOGRAPHY, 97 EXTRUSION, 6 7 40 70 72 183 188 195 225 254 266 324 325

F FADING, 288 FAILURE, 17 30 36 167 178 182 254 271 289 296 341 347 357 FAILURE ANALYSIS, 36 108 145 167 254 289 329 FAST ATOM BOMBARDMENT MASS SPECTROSCOPY, 376 FATTY ACID, 232 FIBRE, 31 33 43 82 100 178 179 182 231 256 260 330 339 371 FIBRE GLASS, 76 176 197 FIBRE OPTIC, 36 FIBRE-REINFORCED PLASTIC, 36 100 141 178 231 258 281 320 FIELD EMISSION SCANNING TRANSMISSION ELECTRON MICROSCOPY, 289 FIELD-FLOW FRACTIONATION, 35 97 FILLED, 179 318 325

© Copyright 2002 Rapra Technology Limited

Subject Index

FILLER, 17 43 45 65 81 90 93 184 207 211 226 289 306 307 318 324 325 399 FILLER CONTENT, 81 90 324 FILLER DISTRIBUTION, 289 324 FILM, 1 3 16 27 37 38 40 41 49 56 57 61 62 65 86 92 102 104 106 115 117 118 135 142 148 156 167 168 186 205 246 257 262 266 269 288 289 308 324 327 349 351 362 373 374 386 387 FINITE ELEMENT ANALYSIS, 108 FIRE RETARDANT, 359 FLAME IONISATION, 185 FLAME RETARDANT, 95 152 211 218 273 FLAMMABILITY, 150 173 273 359 FLASH CHROMATOGRAPHY, 97 FLASH PYROLYSIS, 4 FLAVOUR, 183 FLEXIBLE, 84 277 283 353 FLOATATION, 97 FLOW INJECTION ANALYSIS, 50 FLOW MICROCALORIMETRY, 93 FLOW RATE, 50 143 233 324 372 FLUORESCENCE, 17 293 FLUORESCENCE SPECTROSCOPY, 108 116 157 FLUOROPOLYMER, 279 387 FOAM, 80 84 97 302 FOOD-CONTACT APPLICATION, 124 177 195 208 264 286 387 FOOD PACKAGING, 57 124 168 195 266 278 311 FORMULATION, 30 108 164 174 217 312 FOURIER TRANSFORM INFRARED SPECTROSCOPY, 1 3 6 8 11 24 25 26 29 30 34 36 40 41 60 63 64 72 77 83 88 92 93 94 98 102 107 108 113 117 126 135 136 150 153 156 160 161 163 165 169 170 173 181 189 190 213 215 216 226 228 246 249 250 252 259 262 264 271 274 275 277 288 300 306 309 316 318 321 328 341 343 344 345 352 360 364 374 381 385 386 397 FRACTION, 35 170 204 394 FRACTIONATION, 28 52 97 107 113 337 370 398

FRACTURE, 67 82 98 178 236 271 289 FRACTURE MORPHOLOGY, 2 13 54 61 98 115 191 319 346 391 394 FREE ENERGY, 339 FREE RADICAL, 45 266 FREE VOLUME, 18 56 99 338 367 382 FREEZING POINT, 324 FREQUENCY, 78 118 179 255 256 287 309 325 336 FUEL TANK, 56 FUNCTIONAL GROUP, 36 83 274 331 FUNGUS, 5 FURAN RESIN, 199 FURNITURE, 274

G GAMMA-IRRADIATION, 4 99 133 393 GAS, 67 80 277 311 GAS BARRIER, 56 57 168 GAS CHROMATOGRAPHY, 3 4 30 34 39 53 56 66 71 72 75 76 80 81 84 87 90 96 107 112 119 120 124 128 132 141 143 160 174 183 185 186 191 194 195 198 208 217 218 221 232 235 250 270 273 278 303 307 311 339 349 353 373 382 383 390 392 398 GAS DIFFUSION, 274 GAS LIQUID CHROMATOGRAPHY, 97 GAS-PHASE, 67 80 277 311 GAS PIPE, 277 GAS TRANSMISSION, 311 GEL, 46 319 326 GEL ELECTROPHORESIS, 97 GEL PERMEATION CHROMATOGRAPHY, 50 107 113 137 152 169 172 190 200 233 259 264 295 310 325 334 356 376 383 388 396 399 GELATION, 7 73 134 161 294 GLASS, 145 167 276 351 GLASS CONTENT, 296 GLASS FIBRE, 76 176 197 GLASS FIBRE-REINFORCED PLASTIC, 17 179 202 211 231 271 288 296 333 GLASS TRANSITION TEMPERATURE, 12 15 18 20 29 36 49 51 56 74 77 81 85 94 101 106 110 114 117 122 135

© Copyright 2002 Rapra Technology Limited

149 155 161 163 164 170 179 207 213 220 249 261 269 280 282 287 290 305 308 309 323 328 338 357 367 377 382 390 394 GLOW DISCHARGE, 343 GLOW DISCHARGE SPECTROSCOPY, 202 GRAVIMETRIC ANALYSIS, 23 82 85 93 94 152 189 196 211 244 258 296 317 347 377 380

H HEADSPACE ANALYSIS, 311 HEADSPACE CHROMATOGRAPHY, 185 HEAT CAPACITY, 20 74 78 125 161 179 220 253 261 276 280 287 290 309 324 336 394 HEAT DEGRADATION, 23 26 29 75 76 83 152 160 163 189 192 194 196 244 266 273 318 325 380 381 HEAT FLOW, 36 155 245 252 261 276 309 324 HEAT INSULATION, 80 276 HEAT RESISTANCE, 11 24 26 57 85 126 163 196 228 266 267 269 295 317 377 HEAT STABILITY, 146 196 HEAT TREATMENT, 57 119 HEATING, 36 179 187 244 266 309 323 348 354 HEATING RATE, 36 54 144 179 309 328 332 348 380 HELIUM, 57 HETEROGENEITY, 25 217 268 HETEROGENEOUS, 129 146 170 HEXANE, 240 319 HIGH DENSITY POLYETHYLENE, 52 56 57 63 87 91 102 109 112 128 132 143 164 195 212 214 307 357 372 392 HIGH IMPACT PS, 48 HIGH PERFORMANCE LIQUID CHROMATOGRAPHY, 21 35 39 46 76 97 165 171 183 195 200 222 233 238 239 242 247 264 266 286 304 337 366 375 383 399 400 HIGH TEMPERATURE, 62 107 277 381 HIGH RESOLUTION, 179 209 289 340 354 363 389 HINDERED AMINE, 3 31 66 123 225

137

Subject Index

HINDERED PHENOL, 41 HIP JOINT, 42 HOMOGENEITY, 100 289 340 HOT STAGE MICROSCOPY, 2 181 HUMIDITY, 44 56 57 309 HYDROFLUOROCARBON, 321 HYDROGEN BONDING, 77 94 99 114 342 364 HYDROGEN CHLORIDE, 34 48 194 228 HYDROLYSIS, 34 58 59 165 319 341 352 HYDROPHILICITY, 46 51 360 HYDROPHOBICITY, 37 46 360 375 HYDROXYBENZENE, 75 297 300 HYDROXYETHYL METHACRYLATE COPOLYMER, 46 HYDROXYL GROUP, 36 69

I IDENTIFICATION, 30 79 121 128 132 212 214 353 370 397 ILLUMINATION, 311 IMAGING, 13 67 88 168 179 275 289 346 IMIDAZOLE, 262 IMIDISATION, 8 355 IMMERSION, 178 223 237 IMMISCIBLE, 188 367 394 IMMUNOELECTROPHORESIS, 97 IMPACT PROPERTIES, 56 63 231 370 388 IMPLANT, 219 262 393 IMPURITY, 221 INDUCTION PERIOD, 41 88 INDUCTIVELY COUPLED PLASMA SPECTROMETRY, 351 INELASTIC NEUTRON SCATTERING, 361 INFRARED ABSORPTION, 36 274 362 INFRARED CAMERA, 67 INFRARED DICHROISM, 284 INFRARED SPECTROSCOPY, 1 3 8 11 14 17 24 26 29 33 34 36 39 41 43 51 60 63 66 69 72 77 79 85 88 92 93 94 98 108 113 126 135 142 150 153 156 160 161 163 164 165 169 172 173 181 184 186 188 189 207 215 216 225 226 228 230 244 246 249

138

250 256 257 259 262 264 269 271 274 275 277 284 294 297 301 306 316 318 321 328 341 343 344 345 353 360 362 364 365 371 374 381 383 385 386 387 393 399 INFRARED THERMOGRAPHY, 67 INJECTION MOULDING, 67 160 231 296 357 INK, 239 INSULATION, 80 276 INTERACTION, 90 167 178 235 249 285 311 318 341 342 364 INTERACTION PARAMETER, 220 235 285 INTERCHAIN PACKING, 135 INTERFACE, 178 179 182 206 229 236 322 341 342 346 367 394 INTERFACIAL ADHESION, 333 INTERFACIAL DEBONDING, 167 INTERFACIAL INTERACTION, 90 167 178 INTERFACIAL PROPERTIES, 81 90 111 141 167 178 249 320 342 INTERFEROMETRY, 13 275 363 INTERNAL MOULD RELEASE, 202 INTRINSIC VISCOSITY, 29 172 266 330 INVERSE GAS CHROMATOGRAPHY, 81 90 141 143 191 217 235 339 382 390 ION CHROMATOGRAPHY, 97 218 ION CYCLOTRON RESONANCE, 397 ION EXCHANGE, 50 97 351 IONISATION, 46 50 206 222 379 IRON OXIDE, 112 IRRADIATION, 4 40 92 153 358 IRRADIATION DEGRADATION, 133 ISOELECTRIC POINT, 46 333 ISOMERISATION, 11 288 ISOPHORONE DIISOCYANATE, 121 ISOTACHOPHORESIS, 46 ISOTACTIC, 129 133 274 314 ISOTHERM, 67 178 309 339 ISOTHERMAL, 36 78 117 125 276 317 338 348 375 ISOTROPY, 117

K KAOLIN, 226 306

KEVLAR, 191 KINETIC, 8 10 45 73 83 125 377 KINETICS, 3 23 52 73 75 94 144 149 302 317 323 332 363 380 381

L LAC RESIN, 352 LACQUER, 185 LAMELLAE, 78 139 LAMINATE, 56 57 168 182 266 342 LAMINATED FILM, 57 168 266 293 LANGIVIN EQUATION, 3 46 50 60 75 LASER, 62 212 236 298 351 397 LASER INDUCED DECOHESION SPECTROSCOPY, 236 LASER INTERFEROMETRY, 363 LASER IONISATION MASS SPECTROMETRY, 6 LASER LIGHT SCATTERING, 35 200 LASER RAMAN SPECTROSCOPY, 168 LATERAL FORCE MICROSCOPY, 308 LATEX, 46 156 174 193 198 LEACHING, 183 LEAD, 201 LEAST-SQUARES ANALYSIS, 70 214 345 LENS, 219 265 LIFETIME PREDICTION, 108 255 377 LIGHT ABSORPTION, 229 274 LIGHT DEGRADATION, 3 40 129 153 196 274 288 LIGHT MICROSCOPY, 181 295 LIGHT SCATTERING, 111 116 117 172 203 238 260 310 396 LIGHT STABILISER, 3 31 123 132 288 LIGHT STABILITY, 3 288 LIGNOCELLULOSE, 82 LINEAR LOW DENSITY POLYETHYLENE, 57 92 107 139 186 216 225 324 386 LINEAR REGRESSION ANALYSIS, 144 LIQUID CHROMATOGRAPHY, 21 25 35 39 46 50 55 76 97 103 105 108 124 159 165 171 183 195 200 203 206 210 222 229 233 238 239 240 241 242 243

© Copyright 2002 Rapra Technology Limited

Subject Index

247 264 266 285 286 299 304 319 337 353 355 366 375 379 383 384 395 LIQUID CRYSTAL POLYMER, 309 367 387 LIQUID NITROGEN, 358 LOW DENSITY POLYETHYLENE, 3 57 86 87 139 143 164 168 186 207 214 266 324 325 348 372 373 386 LOW FREQUENCY, 126 363 LOW MOLECULAR WEIGHT, 128 375

M MAGIC ANGLE, 209 268 283 291 300 340 MAGNESIUM-25, 359 MALDI-TOF SPECTROSCOPY, 28 103 127 137 158 159 166 204 310 322 335 356 376 MALEIC ANHYDRIDE, 82 MALEIC ANHYDRIDE COPOLYMER, 28 341 MAPPING, 69 275 289 339 342 344 MASS SELECTIVE DETECTOR, 76 218 MASS SPECTROMETRY, 4 6 13 28 30 50 75 103 107 112 127 132 178 186 192 194 204 222 229 266 278 307 311 376 379 382 392 396 397 398 MASS SPECTROSCOPY, 28 66 72 84 86 103 121 124 127 128 137 153 158 159 166 177 185 190 195 202 204 206 244 250 270 273 303 310 312 322 335 356 376 399 MATRIX, 36 82 141 178 182 351 359 MATRIX-ASSISTED LASER DESORPTION, 28 103 127 137 158 159 166 204 310 322 335 356 376 MDI, 9 MECHANICAL DEGRADATION, 266 MECHANICAL PROPERTIES, 9 40 41 56 61 62 63 65 67 82 84 86 91 114 115 126 151 163 168 178 179 182 207 231 249 256 269 271 277 281 288 289 296 309 315 316 324 325 333 353 365 370 388 MECHANICAL RECYCLING, 195 MECHANICAL SPECTROSCOPY,

325 MEDICAL APPLICATION, 42 262 MELAMINE-FORMALDEHYDE RESIN, 159 365 MELT, 54 170 254 282 290 354 MELT TRANSITION, 267 MELTING, 2 24 54 78 79 136 155 179 209 252 309 332 MELTING POINT, 12 52 56 63 94 114 164 266 295 324 MELTING TEMPERATURE, 20 57 179 207 309 323 332 370 MEMBRANE OSMOMETRY, 396 METAL, 177 179 298 341 METAL ADHESION, 62 223 341 METAL COATING, 62 255 METAL SALT, 352 METALLISED FILM, 168 266 387 METHACRYLATE COPOLYMER, 190 METHACRYLIC ACID COPOLYMER, 15 63 259 METHACRYLIC ESTER COPOLYMER, 190 METHACRYLIC ESTER POLYMER, 45 245 METHANOL, 39 56 76 171 266 METHANOLYSIS, 39 METHYL ACETATE, 185 METHYL ACRYLATE COPOLYMER, 33 172 299 395 METHYL ETHYL KETONE, 285 METHYL METHACRYLATE, 288 METHYL METHACRYLATE COPOLYMER, 28 33 166 198 308 384 METHYLBENZENE, 56 185 241 261 METHYLENE CHLORIDE, 266 MICROANALYSIS, 179 231 289 MICROBIAL DEGRADATION, 5 MICROCALORIMETRY, 154 MICRODIELECTROMETRY, 9 MICROEXTRACTION, 71 185 MICRORAMAN SPECTROSCOPY, 168 346 MICROSCOPY, 2 13 16 27 38 41 58 59 61 98 111 125 126 142 145 168 179 181 213 231 256 257 277 289 295 308 324 387 MICROSTRUCTURE, 13 58 60 168 170 198 274 370 388 392 MICROTOMY, 168 MICROWAVE, 112 128 262 MICROWAVEABLE, 266 387 MID-INFRARED SPECTROSCOPY, 362 MIGRATION, 46 65 183 264 266

© Copyright 2002 Rapra Technology Limited

288 387 MINERAL FILLER, 45 288 289 324 MISCIBILITY, 12 64 77 98 125 146 209 213 220 309 367 390 391 394 MOBILE PHASE, 50 375 395 MODEL, 28 105 149 152 172 216 290 311 319 336 341 360 381 382 394 MODULATED DIFFERENTIAL SCANNING CALORIMETRY, 10 36 74 125 131 135 161 220 261 282 309 377 394 MODULATED TEMPERATURE THERMOMECHANICAL ANALYSIS, 20 MOISTURE CONTENT, 6 51 148 266 309 MOLAR MASS, 25 35 102 103 107 140 159 MOLECULAR CONFIGURATION, 117 130 135 168 328 338 355 367 MOLECULAR INTERACTION, 178 220 342 375 MOLECULAR MOBILITY, 26 268 301 389 MOLECULAR ORIENTATION, 257 281 284 327 360 MOLECULAR STRUCTURE, 1 8 12 16 25 31 47 49 51 53 56 66 68 72 73 77 80 83 89 93 98 101 102 103 107 114 130 133 140 146 152 158 159 164 166 168 172 180 197 198 200 211 213 222 228 229 232 243 264 268 269 274 275 277 283 284 286 289 291 300 301 308 310 317 318 328 331 334 337 355 356 364 365 368 370 376 382 391 MOLECULAR WEIGHT, 1 28 29 42 46 50 52 54 55 62 73 89 102 112 113 114 116 120 127 128 130 158 164 166 172 185 190 200 204 210 222 224 235 239 243 285 310 314 319 322 323 325 330 332 334 337 355 356 375 376 378 381 382 388 395 396 MOLECULAR WEIGHT DISTRIBUTION, 102 116 190 200 204 224 310 314 319 322 325 356 375 381 396 MONITORING, 5 70 149 174 188 223 261 272 298 311 321 348 MONOETHYLENE GLYCOL, 39 266

139

Subject Index

MONOMER, 124 229 269 270 387 MORPHOLOGY, 2 13 54 61 63 98 115 118 136 191 213 256 309 319 346 367 391 394 MOULDING, 134 225 343 MULTI-ANGLE LASER LIGHT SCATTERING, 35 200 MULTILAYER, 168 266 344 387 MULTILAYER FILM, 57 168 MULTIPLE PULSE NMR, 291 MULTIVARIATE ANALYSIS, 216 MUNICIPAL WASTE, 128

N N-METHYL-2-PYRROLIDONE, 355 NANOCOMPOSITE, 62 NAPHTHA, 215 NATURAL FIBRE, 82 NATURAL FIBRE-REINFORCED PLASTIC, 141 NATURAL POLYMER, 232 352 NEAR-INFRARED CORRELATION SPECTROSCOPY, 364 NEAR-INFRARED SPECTROSCOPY, 14 36 215 225 362 371 NITROCELLULOSE, 46 79 185 NITROGEN, 57 76 95 NITROGEN-CONTAINING POLYMER, 250 NON-DESTRUCTIVE TEST, 19 32 67 106 126 157 327 NOVOLAC RESIN, 73 300 NUCLEAR MAGNETIC RESONANCE, 1 22 28 30 31 32 34 57 60 68 73 77 100 108 113 114 123 130 138 148 162 169 172 180 189 193 201 209 212 246 248 251 265 268 272 283 291 297 300 314 331 334 340 350 359 370 372 376 383 388 389 391 392 NUMBER-AVERAGE MOLECULAR WEIGHT, 130 375 378 NYLON, 33 56 57 79 125 164 168 192 199 207 225 231 309 331 NYLON 1010, 24 NYLON-12, 294 364 NYLON-6, 33 56 57 132 207 387 NYLON-6,6, 17 33 57 130 231 329

O ODOUR, 57 183 307

140

OIL, 194 277 OLIGOMER, 26 46 103 124 172 190 192 238 242 264 266 335 ON-LINE MEASUREMENT, 314 OPTICAL FIBRE, 36 188 292 OPTICAL MICROSCOPY, 2 13 41 98 125 142 181 213 289 324 387 OPTICAL PROPERTIES, 1 3 47 57 162 181 199 200 206 263 274 288 292 293 323 332 350 362 375 OPTIMISATION, 50 102 105 171 233 318 373 ORGANOLEPTIC PROPERTIES, 57 183 ORIENTED, 104 117 283 284 361 387 ORTHOPAEDIC APPLICATION, 393 OSCILLATING DIFFERENTIAL SCANNING CALORIMETRY, 7 OSMOMETRY, 29 46 200 378 OVEN STABILITY, 266 OXIDATION, 40 41 61 66 88 94 104 129 152 153 205 266 269 274 288 325 329 348 381 393 OXYGEN, 57 104 153 262 274 311 OXYGEN ABSORPTION, 104 387 OXYGEN BARRIER, 56 57 168

P PACKAGING, 5 57 128 131 168 212 264 266 278 323 387 PACKAGING FILM, 57 168 266 387 PAINT, 62 174 185 217 255 298 PAPER, 266 387 PAPER CHROMATOGRAPHY, 97 PARACRYSTALLINE, 102 207 213 315 PARTIAL LEAST SQUARES, 215 216 PARTICLE BEAM ANALYSIS, 206 PARTICLE PACKING, 324 PARTICLE SIZE, 13 45 50 81 225 233 319 324 372 375 PARTICLE SIZE DISTRIBUTION, 62 324 PEAK INTENSITY, 168 178 260 289 392 PELLET, 216 266 296 373 PERMEABILITY, 56 57 168 237

PERMITTIVITY, 338 PEROXIDE, 294 326 PEROXY COMPOUND, 393 PESTICIDE, 373 PH, 46 50 130 183 PHARMACEUTICAL APPLICATION, 46 221 PHASE BEHAVIOUR, 267 340 365 PHASE SEPARATION, 110 125 156 391 394 PHENOL, 75 297 300 PHENOL-FORMALDEHYDE RESIN, 73 297 300 PHENOLIC ANTIOXIDANT, 183 PHENOLIC RESIN, 83 199 300 PHOSPHORUS, 95 312 373 PHOTOACOUSTIC SPECTROSCOPY, 249 288 344 PHOTOCALORIMETRY, 377 PHOTOCHEMICAL DEGRADATION, 288 PHOTOCROSSLINKING, 45 187 PHOTODEGRADATION, 16 19 65 66 274 279 PHOTOELECTRON SPECTROSCOPY, 13 37 48 100 104 121 167 175 176 196 197 202 205 277 279 298 308 312 316 320 333 343 PHOTOINITIATOR, 27 312 PHOTOISOMERISATION, 288 PHOTOLYSIS, 153 PHOTON CORRELATION SPECTROSCOPY, 224 PHOTOOXIDATION, 40 129 153 274 288 PHOTOVOLTAIC PROPERTIES, 38 PHTHALATE, 288 PHTHALOCYANINE GREEN, 65 PHYSICAL AGEING, 101 135 213 309 338 PHYSICAL PROPERTIES, 12 42 52 56 63 94 114 164 188 215 216 236 259 266 295 324 353 382 PIGMENT, 65 121 181 217 225 236 237 325 399 PIPE, 52 183 277 307 329 PLANT FIBRE, 82 PLASMA TREATMENT, 61 69 106 230 262 298 343 PLASTICISATION, 36 56 301 348 PLASTICISER, 33 34 120 184 258 277 353 387 399 PLASTICS WASTE, 87 211 212 PLATE-OUT, 6

© Copyright 2002 Rapra Technology Limited

Subject Index

POLARISATION, 256 257 284 POLARISED CONFOCAL RAMAN MICROSCOPY, 257 POLARISED FLUORESCENCE, 284 POLARISED LIGHT MICROSCOPY, 181 POLARISED OPTICAL MICROSCOPY, 13 POLARISING MICROSCOPY, 168 POLARITY, 50 203 339 POLYACETAL, 164 POLYACRYLAMIDE, 46 240 POLYACRYLATE, 245 269 POLYACRYLIC, 249 343 POLYACRYLIC ACID, 46 172 342 POLYACRYLIC IMIDE, 387 POLYACRYLONITRILE, 33 79 119 342 POLYALPHAMETHYLSTYRENE, 153 POLYAMIC ACID, 355 POLYAMIDE, 33 56 57 79 125 164 168 192 199 207 225 231 309 331 POLYAMIDE-1010, 24 POLYAMIDE-12, 159 POLYAMIDE-6, 33 56 57 132 165 207 387 POLYAMIDE-6,6, 17 130 POLYAMIDE-IMIDE, 316 POLYAMINE, 46 272 POLYANILINE, 46 115 POLYARAMIDE, 191 339 POLYARYL ETHER KETONE, 213 POLYARYLATE, 367 POLYBENZIMIDAZOLE, 79 POLYBENZYL METHACRYLATE, 35 POLYBIBENZOATE, 309 POLYBISGLYCIDYL METHACRYLATE, 247 POLYBUTYL ACRYLATE, 156 394 POLYBUTYL METHACRYLATE, 21 376 POLYBUTYL THIOPHENE, 327 POLYBUTYLENE NAPHTHALATE, 98 POLYBUTYLENE TEREPHTHALATE, 164 273 POLYCAPROLACTONE, 147 267 390 POLYCARBONATE, 14 57 62 72 79 99 101 199 207 245 273 280 309 340 356 363 367 382 398

POLYCYANATE, 11 POLYCYANURATE, 317 POLYDEUTEROPOLYETHYLENE, 361 POLYDICYANATE, 11 POLYDIMETHYLPHENYLENE OXIDE, 356 POLYDIMETHYLSILOXANE, 140 POLYDISPERSITY, 29 35 127 137 204 224 325 335 356 POLYEPICHLOROHYDRIN, 390 POLYEPOXIDE, 10 20 32 36 47 62 68 144 145 149 151 157 161 178 179 182 199 200 222 249 255 269 272 282 292 305 309 312 320 POLYESTER RESIN, 199 204 288 POLYESTER-URETHANE, 114 POLYESTERIMIDE, 355 POLYETHER, 54 66 158 235 238 242 384 398 POLYETHER SULPHONE, 75 125 151 356 POLYETHER-ETHERKETONE, 54 79 126 213 295 315 POLYETHER-URETHANE, 90 POLYETHERETHERKETONE, 79 126 POLYETHERIMIDE, 64 79 98 192 296 367 387 POLYETHERSULPHONE, 75 125 151 356 POLYETHYL ACRYLATE, 58 POLYETHYL METHACRYLATE, 390 POLYETHYLENE, 42 52 56 57 60 61 63 65 79 87 91 92 99 102 107 109 112 128 132 139 143 146 148 154 157 164 168 181 186 188 195 199 207 212 214 216 225 249 256 260 263 266 267 283 293 307 315 324 325 344 348 357 361 365 366 368 370 372 373 386 392 393 398 400 POLYETHYLENE GLYCOL, 46 233 310 369 378 POLYETHYLENE GLYCOL TEREPHTHALATE, 26 POLYETHYLENE NAPHTHALATE, 387 POLYETHYLENE OXIDE, 125 154 235 337 POLYETHYLENE TEREPHTHALATE, 2 12 26 39 40 57 63 64 74 76 79 106 117 118 131 136 157 164 168

© Copyright 2002 Rapra Technology Limited

207 212 214 257 261 263 266 269 283 293 309 323 336 357 358 382 388 398 POLYFLUOROETHYLENE, 79 164 180 279 296 POLYHYDROXYBUTYRATE, 59 POLYHYDROXYBUTYRIC ACID, 246 POLYHYDROXYETHYL METHACRYLATE, 172 248 POLYHYDROXYKETONE, 349 POLYHYDROXYSTYRENE, 77 367 POLYIMIDE, 5 23 79 196 199 320 355 POLYIONENE, 57 276 POLYISOCYANATE, 9 POLYKETONE, 54 POLYLACTIC ACID, 267 POLYMERIC FLAME RETARDANT, 218 273 POLYMERIC MOULD RELEASE AGENT, 202 POLYMETHACRYLATE, 45 245 398 POLYMETHACRYLIC ACID, 15 141 POLYMETHACRYLONITRILE, 141 POLYMETHYL METHACRYLATE, 14 21 116 132 137 141 159 166 178 204 219 220 221 224 229 240 241 284 285 289 299 301 304 314 319 335 338 343 363 375 382 384 394 397 398 POLYMETHYLENE OXIDE, 79 POLYOL, 84 110 POLYOXYETHYLENE, 154 POLYOXYMETHYLENE, 79 POLYPHENYLENE, 398 POLYPHENYLENE ETHER, 79 152 220 367 POLYPHENYLENE OXIDE, 79 152 220 357 367 394 POLYPHENYLENE SULPHIDE, 79 170 296 320 328 POLYPHENYLENE TEREPHTHALAMIDE, 339 POLYPHENYLMETHACRYLATE, 367 POLYPHENYLSULPHONE, 79 POLYPROPYLENE, 31 41 57 59 79 87 88 91 102 104 109 112 118 123 128 129 132 133 168 171 183 188 205 206 207 212 214 249 264 281 284 289 293 329 330 370 380 381 398

141

Subject Index

POLYPROPYLENE GLYCOL, 334 POLYPROPYLENE GLYCOL MALEATE, 288 POLYPROPYLENE OXIDE, 103 POLYPYRROLE, 46 POLYSTYRENE, 14 21 35 46 48 57 58 79 82 85 87 118 141 153 156 159 160 164 166 203 207 212 214 220 230 245 278 290 299 304 308 315 334 351 363 367 375 382 394 395 398 POLYSULPHONE, 75 79 99 125 331 POLYTETRAFLUOROETHYLENE, 79 164 180 279 296 363 POLYTETRAMETHYLENE OXIDE, 384 POLYTHIOPHENE, 38 POLYURETHANE, 19 66 79 80 84 89 110 157 158 163 169 187 199 207 255 POLYVINYL ACETATE, 79 199 209 220 268 270 367 394 POLYVINYL ALCOHOL, 1 46 51 57 284 342 POLYVINYL CARBAZOLE, 162 POLYVINYL CHLORIDE, 6 7 17 57 79 87 108 141 145 146 167 184 194 201 207 212 214 227 228 254 262 315 326 353 374 385 392 394 POLYVINYL ESTER, 320 POLYVINYL METHYL ETHER, 363 POLYVINYL PHENOL, 77 367 POLYVINYL PYRROLIDONE, 46 77 248 250 340 POLYVINYLBENZENE, 79 85 87 118 153 212 290 315 POLYVINYLCARBAZOLE, 162 POLYVINYLIDENE CHLORIDE, 57 168 387 POLYVINYLIDENE FLUORIDE, 12 79 277 390 POLYVINYLPYRROLIDONE, 46 77 248 250 340 PORE SIZE, 50 241 285 319 375 POROSITY, 50 126 142 203 241 285 319 367 375 POSITRON ANNIHILATION LIFETIME SPECTROSCOPY, 19 99 338 367 POST-CONSUMER, 195 214 266 373 POTABLE WATER, 183 307 POTASSIUM BROMIDE, 262 271 POWDER, 126 175 194

142

POWDER COATING, 222 PRE-TREATMENT, 176 197 215 223 351 PRECIPITATION, 35 266 PRESSURE, 50 56 171 194 206 222 236 395 PRINCIPAL COMPONENTS ANALYSIS, 216 PROBE, 179 339 382 PROBLEM PREVENTION, 30 181 296 303 PROCESSING, 115 168 199 207 209 231 254 261 323 325 329 373 388 PROPYLENE, 264 PROPYLENE COPOLYMER, 18 22 69 102 PROPYLENE-ETHYLENE COPOLYMER, 69 274 370 PROTECTIVE COATING, 217 255 PROTON MAGNETIC RESONANCE, 265 291 314 388 PROTON SPIN RELAXATION, 209 268 PULSED NMR, 272 PURITY, 120 192 PYROLYSIS, 4 75 83 87 119 192 194 212 234 270 273 296 303 374 380 392 PYROLYSIS GAS CHROMATOGRAPHY, 4 96 107 132 198 218 221 232 250 270 392 PYROLYSIS-IR SPECTROPHOTOMETRY, 4 PYROLYSIS MASS SPECTROMETRY, 4 192

Q QUALITATIVE ANALYSIS, 195 QUALITY, 183 311 361 QUALITY CONTROL, 67 131 329 347 353 357 386 QUANTITATIVE ANALYSIS, 102 171 179 184 195 221 278 373 QUENCHING, 101 117 135 261 363

R RADIATION CURING, 269 RADIO FREQUENCY DISCHARGE, 343 RADIOLYSIS, 4 RAMAN SPECTROSCOPY, 16 27

30 33 42 47 69 70 108 109 129 140 151 168 182 212 214 215 216 256 257 263 281 284 288 293 300 342 346 365 369 393 RAPID SCAN, 344 345 REACTIVITY, 151 274 388 392 REARVIEW MIRROR, 67 RECLAIM, 289 RECOVERY, 319 RECRYSTALLISATION, 54 136 309 332 RECYCLABILITY, 57 88 266 387 RECYCLATE, 64 91 122 195 329 373 RECYCLING, 39 57 64 88 91 122 128 165 195 211 212 231 266 373 387 REFLECTANCE SPECTROSCOPY, 257 343 REFRACTIVE INDEX, 1 106 190 200 229 292 375 REFRIGERATOR, 80 REGRESSION ANALYSIS, 144 214 215 216 224 345 REINFORCED PLASTIC, 13 17 36 79 81 90 100 134 141 176 178 179 182 196 197 199 202 211 231 234 271 281 288 296 318 320 333 339 357 377 RELATIVE HUMIDITY, 44 56 57 309 RELAXATION, 74 282 287 290 309 363 RELAXATION MAP ANALYSIS SPECTROSCOPY, 377 RELAXATION SPECTRA, 325 RELAXATION TIME, 209 291 340 RELAXATION TRANSITION, 290 RELEASE AGENT, 202 REPEATABILITY, 347 REPRODUCIBILITY, 6 46 347 375 RESIDENCE TIME, 266 325 357 RESIDUAL ADDITIVE, 221 RESIDUAL CATALYST, 129 RESIDUAL STRESS, 67 316 RESOLUTION, 50 118 229 RETENTION TIME, 119 222 RETENTION VOLUME, 143 375 REVERSE OSMOSIS, 97 REVERSE-PHASE CHROMATOGRAPHY, 50 195 233 REVIEW, 13 55 59 71 79 107 199 205 212 283 284 310 350 363 364 365 367 372 377 383 387

© Copyright 2002 Rapra Technology Limited

Subject Index

390 391 396 RHEOLOGICAL PROPERTIES, 10 20 29 41 46 73 149 161 163 217 266 295 324 325 338 354 RHEOMETRY, 10 324 325 RHEOPHOTOACOUSTIC SPECTROSCOPY, 249 ROPE, 281 ROTATING FRAME, 209 268 340 ROUND ROBIN TEST, 173

S SAMPLE PREPARATION, 13 72 123 124 207 SAMPLE SIZE, 72 124 143 SAMPLING, 13 71 72 123 124 207 233 351 SAN, 110 147 207 220 284 315 345 SATURATED POLYESTER, 26 49 106 114 204 229 267 322 336 367 376 388 398 SCANNING ELECTRON MICROSCOPY, 2 5 6 13 59 61 62 63 82 98 108 129 181 202 231 289 316 324 358 SCANNING PROBE MICROSCOPY, 59 179 SCISSION, 4 152 274 380 SCRAP POLYMER, 122 128 214 231 SEALANT, 247 SEALING, 387 SEAT, 274 SECONDARY AMINE, 36 151 SECONDARY ANTIOXIDANT, 93 SECONDARY ION MASS SPECTROSCOPY, 13 121 178 202 312 SECONDARY STABILISER, 228 SEMICONDUCTOR, 321 SEMICRYSTALLINE, 102 106 122 207 213 235 315 SENSITIVITY, 118 291 SENSOR, 20 292 SEPARATION, 35 55 97 105 128 243 341 351 370 375 384 SEQUENCE ANALYSIS, 50 SHEAR, 9 178 182 324 325 333 SHEET, 186 SHEET MOULDING COMPOUND, 202 211 SHELF LIFE, 57 311 387 SHELLAC, 232 352 SHIFT FACTOR, 209 SIDING, 385

SILICA, 6 21 40 45 46 90 203 289 319 375 SILICA GEL, 241 319 SILICATE, 65 81 SILICONE POLYMER, 204 284 SIMULATED BODY FLUID, 34 SIMULATION, 34 134 149 323 362 367 SIZE EXCLUSION CHROMATOGRAPHY, 28 29 34 35 40 50 52 55 60 97 102 103 108 112 114 116 158 166 204 229 239 240 243 299 314 322 334 375 381 SIZING, 176 SMALL-ANGLE, 117 291 354 SMOKE EMISSION, 76 150 173 SOFTENING TEMPERATURE, 179 SOFTWARE, 67 195 344 SOL-GEL, 53 SOLAR ENERGY APPLICATION, 38 SOLID STATE, 193 209 268 283 291 300 340 359 389 SOLUBILITY, 56 79 90 97 114 115 160 372 375 SOLUTE, 50 235 382 SOLUTION, 21 46 55 77 115 116 130 178 224 268 291 351 367 389 SOLUTION CASTING, 94 262 367 SOLUTION VISCOSITY, 396 SOLVENT, 21 29 35 56 113 124 130 185 203 210 235 259 261 266 285 349 360 366 369 375 388 SOLVENT EXTRACTION, 266 331 SOLVENT PERMEABILITY, 56 SOXHLET EXTRACTION, 112 SPECIFIC HEAT, 20 122 207 309 324 354 SPECIFIC VOLUME, 18 SPIN-PROBE ANALYSIS, 45 SPIN RELAXATION, 209 268 300 SPOILAGE INDICATOR, 311 STABILISER, 3 40 41 66 86 183 184 201 225 228 288 372 STABILITY, 24 26 57 85 126 163 196 228 266 267 269 295 317 324 377 STANDARD, 120 183 184 392 STAR-BRANCHED, 35 STARCH, 112 267 348 STARCH POLYMER, STATIC HEAD SPACE GAS

© Copyright 2002 Rapra Technology Limited

CHROMATOGRAPHY, 71 STATIONARY PHASE, 50 203 235 375 STEEL, 223 341 STEP-SCAN PHOTOACOUSTIC SPECTROSCOPY, 344 STEREOREGULARITY, 168 STERIC EXCLUSION CHROMATOGRAPHY, 41 STERILISATION, 42 393 STORAGE, 309 311 STORAGE TIME, 311 STRAIN, 315 325 365 STRENGTH, 9 167 269 315 STRESS, 67 168 182 281 289 315 316 325 STRESS CRACKING, 271 STRESS-STRAIN PROPERTIES, 61 231 281 325 STRUCTURAL ADHESIVE, 62 STRUCTURAL ANALYSIS, 168 STRUCTURE-PROPERTY RELATIONSHIP, 209 269 389 STYRENE, 199 278 288 STYRENE-ACRYLONITRILE COPOLYMER, 72 110 147 207 220 284 315 345 STYRENE COPOLYMER, 28 69 127 198 299 308 363 395 STYRENE-ISOPRENESTYRENE BLOCK COPOLYMER, 394 STYRENE-METHACRYLIC ACID COPOLYMER, 81 SUB-GLASS TRANSITION, 170 SUBSTRATE, 126 223 236 262 285 298 SULPHUR DIOXIDE, 75 SUPERCRITICAL, 39 SUPERCRITICAL FLUID CHROMATOGRAPHY, 50 372 SUPERCRITICAL FLUID EXTRACTION, 97 171 372 373 SUPERCRITICAL GAS, 301 SURFACE ANALYSIS, 19 30 37 38 44 58 59 62 67 69 118 175 178 179 202 219 289 324 333 SURFACE AREA, 197 324 SURFACE CHEMISTRY, 93 298 319 SURFACE ENERGY, 52 141 217 235 277 339 SURFACE PROPERTIES, 42 44 106 118 179 191 196 217 219 277 308 312 360 383 SURFACE TREATMENT, 61 62 81 168 176 178 182 197 205

143

Subject Index

223 230 262 277 298 343 371 SURFACTANT, 46 65 233 SURGICAL APPLICATION, 219 393 SWELLING, 15 237 250 326 360 SYNCHROTRON RADIATION, 291 SYNTHETIC FIBREREINFORCED PLASTIC, 281

T TALC, 65 318 324 TAPE, 284 TAPPING MODE ATOMIC FORCE MICROSCOPY, 58 TASTE, 57 TEMPERATURE DEPENDENCE, 49 99 135 146 147 170 196 259 269 308 336 354 364 382 TEMPERATURE GRADIENT INTERACTION CHROMATOGRAPHY, 304 375 TEMPERATURE MODULATED DIFFERENTIAL SCANNING CALORIMETRY, 54 78 136 252 253 280 287 290 309 336 TEMPERATURE PROFILE, 67 324 TEMPERATURE PROGRAMMED ANALYTICAL PYROLYSIS, 273 TEMPERATURE RANGE, 207 317 364 380 382 TEMPERATURE RISING ELUTION FRACTIONATION, 370 396 TENSILE PROPERTIES, 40 41 61 63 65 86 114 115 231 277 315 333 TEREPHTHALIC ACID, 76 TERTIARY AMINE, 36 151 TEST SPECIMEN, 236 346 351 358 TESTING, 19 43 58 59 62 71 79 96 108 112 120 123 124 134 145 174 182 183 184 185 195 206 208 254 255 270 288 293 304 315 321 329 332 345 347 357 363 365 379 382 398 TETRAHYDROFURAN, 29 35 240 241 319 395 TEXTILE APPLICATION, 371 THERMAL AGEING, 88 152 THERMAL ANALYSIS, 7 20 26 36 54 56 67 78 83 92 95 110

144

133 134 144 147 149 154 155 170 179 186 187 189 207 245 252 258 267 269 270 305 309 313 324 325 367 377 383 386 394 THERMAL CONDUCTIVITY, 80 179 309 324 377 THERMAL DEGRADATION, 23 26 29 75 76 83 85 152 160 163 189 192 194 196 244 258 266 273 318 325 380 381 THERMAL DIFFUSIVITY, 179 324 394 THERMAL FIELD-FLOW FRACTIONATION, 35 THERMAL HISTORY, 57 135 136 207 245 254 262 287 309 THERMAL IMAGING, 67 THERMAL INSULATION, 80 276 THERMAL MECHANICAL ANALYSIS, 196 377 THERMAL RELAXATION, 282 290 THERMAL RESISTANCE, 196 THERMAL STABILITY, 11 24 26 57 85 126 163 196 228 266 267 269 295 317 377 THERMAL TRANSITION, 56 78 220 282 290 309 THERMAL VOLATILISATION ANALYSIS, 189 THERMALLY STIMULATED CURRENT, 323 377 THERMOANALYTICAL, 348 THERMODYNAMIC PROPERTIES, 21 90 122 155 169 172 220 235 290 339 THERMOGRAM, 36 67 323 348 370 THERMOGRAVIMETRIC ANALYSIS, 2 8 12 15 17 23 24 26 29 48 82 83 85 93 94 98 146 152 163 164 189 192 194 196 211 228 231 244 258 267 269 295 296 316 317 318 326 330 347 348 377 380 381 398 THERMOLYSIS, 189 THERMOMECHANICAL DEGRADATION, 266 THERMOMECHANICAL PROPERTIES, 179 269 THERMOOXIDATIVE DEGRADATION, 41 94 152 269 348 THERMORHEOLOGICAL PROPERTIES, 338 THICKNESS, 27 56 62 67 168 179 236 255 257 263

THIN LAYER CHROMATOGRAPHY, 97 399 TIE LAYER, 168 TIME, 54 61 94 135 209 223 253 261 268 277 289 317 338 354 394 TIME DEPENDENCE, 125 196 360 TIME OF FLIGHT, 103 127 137 158 159 166 178 202 204 229 310 312 322 335 356 376 TIME RESOLVED SPECTROSCOPY, 170 TITANIUM DIOXIDE, 40 65 217 237 325 TOLUENE, 56 185 241 261 319 TOTAL ORGANIC CARBON, 183 TOXICITY, 173 195 TRACE ELEMENT, 177 TRANSITION PHENOMENA, 254 TRANSITION PROPERTIES, 203 269 340 354 TRANSITION TEMPERATURE, 179 TRANSMISSION ELECTRON MICROSCOPY, 2 5 13 59 63 82 108 129 181 213 289 331 358 TRANSMISSION SPECTROSCOPY, 234 292 362 TRANSPARENCY, 57 236 323 TRANSPORT PROPERTIES, 56 115 TRIAZINE, 40 TRICHLOROBENZENE, 29 TRICHLOROMETHANE, 29 TRIETHYLAMINE, 298 TRIFLUOROACETIC ACID, 388 TROUBLESHOOTING, 30 181 296 303 TWO-DIMENSIONAL, 55 58 209 233 242 275 283 344 345 364 365

U UHMWPE, 260 393 ULTRA-HIGH RESOLUTION SPECTROSCOPY, 363 ULTRASONIC, 112 126 272 ULTRAVIOLET ABSORPTION, 229 274 ULTRAVIOLET CURING, 27 269 349 ULTRAVIOLET DEGRADATION, 16 19 196 ULTRAVIOLET IRRADIATION,

© Copyright 2002 Rapra Technology Limited

Subject Index

19 40 44 196 ULTRAVIOLET RESISTANCE, 57 196 ULTRAVIOLET SPECTRA, 3 41 65 86 157 264 372 383 399 ULTRAVIOLET SPECTROSCOPY, 1 3 41 46 65 86 115 157 288 372 ULTRAVIOLET STABILISER, 225 288 399 UNIT CELL, 13 168 UNPLASTICISED POLYVINYL CHLORIDE, 254 UNSATURATED POLYESTER, 82 199 204 288 333 UV VIS SPECTROSCOPY, 1 46 115 288

V VACUUM DISTILLATION, 97 185 VACUUM PYROLYSIS, 87 194 VAPOUR PERMEABILITY, 56 168 VAPOUR PHASE OSMOMETRY, 396 VAPOUR PRESSURE OSMOMETRY, 29 200 378 VARNISH, 174 VEHICLE BONNET, 329 VEHICLE MIRROR, 67 VIBRATIONAL SPECTROSCOPY, 14 16 17 26 27 30 33 36 39 42 43 47 51 69 70 85 108 109 129 140 142 150 151 156 164 168 172 173 182 184 186 188 207 212 214 215 216 225 226 230 244 256 257 263 269 274 281 284 288 293 297 300 318 342 345 346 353 365 369 393 VINYL ACETATE, 251 270 VINYL ACETATE COPOLYMER, 209 359 389 VINYL ACETATE-ETHYLENE COPOLYMER, 100 270 341 359 VINYL CHLORIDE, 199 392 VINYL CYANIDE, 119 VINYL CYANIDE COPOLYMER, 57

VINYL ESTER RESIN, 320 VINYL GROUP, 274 VINYL PYRROLIDONE COPOLYMER, 46 VISCOELASTICITY, 20 219 308 VISCOMETRY, 29 200 203 355 VISCOSITY, 10 29 46 149 172 266 324 325 330 VISIBLE SPECTROSCOPY, 1 46 115 288 VITRIFICATION, 78 161 290 VOLATILE CONTENT, 72 185 VOLATILE ORGANIC COMPOUND, 84 174 185 255 278 321 VOLATILISATION, 72 97 VOLUME FRACTION, 13 227 231 324 332 367

W WASTE, 87 122 128 211 212 266 387 WATER, 39 56 61 266 360 WATER ABSORPTION, 51 56 237 309 WATER CONTENT, 6 51 148 WATER PERMEABILITY, 56 237 WATER PIPE, 307 329 WATER TREE GROWTH RATE, 148 WATER VAPOUR PERMEABILITY, 56 168 WAVE NUMBER, 168 WAVELENGTH, 44 207 288 WAX, 232 WEATHERING, 44 62 86 92 222 385 WEIGHT AVERAGE MOLECULAR WEIGHT, 375 WEIGHT CHANGE, 348 WEIGHT FRACTION, 176 394 WEIGHT GAIN, 56 WEIGHT LOSS, 56 94 164 267 296 347 380 WETTABILITY, 37 343 WIDE ANGLE, 117 213 260 WIDE ANGLE X-RAY SCATTERING, 24 WINDOW, 7 WOOD FIBRE-REINFORCED PLASTIC, 9 82 141 258

© Copyright 2002 Rapra Technology Limited

X X-RAY ANALYSIS, 6 108 129 212 231 289 328 383 X-RAY DIFFRACTION, 13 41 57 83 92 95 117 213 260 277 291 327 328 398 399 X-RAY FLUORESCENCE, 17 399 X-RAY FLUORESCENCE SPECTROSCOPY, 108 X-RAY NEAR EDGE ABSORPTION SPECTROSCOPY, 358 X-RAY PHOTOELECTRON SPECTROSCOPY, 13 37 48 100 121 145 167 175 176 196 197 202 277 279 298 308 312 316 320 333 343 X-RAY RESISTANCE, 104 279 X-RAY SCATTERING, 13 24 41 57 83 92 95 117 213 260 277 291 327 328 X-RAY SPECTROSCOPY, 13 37 48 63 100 108 121 167 175 176 196 197 202 277 279 298 308 312 316 320 328 333 343 354 358 XENON LIGHT, 274

Y YELLOWING, 288 YOGHURT POT, 278 YOUNG’S MODULUS, 40 114 168 231 256 269 309 365

Z ZEOLITE, 307 ZIEGLER CATALYST, 102 129 ZINC, 298 ZINC BORATE, 359 ZIRCONOCENE, 365

145

Subject Index

146

© Copyright 2002 Rapra Technology Limited

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