Analysis of Plastics, Vol. 13 (2002)
Analysis of Plastics, Vol. 13 (2002)
Analysis of Plastics, Vol. 13 (2002)
Analysis of Plastics
Martin J. Forrest
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.
Item 1
Source of
Macromolecules
original article
33, No.6, 21st March 2000, p.2171-83
Title EFFECT OF THERMAL HISTORY ON THE RHEOLOGICAL
BEHAVIOR OF THERMOPLASTIC POLYURETHANES
Authors and
Pil Joong Yoon; Chang Dae Han affiliation
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 Abstract
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. Companies or
GOODRICH B.F. organisations
Location USA mentioned
Accession no.771897
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Previous Titles Still Available
Volume 1 Volume 4
Report 3 Advanced Composites, D.K. Thomas, RAE, Farnborough. Report 37 Polymers in Aerospace Applications, W.W. Wright,
Report 4 Liquid Crystal Polymers, M.K. Cox, ICI, Wilton. University of Surrey.
Report 5 CAD/CAM in the Polymer Industry, N.W. Sandland Report 39 Polymers in Chemically Resistant Applications,
and M.J. Sebborn, Cambridge Applied Technology. 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, Report 42 Polycarbonates, R. Pakull, U. Grigo, D. Freitag, Bayer
R. Spratling, British Telecom. AG.
Report 12 Process Control in the Plastics Industry, Report 43 Polymeric Materials from Renewable Resources,
R.F. Evans, Engelmann & Buckham Ancillaries. J.M. Methven, UMIST.
Report 44 Flammability and Flame Retardants in Plastics,
Volume 2 J. Green, FMC Corp.
Report 13 Injection Moulding of Engineering Thermoplastics, Report 45 Composites - Tooling and Component Processing,
A.F. Whelan, London School of Polymer Technology. N.G. Brain, Tooltex.
Report 14 Polymers and Their Uses in the Sports and Leisure Report 46 Quality Today in Polymer Processing, S.H. Coulson,
Industries, A.L. Cox and R.P. Brown, Rapra J.A. Cousans, Exxon Chemical International Marketing.
Technology Ltd. Report 47 Chemical Analysis of Polymers, G. Lawson, Leicester
Report 15 Polyurethane, Materials, Processing and Polytechnic.
Applications, G. Woods, Consultant.
Report 16 Polyetheretherketone, D.J. Kemmish, ICI, Wilton. Volume 5
Report 17 Extrusion, G.M. Gale, Rapra Technology Ltd.
Report 49 Blends and Alloys of Engineering Thermoplastics,
Report 18 Agricultural and Horticultural Applications of H.T. van de Grampel, General Electric Plastics BV.
Polymers, J.C. Garnaud, International Committee for
Plastics in Agriculture. Report 50 Automotive Applications of Polymers II,
A.N.A. Elliott, Consultant.
Report 19 Recycling and Disposal of Plastics Packaging,
R.C. Fox, Plas/Tech Ltd. Report 51 Biomedical Applications of Polymers, C.G. Gebelein,
Youngstown State University / Florida Atlantic University.
Report 20 Pultrusion, L. Hollaway, University of Surrey.
Report 52 Polymer Supported Chemical Reactions, P. Hodge,
Report 21 Materials Handling in the Polymer Industry,
University of Manchester.
H. Hardy, Chronos Richardson Ltd.
Report 53 Weathering of Polymers, S.M. Halliwell, Building
Report 22 Electronics Applications of Polymers, M.T.Goosey,
Research Establishment.
Plessey Research (Caswell) Ltd.
Report 23 Offshore Applications of Polymers, J.W.Brockbank, Report 54 Health and Safety in the Rubber Industry, A.R. Nutt,
Avon Industrial Polymers Ltd. Arnold Nutt & Co. and J. Wade.
Report 24 Recent Developments in Materials for Food Report 55 Computer Modelling of Polymer Processing,
Packaging, R.A. Roberts, Pira Packaging Division. 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 Foams and Blowing Agents, J.M. Methven, Cellcom Report 57 Joining of Plastics, K.W. Allen, City University.
Technology Associates.
Report 58 Physical Testing of Rubber, R.P. Brown, Rapra
Report 26 Polymers and Structural Composites in Civil
Technology Ltd.
Engineering, L. Hollaway, University of Surrey.
Report 59 Polyimides - Materials, Processing and Applications,
Report 27 Injection Moulding of Rubber, M.A. Wheelans,
A.J. Kirby, Du Pont (U.K.) Ltd.
Consultant.
Report 28 Adhesives for Structural and Engineering Report 60 Physical Testing of Thermoplastics, S.W. Hawley,
Applications, C. O’Reilly, Loctite (Ireland) Ltd. Rapra Technology Ltd.
Report 29 Polymers in Marine Applications, C.F.Britton,
Corrosion Monitoring Consultancy. Volume 6
Report 30 Non-destructive Testing of Polymers, W.N. Reynolds, Report 61 Food Contact Polymeric Materials, J.A. Sidwell,
National NDT Centre, Harwell. Rapra Technology Ltd.
Report 31 Silicone Rubbers, B.R. Trego and H.W.Winnan, Report 62 Coextrusion, D. Djordjevic, Klöckner ER-WE-PA GmbH.
Dow Corning Ltd.
Report 63 Conductive Polymers II, R.H. Friend, University of
Report 32 Fluoroelastomers - Properties and Applications, Cambridge, Cavendish Laboratory.
D. Cook and M. Lynn, 3M United Kingdom Plc and
3M Belgium SA. Report 64 Designing with Plastics, P.R. Lewis, The Open University.
Report 33 Polyamides, R.S. Williams and T. Daniels, Report 65 Decorating and Coating of Plastics, P.J. Robinson,
T & N Technology Ltd. and BIP Chemicals Ltd. International Automotive Design.
Report 34 Extrusion of Rubber, J.G.A. Lovegrove, Nova Report 66 Reinforced Thermoplastics - Composition, Processing
Petrochemicals Inc. and Applications, P.G. Kelleher, New Jersey Polymer
Extension Center at Stevens Institute of Technology.
Report 35 Polymers in Household Electrical Goods, D.Alvey,
Hotpoint Ltd. Report 67 Plastics in Thermal and Acoustic Building Insulation,
Report 36 Developments in Additives to Meet Health and V.L. Kefford, MRM Engineering Consultancy.
Environmental Concerns, M.J. Forrest, Rapra Report 68 Cure Assessment by Physical and Chemical
Technology Ltd. Techniques, B.G. Willoughby, Rapra Technology Ltd.
Report 69 Toxicity of Plastics and Rubber in Fire, P.J. Fardell, Report 94 Compressive Behaviour of Composites,
Building Research Establishment, Fire Research Station. C. Soutis, Imperial College of Science, Technology
and Medicine.
Report 70 Acrylonitrile-Butadiene-Styrene Polymers,
M.E. Adams, D.J. Buckley, R.E. Colborn, W.P. England Report 95 Thermal Analysis of Polymers, M. P. Sepe, Dickten &
and D.N. Schissel, General Electric Corporate Research Masch Manufacturing Co.
and Development Center. Report 96 Polymeric Seals and Sealing Technology, J.A. Hickman,
Report 71 Rotational Moulding, R.J. Crawford, The Queen’s St Clair (Polymers) Ltd.
University of Belfast.
Report 72 Advances in Injection Moulding, C.A. Maier,
Econology Ltd.
Volume 9
Report 97 Rubber Compounding Ingredients - Need, Theory
and Innovation, Part II: Processing, Bonding, Fire
Volume 7 Retardants, C. Hepburn, University of Ulster.
Report 98 Advances in Biodegradable Polymers, G.F. Moore &
Report 73 Reactive Processing of Polymers, M.W.R. Brown,
S.M. Saunders, Rapra Technology Ltd.
P.D. Coates and A.F. Johnson, IRC in Polymer Science
and Technology, University of Bradford. Report 99 Recycling of Rubber, H.J. Manuel and W. Dierkes,
Vredestein Rubber Recycling B.V.
Report 74 Speciality Rubbers, J.A. Brydson.
Report 100 Photoinitiated Polymerisation - Theory and
Report 75 Plastics and the Environment, I. Boustead, Boustead Applications, J.P. Fouassier, Ecole Nationale Supérieure
Consulting Ltd. de Chimie, Mulhouse.
Report 76 Polymeric Precursors for Ceramic Materials, Report 101 Solvent-Free Adhesives, T.E. Rolando, H.B. Fuller
R.C.P. Cubbon. Company.
Report 77 Advances in Tyre Mechanics, R.A. Ridha, M. Theves, Report 102 Plastics in Pressure Pipes, T. Stafford, Rapra
Goodyear Technical Center. Technology Ltd.
Report 78 PVC - Compounds, Processing and Applications, Report 103 Gas Assisted Moulding, T.C. Pearson, Gas Injection Ltd.
J.Leadbitter, J.A. Day, J.L. Ryan, Hydro Polymers Ltd. Report 104 Plastics Profile Extrusion, R.J. Kent, Tangram
Report 79 Rubber Compounding Ingredients - Need, Theory Technology Ltd.
and Innovation, Part I: Vulcanising Systems, Report 105 Rubber Extrusion Theory and Development,
Antidegradants and Particulate Fillers for General B.G. Crowther.
Purpose Rubbers, C. Hepburn, University of Ulster.
Report 106 Properties and Applications of Elastomeric
Report 80 Anti-Corrosion Polymers: PEEK, PEKK and Other Polysulfides, T.C.P. Lee, Oxford Brookes University.
Polyaryls, G. Pritchard, Kingston University.
Report 107 High Performance Polymer Fibres, P.R. Lewis,
Report 81 Thermoplastic Elastomers - Properties and Applications, The Open University.
J.A. Brydson. Report 108 Chemical Characterisation of Polyurethanes,
Report 82 Advances in Blow Moulding Process Optimization, M.J. Forrest, Rapra Technology Ltd.
Andres Garcia-Rejon,Industrial Materials Institute,
National Research Council Canada.
Report 83 Molecular Weight Characterisation of Synthetic
Volume 10
Polymers, S.R. Holding and E. Meehan, Rapra Report 109 Rubber Injection Moulding - A Practical Guide,
Technology Ltd. and Polymer Laboratories Ltd. J.A. Lindsay.
Report 84 Rheology and its Role in Plastics Processing, Report 110 Long-Term and Accelerated Ageing Tests on Rubbers,
P. Prentice, The Nottingham Trent University. R.P. Brown, M.J. Forrest and G. Soulagnet,
Rapra Technology Ltd.
Report 111 Polymer Product Failure, P.R. Lewis,
Volume 8 The Open University.
Report 85 Ring Opening Polymerisation, N. Spassky, Université Report 112 Polystyrene - Synthesis, Production and Applications,
Pierre et Marie Curie. J.R. Wünsch, BASF AG.
Report 86 High Performance Engineering Plastics, Report 113 Rubber-Modified Thermoplastics, H. Keskkula,
D.J. Kemmish, Victrex Ltd. University of Texas at Austin.
Report 87 Rubber to Metal Bonding, B.G. Crowther, Rapra Report 114 Developments in Polyacetylene - Nanopolyacetylene,
Technology Ltd. V.M. Kobryanskii, Russian Academy of Sciences.
Report 88 Plasticisers - Selection, Applications and Implications, Report 115 Metallocene-Catalysed Polymerisation, W. Kaminsky,
A.S. Wilson. University of Hamburg.
Report 116 Compounding in Co-rotating Twin-Screw Extruders,
Report 89 Polymer Membranes - Materials, Structures and
Y. Wang, Tunghai University.
Separation Performance, T. deV. Naylor, The Smart
Chemical Company. Report 117 Rapid Prototyping, Tooling and Manufacturing,
R.J.M. Hague and P.E. Reeves, Edward Mackenzie
Report 90 Rubber Mixing, P.R. Wood. Consulting.
Report 91 Recent Developments in Epoxy Resins, I. Hamerton, Report 118 Liquid Crystal Polymers - Synthesis, Properties and
University of Surrey. Applications, D. Coates, CRL Ltd.
Report 92 Continuous Vulcanisation of Elastomer Profiles, Report 119 Rubbers in Contact with Food, M.J. Forrest and
A. Hill, Meteor Gummiwerke. J.A. Sidwell, Rapra Technology Ltd.
Report 93 Advances in Thermoforming, J.L. Throne, Sherwood Report 120 Electronics Applications of Polymers II, M.T. Goosey,
Technologies Inc. Shipley Ronal.
Volume 11
Report 121 Polyamides as Engineering Thermoplastic Materials,
I.B. Page, BIP Ltd.
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 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
2.3 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
2.4 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
2.5 Elemental Techniques ................................................................................................................... 12
2.6 Microscopy Techniques ................................................................................................................ 12
2.7 Miscellaneous Techniques ............................................................................................................ 12
3. Determination of Molecular Weight and Microstructure of Plastic Polymers ................................ 12
3.1 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
3.2 Monomer Types and Microstructure ............................................................................................ 15
4. Determination of Polymer Type ........................................................................................................... 15
5. Determination of the Plasticiser and Filler in a Plastic Compound ................................................. 19
5.1 Determination of Plasticiser ......................................................................................................... 19
5.2 Determination of Fillers ................................................................................................................ 19
5.2.1 Particulate Fillers .............................................................................................................. 19
5.2.2 Fibrous Fillers ................................................................................................................... 20
6. Determination of Stabilisers in a Plastics Compound ....................................................................... 21
6.1 UV Stabilisers ............................................................................................................................... 21
6.2 Antioxidants .................................................................................................................................. 22
1
Analysis of Plastics
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
3
Analysis of Plastics
4
Analysis of Plastics
Figure 1
13C NMR spectrum of polypropylene-polyethylene copolymer
2.2.5 X-Ray Fluorescence Spectroscopy (XRF) have led to the development of the Raman microscope -
an instrument analogous to the IR microscope.
This technique is very useful for obtaining semi-
quantitative elemental data from plastic compounds and This has enabled Raman spectroscopy to be used
their ashes. Among other things, it helps to identify routinely for the identification of polymer types and
inorganic fillers and pigments in samples. The the analysis of contaminants within polymer samples.
technique is usually used in conjunction with IR.
5
Analysis of Plastics
organic contaminants that may have degraded the the interface between the chromatograph and the
plastic matrix. detector. Today, the two most popular types of
interface for the benchtop single quadrupole LC-MS
There are a variety of ways that the sample or fractions are the particle beam interface and the atmospheric
of the sample (e.g., an extract) can be analysed by GC- pressure ionisation (API) interface. The particle
MS. These include static headspace, dynamic beam interface is used to generate electron ionisation
headspace, solution injection and pyrolysis. (EI) spectra and the API interface is used to generate
either electrospray (ESI) or atmospheric pressure
chemical ionisation (APCI) spectra. A further
2.3.2 Gas Chromatography (GC) complexity is that the API interface can generate
either positive (i.e., molecular ion plus one
hydrogen) spectra or negative (i.e., molecular ion
This technique can also be used to obtain polymer type
minus one hydrogen) spectra.
information by use of a pyrolysis approach, although
the technique is less powerful because of the absence
The particle beam interface is very good for
of a mass spectrometer, and a pyrogram ‘fingerprint’
qualitative work because the 70 eV spectra contain
has to be used and a comparison made against a library
a significant amount of structural information and
of known standards.
can be searched against conventional mass spectra
libraries. However, in the full scan mode the
This technique is also used for the identification and
sensitivity is restricted to the low nanogram levels.
quantification of additives such as antioxidants and,
where sufficient volatility exists, plasticisers and
In the case of the API interface, both the electrospray
organic flame retardants.
and APCI modes are soft ionisation techniques which
leave the molecular ion (or pseudomolecular ion)
intact without much fragmentation. The interface
2.3.3 High Performance Liquid Chromatography therefore offers more sensitivity and is ideal for
(HPLC) quantitative work at low levels (e.g., contamination
of drug and food matrices by polymer additives/
HPLC can be used to identify and quantify additives breakdown products).
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. 2.3.5 Gel Permeation Chromatography (GPC)
HPLC also comes into its own in the quantification of For this technique to be successful the sample must
plasticisers such as dioctyl phthalate (DOP). 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
2.3.4 Liquid Chromatography-Mass Spectroscopy amorphous plastics and semi-crystalline plastics. In
(LC-MS) the amorphous case (e.g., polystyrene), the system
used is set around ambient temperature (30 °C) and
This instrument is essentially a coupling of an HPLC solvents such as THF, chloroform and toluene are
with a mass selective detector and as such offers a used. With semi-crystalline plastics (e.g.,
significant enhancement in performance to the polymer polyolefins), more aggressive solvents such as ortho-
chemist. Although such combinations have been around dichlorobenzene and meta-cresol are used at elevated
for many years, they were complex and expensive (i.e., (140 °C) temperatures.
effectively research tools only), and it is only within
the last five years or so that single quadrupole benchtop In the case of some complex plastic systems (e.g.,
LC-MS systems have become reasonably common blends), the development of interfaces such as the
place due to their relative ease of use and cost. Lab Connections LC Transform, have proved very
useful in increasing the amount of information that
A mass spectrometer can be the ideal detector for can be obtained in a GPC analysis by enabling IR
liquid chromatography because it offers both data to be recorded on the resultant chromatogram.
universality and the required selectivity for complex Hence, with the correct choice of separating column,
analytical problems. For many years development polymer blends can be separated and identified as
work has concentrated particular on the design of well as plasticisers.
6
Analysis of Plastics
2.3.6 Thin Layer Chromatography (TLC) differentiate between different polyethylenes (i.e.,
LDPE, LLDPE, HDPE, etc.) from their melting points
TLC is a relatively simple technique that can be used and the appearance of their melting endotherms as well
for both the separation and identification of additives as being able to detect and, with appropriate standard
such as antioxidants and UV stabilisers. A number of materials, quantify plastic blends, e.g., PP/PE and nylon
approaches are possible using different developing 6/nylon 6,6.
solvents and spraying agents.
The DSC trace for a quenched sample of PET is shown
It is also the case that TLC can be used in a preparative in Figure 2. This trace shows the Tg (around 75 °C) of
way for the isolation of sample fractions for subsequent the material, the exothermic formation of the crystalline
chromatographic or spectroscopic analysis. phase (at 156.9 °C) and the endotherm due to the
melting of this phase (at 255 °C).
TLC does have the image of being somewhat old
fashioned and it is to be expected that the market The DSC trace of a plastic blend is shown in Figure 3.
penetration of LC-MS systems will further erode the The data obtained has been compared to standards and
standing of this technique in the modern analytical the material has been shown to be a blend of ethylene-
laboratory. vinyl 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).
2.4 Thermal Techniques
Although not as sensitive as dynamic mechanical
2.4.1 Differential Scanning Calorimetry (DSC) thermal analysis (DMTA) to glass transitions, DSC can
be used to identify a plastic from the glass transition in
DSC is used extensively in the analysis of plastics, its thermogram. The glass transition (Tg) and crystalline
particularly those that are semi-crystalline - polyolefins, melting temperatures (Tm) of a range of plastics are
nylons, polyesters, etc. It is sensitive enough to 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 of temperature on this important material property can
fingerprint thermograms from which deviations in the be obtained over a wide temperature range (typically
composition of a plastic compound can be detected. –150 °C to +200 °C), along with the glass transition
One reason for this is that although the technique is temperature and information on thermal stability.
not capable of determining the molecular weight of a
plastic, differences in molecular weight will be apparent The use of DMTA to differentiate between plastic
in the melting endotherm region. samples that have a similar chemical composition, but
very different physical properties is shown in
Using appropriate standard materials it is also Figure 4. Both of these samples are polymethyl-
possible to use DSC to quantify the level of certain methacrylate (PMMA), but the top one is crosslinked
additives, e.g., peroxides, in a sample. having been prepared with a small amount of
difunctional monomer and the bottom sample is the
DSC can also be used in thermal stability studies of standard thermoplastic material. It can be seen that
the plastic compound, and to investigate the the crosslinked sample does not melt and the modulus
effectiveness of antidegradants and fire retardants. does not fall away significantly until thermal
degradation occurs.
2.4.2 Dynamic Mechnanical Thermal Analysis The sensitivity of DMTA to glass transition
(DMTA) temperatures (approximately 1,000 times greater than
DSC which measures heat capacity changes rather than
DMTA is very useful for generating modulus versus modulus) is very useful in the analysis of plastics and
temperature data on plastic compounds. The effects their blends.
8
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
Polyacrylonitrile 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
This technique is useful in the analysis of compounded Heat from ambient to 550 °C in a nitrogen atmosphere
plastic samples. It is possible to obtain accurate at 20 °C/min until no further weight loss occurs. Then,
quantifications of the principal compound constituents reduce the heat to 300 °C, change the atmosphere to
such as plasticiser, polymer and inorganic species. air and heat at 20 °C/min to 1,000 °C.
This data can be obtained on small (e.g., 10 mg)
samples in a relatively short time (around 45 minutes). It is common to plot the weight loss derivative in
By the use of the temperature maxima at which weight conjunction with the weight loss, and this can be used
events occur it is also possible to use the technique to to detect the presence of a polymer blend of two or more
obtain some qualitative assignments for the plasticiser components. Thermal decomposition temperatures of a
and polymer. 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
Other uses for the technique include the production of The introduction of high resolution TGA instruments
compositional fingerprints for quality control purposes has enabled more accurate quantifications of minor
and the investigation of thermal stability and the effects weight loss events to be made. For example, the use of
that additives such as flame retardants and antioxidants high resolution TGA to quantify the amount of residual
have on it. monomer in a sample of polymethylmethacrylate is
shown in Figure 5. The residual monomer weight loss
It is possible to interface modern TGA instruments directly event peaks at 297.5 °C.
to IR instruments or mass spectrometers, thus obtaining
both quantitative and qualitative data in one analytical step.
Figure 5
High resolution TGA of polymethylmethacrylate
11
Analysis of Plastics
2.5 Elemental Techniques of inorganic additives (e.g., rutile and anatase forms
of titanium dioxide) and direct probe mass
The determination of the concentration of certain spectroscopy (for the determination of high molecular
elements can be very useful in plastic analysis work. weight antioxidants).
In particular, it is often necessary to determine the
amount of nitrogen or a halogen such as chlorine or Surface analysis techniques such as secondary ion mass
fluorine in the calculation of polymer content or spectrometry (SIMS), laser induced mass analysis
polymer blend proportions. Also, the targeting of (LIMA) and X-ray photoelectron spectroscopy (XPS)
specific elements can enable the quantity of a are used for failure diagnosis work associated with such
particular additive (e.g., phosphate flame retardant or things as poor bonding to substrates and for surface
titanium dioxide pigment) to be calculated. characterisation work.
The determination of nitrogen is usually done using A chromatography technique that achieved prominence
carbon/hydrogen/nitrogen analysers and the technique in the research literature around ten to fifteen years
is relatively simple and uses small amounts (e.g., 20- ago for the determination of relative high molecular
50 mg) of sample. weight additives (e.g., antioxidants) and the study of
plastic oligomers is supercritical fluid chromatography
With the other elements, the technique will vary (SFC). This is essentially a liquid chromatography
according to the element being quantified. Sulfur and technique that uses similar analytical columns to HPLC
chlorine, for example, can be determined using but where the mobile phase is a substance (e.g., carbon
oxygen combustion followed by ion chromatography dioxide) that is kept in a supercritical state by a suitable
analysis of the products. 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
2.6 Microscopy Techniques
can be deposited on infrared transparent substrates for
analysis using an infrared microscope. The relatively
High magnification (e.g., 150x) optical microscopy
expensive nature of the instrumentation and the
can be used to examine the dispersion of fillers within
development of other techniques (e.g., LC-MS) have
the plastic matrix. The success of this operation is
restricted its market penetration.
usually dependent on the generation of high quality
microtome sections of the sample.
12
Analysis of Plastics
Mn = Number average molecular weight = Sum nM 3.1.1 Gel Permeation Chromatography (GPC)
Sum n
This is the pre-eminent technique and has been refined
Mw = Weight average molecular weight = Sum nM2 and developed extensively over the past 30 years.
Sum nM
It is possible to use it on both uncompounded resins
Mz = Z average molecular weight = Sum nM3 and plastic compounds and Mn, Mw and Mz values
Sum nM2 can be obtained. GPC is essentially a liquid
chromatography technique where the sample is
where n = the number of molecules of molar mass M. dissolved in a suitable solvent (e.g., THF for
polystyrene) and injected into a system where the
molecules are separated according to their molecular
The Z average is very sensitive to high molecular
size by a column that contains a swollen, particulate,
weight molecules within the polymer. The weight
porous gel packing.
average is always of greater value than the number
average. A measure of the breadth of the molecular
Figure 6 shows the GPC chromatograms for two
distribution of the polymer can be obtained by dividing
polymers that have different molecular weight
the weight average by the number average:
distributions but similar calculated molecular weight
averages.
Polydispersity = Mw
Mn
The standard detector for GPC systems is the refractive
index (RI) detector, but a feature of developments over
As the polymer tends to monodispersity the the past 10 years is the development of double (RI and
polydispersity approaches unity. viscosity) or triple detector systems (RI, viscosity and
light scattering). These multiple detection systems
There are a wide variety of methods that can be used provide measures of ‘true’ molecular weight by
to obtain molecular weights. The principal ones are obtaining the actual Mark-Houwink parameters (in the
as follows. 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
Depending on the source of the Mark-Houwink Light scattering can produce precise data and has been
parameters the molecular weight can be expressed as used successfully on polymers with molecular weights
either the number or weight average. ranging from 10,000 to 10,000,000.
14
Analysis of Plastics
NMR instruments can also be used to obtain One of the most comprehensive databases available
fundamental structural information on polymers such of plastic infrared spectra has been produced by
as end group chemistry, branch points and structural Hummel (a.9).
isomerism. It is also possible to use IR for the latter,
although some of the isomeric structures have relatively Where the plastic sample contains both a major organic
weak absorptions which makes detection difficult when additive and a filler, it is necessary to pyrolyse the
they are at a low concentration. 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
4 Determination of Polymer Type and polymer blends. In the case of blends, it is also
possible to express the results semi-quantitatively if
One of the most basic and useful tests to carry out on a the appropriate standards are available.
plastic sample is to determine its polymer type.
If the plastic only contains a filler, the pyrolysis
Due to their relative simplicity, it is usually possible to approach can be employed without using the initial
carry out an infrared analysis of the plastic material in solvent extraction step.
the as received state and identify the plastic by reference
to a standards database. The advent of the single bounce The pyrolysate infrared spectra of nylon 6 and low
attenuated total reflectance (ATR) accessories for density polyethylene are shown in Figures 9 and 10,
Fourier transform infrared spectroscopy (FTIR) respectively.
instruments enables this operation to be carried out in
a matter of minutes on a sample a few millimetres in Another method which enables the polymer type within
size. Some care should be taken as the relative a plastic sample to be identified is pyrolysis gas
intensities of the bands present in ATR spectra can vary 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 Adding a mass spectrometer into the system, so that
received. In the former case any relatively low molecular the technique becomes pyrolysis GC-MS, further
weight plasticiser elutes early on and does not have a increases the usefulness of the method and the
significant influence on the pyrogram as a whole. As information that can be obtained.
with pyrolysis IR, a database of standards needs to be
put together and then the pyrogram fingerprints of The principal diagnostic pyrolysis species which can
unknowns can be matched. The temperature that the be detected in pyrograms of plastics are shown in
pyrolysis unit is set at, and the design of the unit (e.g., Table 4.
Curie point or microfurnace), will affect the pyrograms
produced from a particular sample. Again, it is possible It can be seen from the above list that certain plastics
to identify and quantify blends and blend ratios. ‘unzip’ to regenerate their monomers whereas other
undergo decomposition reactions to generate
Typical experimental conditions for pyrolysis GC characteristic breakdown products. In reality, a
experiments are as follows: certain amount of both types of reaction take place
for the majority of polymers and it is the one that
Sample weights 0.1-5.0 mg
predominates that determines what the major
Pyrolysis temperatures 400-800 °C (microfurnace pyrolysis products will be.
and Curie point)
With respect to the quantification of the polymer
800-1200 °C (platinum component within a plastic compound, the easiest
filament) technique to use is TGA. It is also possible to detect a
blend of polymers with TGA and to often obtain a
Microfurnace type pyrolyser - specific example using semi-quantification of the blend ratio by reference to
an SGE Pyrojector the splitting of the weight loss derivative.
Unfortunately, some plastic types (e.g., PVC) undergo
Weight of sample 0.4 mg two stage weight loss processes when heated and the
Pyrolysis temperature 600 °C first stage (loss of hydrogen chloride) will overlap
with the volatilisation of organics (e.g., plasticiser)
Pyrolysis gas Helium at 0.10 MPa stage. It is therefore not possible to use TGA alone to
determine the polymer content of these samples.
GC column 5% Diphenyl siloxane 30
m x 0.25 mm, 1.0 μm film
Another complicating factor is that a number of plastics
GC column temperature 2 min at 50 °C followed (e.g., halogenated, polyamides, polyurethanes,
program by 10 °C/min to 280 °C polyesters, other heteroatom containing systems) do
and then 10 min at 280 °C not completely pyrolyse during the nitrogen
atmosphere region and leave a carbonaceous residue
GC carrier gas Helium at 0.06 MPa which essentially oxidises to carbon dioxide in the air
region. This carbonaceous residue, which may to an
GC injector temperature 320 °C
extent overlap with any weight loss due to a carbon
Detector Flame ionisation detector black pigment, has to be included in order to obtain an
(FID) at 350 °C accurate polymer content.
18
Analysis of Plastics
5 Determination of the Plasticiser and conventional carbon black; the former having a
maximum oxidation weight loss around 700 °C and
Filler in a Plastic Compound 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 The fact that a number of rubbers (e.g., halogenated,
solvent extraction. Careful choice of solvent is nitrile and polyurethane) produce carbonaceous
required to ensure that the polymer itself doesn’t residues during the nitrogen atmosphere region has
undergo dissolution and that the plasticiser is already been mentioned in Section 4.1, and care must
selectively isolated. A solvent which has been found be taken to ensure that these do not affect the
to be useful for polymers such as PVC is methanol. quantification of the carbonaceous filler in the air
The extraction is carried out under Soxhlet atmosphere region. Use of a high resolution TGA
conditions with the weight of extract being obtained instrument will assist in this as it will improve the
from the weight gain of the conditioned solvent separation of the two weight loss events.
reservoir flask once the solvent has been dried off
at 105 °C. TGA is also convenient for the quantification of
inorganic fillers such as barytes, silica and silicates.
Having quantified the plasticiser present by The limitation of the technique is that the total
extraction it is then possible to obtain an inorganic content of the plastic is obtained, with no
identification by the use of transmission IR. There indication of the relative proportion if a blend of
is an excellent database available (399) which inorganic fillers is present. It is therefore common
enables an identification to be made. Where the practice to complement the TGA data with a least a
plasticisers have distinct IR spectra (e.g., phthalates semi-quantitative elemental technique such as XRF
and sulfonamides) it is possible to detect the in order to obtain qualitative as well as quantitative
presence of a blend of plasticisers. If a quantification data. A useful exception to this rule is where the
of the blend composition is required, though, this is compound contains calcium carbonate (a relatively
usually easier to achieve by HPLC then IR. common diluent filler), in which case the carbonate
will undergo quantitative degradation at around 680-
The TGA technique can usually provide a good 700 °C into carbon dioxide and calcium oxide (which
quantification of plasticiser content. Plasticisers that remains as a residue). It is therefore possible to
have higher molecular weights (e.g., so called quantity the amount of calcium carbonate in the
polymerised plasticisers) can give problems as the sample from the carbon dioxide weight loss (which
weight loss event due to their volatilisation can will represent 44% of the carbonate by mass) and
merge with the pyrolysis weight loss event of the the remaining quantity of residue will indicate if any
polymer. As mentioned in the above section, other inorganics are present.
polymers that lose small molecules by heat
degradation (e.g., HCl lost by PVC) give more The other technique commonly used for the
complicated TGA traces and will require a solvent quantification and isolation of inorganic materials
extraction step to determine their plasticiser level. (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
5.2 Determination of Fillers usually used.
5.2.1 Particulate Fillers Once the ash has been obtained, qualitative
information on the inorganic species present can be
On some occasions, carbonaceous fillers such as a obtained by IR (liquid paraffin mull technique), XRF
conducting black (acetylene black) or graphite are or, where the quantification of specific species is
added to a plastic to enable it to meet certain required, ICP.
conductivity requirements. It is possible to use TGA
to quantify these types of fillers. It is also a useful Some of the principal diagnostic IR absorption bands
way of differentiating between these materials and 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
20
Analysis of Plastics
the wood flour filler type, and be able to detect the type antidegradant identified by reference to its molecular
of synthetic fibre (e.g., nylon or polypropylene) used ion and a database. The direct probe mass spectroscopy
from its characteristic transmission spectrum. technique can be carried out on samples in the as
received state as well as sample extracts, whereas LC-
TGA will enable the amount of carbon fibres in a MS is only used for extracts.
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
6.1 UV Stabilisers
confirmation of their presence.
There is a large range of commercial UV stabilisers
As mentioned above, synthetic polymeric fibres can be
for plastic materials and a number of analytical
identified by the IR microscope once sufficiently isolated
approaches can be used for their detection and
or, by use of their melting point, by the hot stage
quantification.
microscope or DSC. In the case of DSC, some
quantification data can be obtained from the size of the
The UV stabilisers can be divided into five different
melting endotherm providing standards are available.
groups:
21
Analysis of Plastics
solution (0.8% w/v of polymer) of polystyrene by The chromatogram obtained for the determination of
excitation at 370 nm and recording the fluorescence at Irganox 1076 in an HDPE compound is shown in
435 nm. Standard solutions at the 0.8 w/v level of virgin Figure 12. An extract of the polymer was analysed
polystyrene and known amounts of Uvitex OB are used using a C18 reverse phase column with UV detection at
as calibrants. 230 nm and a mobile phase of 70:30 methanol/water
changing to 100% methanol.
It is also possible to use gas chromatography (e.g.,
Tinuvin P, Tinuvin 326, Tinuvin 327 and Cyasorb There is a useful HPLC method which can be used on
UV531 in toluene extracts of polyethylenes), thin layer plastics for the detection and quantification of a wide
chromatography (e.g., benzophenone and salicylic acid range (20 species) of antidegradants. The sample is
types in polyethylenes) and HPLC. This latter method dissolved up using a suitable solvent at an elevated
has been used extensively for the determination of temperature if necessary. A non-solvent (e.g., methanol)
antioxidants but has not received as much attention in is then added and the extract analysed by HPLC using
the literature for UV stabilisers. the following conditions:
It is also the case that the white pigment titanium Injection volume 25 μl
dioxide provides protection against UV light and so
this can be added at reasonable high loadings (e.g., 10% HPLC column Aqua 5 C18 ODS reverse phase
or greater) to products such as window frames. The column 150 mm x 3.0 mm
amount of titanium dioxide in a plastic can be (or similar)
determined after acid digestion of the matrix by the
use of an elemental technique such as AAS/ICP. Mobile phase A= 75:25 Methanol/Water
B= 50:50 Ethyl Acetate/Acetonitrile
Gradient Time %A %B
6.2 Antioxidants
Initial 90 10
HPLC based techniques have been widely used by After 25 min 0 100
analysts for the determination of antioxidants in plastics
and a review has been provided by Sidwell (400). Flow rate 2.0 ml/min
Figure 12
HPLC chromatogram of HDPE for determining Irganox 1076
22
Analysis of Plastics
Detection UV detector set at 270 nm The chromatogram obtained using this method to
separate a complex cocktail of antidegradants is shown
Temperature 40 °C in Figure 13.
The following antioxidants are examples of those that The wide applicability of this method is due to the
can be determined using this technique: mobile phase mixture.
(1) Irganox 1010 The capability of HPLC has been greatly extended by
the commercialisation of affordable liquid
(2) Irganox 1098 chromatography-mass spectroscopy (LC-MS)
instruments. The mass selective detector enables
(3) Irganox 1076 unknown samples to be analysed and the antioxidants
present to be identified. The LC-MS technique
(4) Irganox 1330
therefore compliments GC-MS and, with it, enables
(5) Butylated hydroxytoluene the complete molecular weight/volatility/polarity range
to be covered.
(6) Irgafos 168
TLC is comparatively easy and cheap to use and it is
(7) Triclosan both quick and accurate for the identification of
Figure 13
HPLC chromatogram of a complex mixture of antidegradants
23
Analysis of Plastics
Using the general analysis conditions shown below a 7.1 Process Aids and Lubricants
number of antioxidants can be detected in toluene or
chloroform extracts of plastics: In PVC technology certain polymeric additives can be
considered as process aids. These polymers have a
Sample preparation: Around 5 mg of extract is diluted similar composition to those used as impact modifiers
1/20 with 80% acetonitrile/water in PVC formulations but are more compatible and so
are primarily included to ensure more uniform flow
Instrument: Agilant 1100 series LC-MS and hence improve surface finish. Such process aids
include ABS, chlorinated polyethylene, MBS, EVA-
Column: Zorbac SB-C18, 5 um, PVC graft polymers and acrylate-methacrylate
2.1 mm x 150 mm copolymers. As these are usually found in unplasticised
PVC, direct analysis of the product by IR will usually
Mobile phase: A=water, B=acetonitrile indicate the presence of those that have a distinctive
spectrum as no masking by plasticiser will take place.
Gradient Time A B However, even rigid PVC can contain a small amount
of phthalate and so it is advisable to carry out a solvent
Initially 15% 85%
extraction to clean up the matrix first. Where the
after 10 min 1% 99% process aid (e.g., chlorinated polyethylene) has a
relatively bland spectrum, a technique such as NMR
or Initially 35% 65% will be required to both detect and quantify it. NMR
after 10 min 10% 90% will usually be required to quantify the other types as
well, unless the spectrum is very distinctive and
Flow rate: 0.7 ml/min standards of known composition are available.
24
Analysis of Plastics
In the case where a relatively large quantity of filler available, they have relatively high molecular weights
(talc) has to be incorporated into a polymer (e.g., and so cannot be easily removed from the matrix by
polypropylene) it is often necessary to use a process solvent extraction and can be thermally labile.
aid/lubricant such as a zinc or calcium stearate. A
quantification of the process aid can be achieved by One technique which has been used to identify both these
the analysis of the sample for the metal by acid types of pigment and inorganic ones is vapour phase
digestion-AAS. The stearate can be qualitatively ultraviolet absorption spectrometry at 200 nm (a.11). In
detected by solvent extraction GC-MS. this method the samples are powdered and then directly
vapourised in the heated graphite atomiser. Thermal
ultraviolet profiles of organic pigments show absorption
7.2 Slip Additives 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
It is common for aliphatic amides to be incorporated
made with respect to temperature, relative intensity and
into plastics, particularly polyethylenes, to act as slip
additives. width of the absorption bands.
It is possible to use LC-MS to detect these types of A relatively unknown technique (laser desorption fourier
slip additives in plastic samples. Using the LC-MS transform ion cyclotron resonance mass spectroscopy)
conditions described in Section 6.2, it is possible to has been used (397) to identify dyes in plastics such as
detect Behenamide (mixture of two aliphatic amides polymethylmethacrylate. A detection limit of 0.1% was
of molecular weight 331 and 339) and erucamide obtained, which compared with a limit of 1-2% using
(molecular weight 337) in solvent extracts of an ATR infrared spectroscopy technique.
polyethylene and polypropylene.
Infrared spectroscopy techniques can be useful,
It is also possible to use GC and GC-MS to analyse particularly if the plastic matrix itself (e.g., polyethylene)
these and another common slip additive oleamide in has a relatively simple infrared spectrum and if standard
extracts from plastics as they have sufficient volatility infrared spectra of a wide range of pigments is available.
to elute from the GC column.
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
7.3 Pigments can be difficult due to the small sample size (10 mg)
used. The standard method to quantify the amount of
Pigments are used extensively in plastic compounds carbon black in such a product is therefore the tube
and can be of one of four main types: furnace as much larger sample sizes can be used (e.g.,
2 g) and hence more accurate quantifications obtained.
(1) Inorganic compounds
25
Analysis of Plastics
In the case of polystyrene, quaternary ammonium Column type: RTX5-MS 30 m x 0.25 mm,
compounds are widely used and for polyethylene, 0.25 μm film thickness
polyethylene glycol alkyl esters can be used.
Column temperature: 40 °C for 5 min, 20 °C/min
In the case of the glycol esters, these can of sufficiently up to 300 °C held for 12 min
low molecular weight to be extractable by solvents such
as diethyl ether and then identified by a chromatographic MS settings: 20 to 620 Daltons scanned
technique such as GC-MS. As in a number of cases it is every 0.33 s
to be expected that LC-MS will play a role in the analysis
of these additives in the future. 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
7.5 Crosslinking Agents and Co-Agents
Tenax filled trap. The experimental conditions are as
follows:
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 Dynamic Headspace
properties. This can be achieved by irradiation using Instrument: Perkin Elmer ATD 400
gamma rays. However, some polymers degrade when
subjected to high energy radiation as illustrated in Desorption temperature: 150 °C for 10 min
Table 6. Chemical agents such as peroxides are also
used. These species produce diagnostic breakdown Desorption flow: Helium @ 20 ml/min
products the identification of which will reveal the Trap collection temperature: –30 °C
type of peroxide used.
Trap injection temperature: 250 °C
The most useful technique for this type of work is GC-
MS. There are two possible modes of sample Trap outlet split flow: 9 ml/min
introduction: solution injection and dynamic Trap inlet split flow: off
headspace. In the case of the former a useful method
of sample preparation involves cryogenic grinding of Split: 10:1
0.3 g of the sample, followed by extraction using 2 ml
of diethyl ether in an ultrasonic bath for 30 minutes. GC-MS
The resulting extract is then analysed under the
following conditions: The conditions used are the same as for the diethyl
ether method with the exception of the following:
Instrument: Hewlett Packard 6890/5973 GC-MSD
GC Column temperature: –30 °C to 50 °C at 5 °C/min,
Carrier: Helium @ 2.0 ml/min constant flow following by 20 °C/min to
300 °C and then held at
Injection mode: 1 μl splitless (0.75 min; 50 ml/min) 300 °C for 12 min
26
Analysis of Plastics
For either analytical approach, identification of the (2) Physical Low boiling point organic compounds
diagnostic cure system breakdown species is by (e.g., dichloromethane or pentane)
reference to mass spectral libraries such as those which volatilise at the processing
produced by the National Institute of Standards and temperature to create a cellular
Technology (USA) (NIST), the Royal Society of structure.
Chemistry, Wiley/NBS (a.12) and the US
Environmental Protection Agency (EPA)/National With plastics, the most widely used type are the
Institute of Health (NIH). The mass spectra of the physical blowing agents.
majority of species of interest are in these libraries and
so, providing the knowledge to reconstruct cure systems Where it is suspected that a physical type blowing
is available, successful attempts can be made. agent has been used to produce a foam, is it possible
to use headspace GC-MS to identify it. Even in the
One problem associated with this task is that a number blown state, the high sensitivity of the technique
of peroxide curing agents breakdown to give more that enables an assignment to be made from the small
one product and a number of these are common to more amount of residual blowing agent that will be present.
than one peroxide species. This is demonstrated in It is usual to use this type of blowing agent in
Table 7. amorphous plastics that have glass transition
temperatures around 100 °C, e.g., styrenics. This
In addition to identifying the type of peroxide used, enable the expansion of the plastic to be well
these GC-MS techniques will also identify the type of controlled.
co-agent (e.g., triallyl cyanurate (TAC) or triallyl
isocyanurate (TAIC)) used. 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
7.6 Blowing Agents approach that is used is to indirectly identify them by
the determination of breakdown fragments. The GC-
There are two main types of blowing agent used with MS instrument is the best choice for this and a library
polymer systems in general: of typical breakdown fragments is required.
(1) Chemical Chemical compounds (principally Quantification of the chemical blowing agent in an
organic) that undergo chemical unblown product is very difficult as the polarity and
decomposition at the processing reactivity (e.g., hydrogen bonding reactions and
temperature to form a gaseous species thermal instability) can cause problems during isolation
(e.g., nitrogen) which will create the from the compound and subsequent analysis. In terms
cellular structure. of reverse engineering, this is unlikely to be required
since the product will invariably be already blown. For
Examples include azo compounds, laboratories that are carrying out quality control work,
nitroso compounds, sulfonyl hydrazide other properties such density and expansion ration can
compounds and sodium bicarbonate. be used to determine compound loadings.
27
Analysis of Plastics
7.7 Flame Retardants distribution within the matrix of the domains that
contain it. Actual impact performance is determined
As with blowing agents, there are two main categories by physical tests such as the Charpy and Izod impact
of flame retardant: organic and inorganic. tests, and the size and distribution of domains is
investigated by transmission electron microscopy
The amount and type of organic flame retardant present (TEM), but there are a number of chemical tests that
in a plastic compound can be determined in an can be carried out to determine the level of modifier.
analogous way to the plasticiser, since this type of flame
retardant is usually similar in molecular weight and (1) IR analysis - this is performed on a pressed film
polarity and, hence, extractability. Once the type of and the relative size of the absorption bands due to
organic flame retardant has been determined by IR, an styrene (700 cm) and butadiene (966 cm) are taken
accurate quantification can be obtained by carrying out and compared to standards of known styrene-
an elemental analysis for the halogen (or other relevant butadiene levels.
element, e.g., phosphorus) on the unextracted sample.
The extract value itself will rarely provide a meaningful (2) NMR - the plastic is dissolved and the level of the
quantification as other species, particularly any process two polymers determined by specific shift areas.
aid/plasticiser, will contribute to it as well. In some
instances (e.g., organophosphates) it may be possible (3) Classical wet chemistry - the butadiene level is
to use an HPLC analysis of the extract to quantify the determined in solution by reaction of a reagent with
flame retardant. GC based techniques can also be used the double bonds.
in some cases, but bromide types present problems for
these techniques because of their relatively high There are some instances (e.g., rubber impact
molecular weights (> 900). modification of nylon) where the chemical properties
of the two polymers are so dissimilar that solubility
Care must be taken over the quantification of inorganic differences can be used to isolate and, in this case,
flame retardants, since some of them (e.g., antimony quantify the rubber modifier. The test is carried out by
trioxide) can react with the organic flame retardant taking an accurately weighed sample and refluxing it
present, or break down to produce volatile products, in formic acid until the plastic is digested and only the
under quantitative ashing conditions, and during rubber phase remains. The rubber is then washed, dried
analysis by thermal techniques such as TGA. A good and weighed.
initial approach is a semi-quantitative elemental
analysis by XRF, to see which types are present. Other plastics which can contain rubber modifiers (or
Accurate quantifications can then be obtained by at least modifiers that have lower glass transition
precise elemental determinations. temperatures than the plastic phase) include PET and
PVC. In the case of PVC, acrylates and methacrylates
If it is known that hydrated alumina is present in the are common and the normal approach is to use IR to
sample, it is possible to quantify this reasonably well detect the modifier and then NMR to quantify it.
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.
8 Analysis of Plastics for Food
Contact Use
7.8 Impact Modifiers
For more than 30 years work has been going on
The most commonly encountered impact modified involving food contact plastics and the effect that
plastic is high impact polystyrene (HIPS). The impact migrants from plastics products have on food. The first
modification is achieved by incorporating discreet European Directive (78/142/EEC), which was on the
domains of a rubber (butadiene) within the polystyrene vinyl chloride monomer content of food contact PVC,
matrix. The level of butadiene can be varied according was published in the late 1970s and this was followed
to the requirements of the end use. A high level can ultimately by the more comprehensive Plastics
convert a glassy brittle material into a ductile, tough Directive (90/128/EEC) in 1990. Since 1990, there has
product. The efficiency of the butadiene to improve been a gradual harmonisation of European testing
impact resistance alone is not solely related to requirements through amendments to 90/128/EEC. The
concentration, but is also dependent on the size and seventh amendment (2002/17/EC) has recently been
28
Analysis of Plastics
published and the initial requirements for testing overall 8.1 Global Migration Tests
and specific monomer migration have now grown to
include additive (e.g., antioxidant) migration. The following food simulants are used for food contact
plastics:
In general, there are two types of analytical test that
are carried out on food contact plastics: Distilled water - Aqueous food use
(1) Global migration tests - In these, the plastic is put Distilled water 95%:Ethanol 5% - Alcoholic
into contact with an appropriate food simulant beverages such as beers and lagers
under representative end use conditions and the
total amount of material that has migrated into the Distilled water 85%:Ethanol 15% - Wines
simulant determined gravimetrically or, in the case
of involatile food simulants such as olive oil, by Distilled water 60%:Ethanol 40% - Spirits
gas chromatography.
A solution of 3% w/v acetic acid in distilled water -
(2) Specific migration tests - Again, the plastic is Acidic aqueous foods
contacted with a food simulant but any analytical
work in targeted on a specific additive and its Olive oil* - Fatty foods (also isopropanol or hexane)
concentration determined using an appropriate (*Isopropanol and Hexane have been introduced
chromatographic technique. as fatty food simulants to circumvent the analytical
problems that can occur with olive oil due to its
In the case of certain plastics materials, e.g., ABS, potential variability as a natural product and
grades that are intended for food use have to meet involatility.)
certain residual monomer targets. Direct analysis of
these polymers is undertaken to determine the As mentioned, the global migration figure for a particular
concentration of these monomers. plastics material is determined gravimetrically. One
29
Analysis of Plastics
approach is to use conditioned glass crucibles and to 8.2 Specific migration and residual monomer tests
dry off the simulant on a hot plate after the contact
experiment has been performed under the appropriate In addition to the global migration limit 90/128/EEC
conditions (time and temperature). also provides a number of specific migration limits
(SMLs) for plastic monomers (Table 9).
Once the appropriate simulant has been chosen the
contact time and temperature to use are given in EC There are also SMLs for plastic additives, some
Directive 82/711/EEC (Table 8). examples are shown in Table 10.
In addition, for plastics in contact with food for which In the case of some monomers, 90/128/EEC gives limits
a preservation temperature of less than 20 °C is required (called quantification limit-monomer (Qm)) relating to
the test condition will be 10 days at 20 °C. the plastic material itself. For example, vinylidene
chloride has a QM of 5 mg/kg of plastic.
The overall global migration limit for plastics is stated
in the EC Directive 90/128/EEC as being 10 mg/dm2 Over the years, the detection of species migrating from
(surface area of plastic). This limit can be expressed as food contact materials has advanced hand in hand with
60 mg/kg of foodstuff in certain situations. To be used the gradual lowering of analytical detection limits
for food contact a plastics product must meet this brought about by the refinement of the techniques. For
requirement. example, the SML for acrylonitrile is set at not
detectable above 0.02 mg/kg (i.e., 20 parts per billion)
In a number of packaging types, only one side of a and this would not be obtainable on a routine basis
plastic film or laminate may contact the food. Specific without the benefits of modern instrumentation.
single side migration cells have been developed (e.g.,
by PIRA) to enable the migration from a material under The development of suitable methods for the detection
these conditions to be investigated. of the wide range of monomers and additives used in
30
Analysis of Plastics
food contact materials requires the application of state 9 Determination of Stabilisers in PVC
of the art analytical techniques. Normally, headspace
methods are preferred for volatile monomers as such
Although it is one of the bulk thermoplastics, PVC
methods overcome a lot of the problems of sample matrix
suffers from relatively poor stability to ageing agencies
clean-up. In principle the food contact simulant, foodstuff
such as heat and UV light. In order to achieve its status
or plastic material is heated in a sealed vial fitted with
as an important plastic it was therefore necessary to
an inert septum (usually PTFE coated rubber). The vial
develop a specific additive group: PVC stabilisers.
is heated to an accurate set temperature normally in the
range 80-100 °C, for an equilibrium time of at least one
These technological developments have resulted in a
hour. The headspace above the sample is then analysed
range of stabilisers being available that are appropriate
for the presence of the analyte. The quantity of analyte
for different grades of PVC, products and end uses.
in the headspace will always be in equilibrium with the
Some of the main types are:
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, (a) Lead stabilisers (e.g., lead carbonate, lead stearate,
temperature and ratio of headspace to bulk material lead phthalate)
(polymer if necessary)) as the samples. To acquire
sufficiently low detection limits it is sometimes (b) Metallic soaps (e.g., stearates, palmitates,
necessary to use specific detectors (e.g., a nitrogen/ ricinoleates and octoates of cadmium, barium,
phosphorus detector (NPD)) or, in the case of mass calcium and zinc)
selective detectors, a single ion monitoring approach.
For species that are too involatile for headspace based (c) Organo-tin compounds (e.g., dibutyltin di-iso-
methods, other chromatographic and spectroscopic octylthioglycollate)
methods are employed.
(d) Epoxide stabilisers (e.g., epoxidised oils and
A summary of the analytical techniques used in food bisphenol A epoxide resins).
migration work is shown in Table 11.
The analyst has to bear in mind that it is common for a
In the cases where HPLC has been assigned, LC-MS number of different stabilisers to be used in a PVC
would also be applicable. compound in order achieve the optimum ageing resistance.
31
Analysis of Plastics
It is obvious that a large number of these stabilisers Of the other types of organo-metallic stabilisers,
contain metal atoms and so a cost effective way of Mal’kova and co-workers (a.17) have described an
achieving an initial evaluation of the type of stabiliser alternating current polarographic method for the
present is to use a semi-quantitative XRF technique determination of cadmium, zinc and barium stearates
on the sample in the as received state. Care should be or laurates in PVC. Other techniques used on PVC
taken with this as some inorganic pigments/fillers extracts include, column chromatography for barium,
(e.g., titanium dioxide) can mask certain key elements cadmium and zinc salts of fatty acids, paper
(e.g., cadmium). chromatography for cadmium, lead and zinc salts of
fatty acids (a.18) and polarography for cadmium, lead
If it is a case of quantifying a known stabiliser, then and zinc salts (a.19).
AAS or ICP can be used to quantify the metal and, with
knowledge of the compound formula, the result obtained. The advent of bench top LC-MS instruments has
enabled the analysis of stabilisers such as the organo-
tin type to be re-examined and laboratories such as
The organo-tin compounds are widely used and for
the Analysis Division at Rapra Technology Limited
analytical considerations it is convenient to divide them
are investigating the capability of this technique in
into those that contain sulfur and those that do not. To
this area. This could be another area of plastics
the first group belong compounds like dialkyltin
analysis where LC-MS replaces the more traditional
mercaptides, mercaptoesters and mercapto
techniques.
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
10 Analysis of Plastic Laminates and
mercaptoesters presents little or no difficulty. However,
the identification of the thioacid and of the alkyl groups Fibres
attached directly to tin can prove more difficult,
especially if long chain acids form part of the compound Plastic laminates are used extensively from the ordinary
or if the stabiliser is not pure, e.g., if it contains crisp packet to high specification products for medical
plasticiser. The thioacid may also tend to decompose and pharmaceutical use. In all these cases, laminates
during hydrolysis procedures. The application of a are used since the application demands a number of
number of analytical methods (e.g., NMR, IR and GC) properties which no single polymer exhibits.
to determine these types of stabiliser in PVC extracts
have been described by Udris (a.13). Taking the example of the crisp packet, the innermost
layer must be inert to the product and provide a barrier
Some classic methods based on titration and TLC to to air, the outside layer has to be capable of being
printed onto and the middle layer (or tie layer) has to
determine organo-tin compounds in solvent extracts
be able to stick both of the other two together.
of PVC include:
One of the principle analytical techniques for the
• Potentiometric titration of organo-tin in the extract
analysis of laminates is the infrared microscope. This
with standard sodium methoxide in pyridine using
instrument is capable of recording transmission infrared
antimony and calomel electrodes (a.14).
spectra from sample down to 10 square microns in size.
The approach is usually to prepare a section of the
• Titration of dialkyltin thiol compounds in benzene/ laminate by microtoming a section and then recording
methanol extract with standard silver nitrate (in IPA a spectrum of each layer aided by the masking off of
medium) using sulfide coated wire electrode (a.13). the other layers. The sectioning is often undertaken
obliquely in order to maximise the apparent layer
• TLC of organo-tin thioacids and thiols using thickness. The microscope also allows the thickness
Kielselgel G plates with development with of each layer to be determined.
glacial acetic acid and detection with catechol
violet (a.15). It is also possible to use an ATR technique to record
infrared spectra of the outside layers and reserve the
• TLC of organo-tins using Kieselgel GF 254 with IR microscope for the central layers. This is possible
development using butanol/glacial acetic acid because the ATR technique only penetrates a few
and detection with catechol violet and UV microns into the surface of the layers. It is also possible
irradiation (a.16). by choosing the appropriate crystal (e.g., germanium,
32
Analysis of Plastics
33
Analysis of Plastics
34
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) formulation of the product initially, which is a
technological failing, the other is where the formulation
In this technique the sample surface is bombarded by a is correct for the application, but where there has been
primary ion beam (positive ions of argon, caesium, a problem in the mixing/processing side, leading to a
oxygen or gallium). These primary ions impart energy product that does not meet the specification. Analysing
to the surface and, as a consequence of the collisions the plastic component can be useful in failure diagnosis.
produced, ions, atoms and molecular fragments (called
sputtered particles) are ejected. The primary ions may
penetrate several atom layers into the surface, but the 12.1 Common Compositional Problems
sputtered particles only come from the outer 2-3 atom
layers. In common with the other two techniques, If it is suspected that the composition of the product is
therefore, SIMS is very surface specific and it is possible not correct, for example that the antioxidant or correct
to restrict it to a single monolayer. The analysis area is cure system has not been incorporated into the
typically 150 μm, the detection limit is 1 ppm and all compound, then the appropriate species specific tests
the elements are detectable. that have been discussed earlier can be carried out. If
possible, it is advisable to conduct the analysis
Two types of SIMS experiment can be carried out: static
alongside that of a sample known to be of the correct
SIMS and dynamic SIMS. In the former case, the surface
composition. This ensures that no product specific
is bombarded with low energy ions and molecular and
matrix effects/interference reactions affect the data
atomic fragments are produced without the experiment
obtained and hence the conclusions reached.
changing the nature of the surface appreciably; the
surface chemistry can therefore be investigated.
A surprisingly large number of failure problems can be
Dynamic SIMS uses high energy ions to obtain highly
solved by carrying out a simple series of tests including a
sensitive elemental data down to ppb levels, but the
polymer identification check by IR, a bulk compositional
structural information is lost.
analysis by TGA and a molecular weight determination.
In the case of static SIMS, dedicated libraries are required
to enable the mass spectra of the fragments to be Molecular weight determination is very important in the
identified (a.22). case of plastics because of the wide use (sometimes
unauthorised) of regrind material. Unfortunately, the
Another application of SIMS is in the study of the quality of regrind plastic can vary greatly due to the
migration of additives (e.g., slip additives and antistats) degradation, and hence reduction in molecular weight
onto the surface of plastics. and associated physical properties, that a plastic
undergoes when it is reground. This depends greatly on
It is often the case that complementary surface analysis the conditions (e.g., heat and time of heating) that it is
techniques such as SIMS and XPS can be used together subjected to during the regrinding process. Also, if a
in order to successfully solve a failure or characterisation material already contains a proportion of reground
problem. In such cases, XPS would be used to generate material the onset of degradation can be accelerated by
quantitative information, whilst SIMS would provide structural anomalies already present in the polymer. The
qualitative clues with respect to the chemistry. An widespread applicability of GPC to determine the
example of this is where XPS has successfully detected molecular weight distribution of the majority of common
and quantified silicon on a surface which is not plastics makes it the perfect technique to investigate if
responding well to bonding with an adhesive, but the regrind is in a sample. Although small amounts (e.g.,
chemical form that the silicon is in is not readily apparent, 5%) of reasonably high quality regrind can be hard to
i.e., it could be silica, silicate or silicone. Analysis of the spot, any significant amount will reveal itself by a shift
same surface by static SIMS enables the mass spectrum in the distribution towards the low molecular weight end.
of the sputtered top layer fragments to be determined As usual with GPC, the availability of reference samples
and the presence of m/e ions at 43, 73 and 147 confirm is important as the technique is mainly comparative.
that a polydimethyl siloxane is present.
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
12 Failure Diagnosis reasonably common type of failure is odour, especially
in packaging applications. This odour is invariably due
It is an unfortunate fact that plastic products fail in to oxygenated degradation products of the plastic and
service. One of the major reasons for this is an incorrect can be detected and analysed by headspace GC-MS.
36
Analysis of Plastics
Contamination can enter the product stream either in There are a number of specific tests that automotive
the ingredients used in the production, or during the companies insist that plastics components manufactured
37
Analysis of Plastics
38
Analysis of Plastics
39
Analysis of Plastics
40
Analysis of Plastics
Appendix 1
Solubility Parameters of Plastics, Plasticisers and Typical Solvents
41
Analysis of Plastics
42
Analysis of Plastics
Appendix 2
Specific Gravities of Plastics and Compound Ingredients
43
Analysis of Plastics
44
Analysis of Plastics
45
Analysis of Plastics
46
References and Abstracts
DEGREE OF CURE, HEAT OF REACTION AND was measured from equilibrium melting point depression
VISCOSITY OF 8552 AND 977-3 HM EPOXY data. 50 refs.
RESINS INDIA
Ng S J; Boswell R; Claus S J; Arnold F; Vizzini A Accession no.850061
US,Naval Air Warfare Center; Maryland,University
The heat of cure, degree of cure and viscosity of two epoxy Item 13
resins (Hexcel 8552 and Cytec Fiberite 977-3 HM) were Chichester, John Wiley & Sons, 1999, pp.xiv,409.
investigated using a modulated differential scanning 23cm. 911
calorimeter and a rheometric digital analyser. MICROSTRUCTURAL CHARACTERISATION
Mathematical models were developed to correlate the rate OF MATERIALS
of the degree of cure and the viscosity with the degree of Brandon D; Kaplan W D
cure and used to predict the kinetic behaviour of the epoxy Haifa,Technion Institute
resins, which was then compared with that of Hercules This unreferenced book describes the technical and
3501-6. A comparison was also made of cure models theoretical aspects of a wide range of techniques for studying
developed based on neat and prepreg forms of the the microstructure of materials, including X-ray and electron
viscosity data. 6 refs. diffraction; optical microscopy, including polarised optical
USA microscopy and interference microscopy; transmission and
scanning electron microscopy; X-ray microanalysis; electron
Accession no.850900
energy loss spectroscopy; and surface analysis by
photoelectron spectroscopy, Auger electron spectroscopy,
Item 11 and secondary ion mass spectrometry. The techniques are
Polymers & Polymer Composites described from sample preparation through information
10, No.3, 2002, p.237-48 acquisition to interpretation of results. A final chapter
CURE BEHAVIOUR AND STRUCTURE OF describes the derivation of quantitative structural data from
DICYANATE-EPOXY NOVOLAC BLENDS the results of these techniques. Examples used in the
Guo B; Fu W; Jia D; Qiu Q; Wang L book mainly involve highly ordered materials such as
South China,University of Technology metals and inorganic crystalline materials, but many of
the techniques used are applicable to polymers. Problems
The objectives of this work are to investigate the cure
for the reader are included.
behaviour and structure of bisphenol A dicyanate-novolac
ISRAEL
epoxy blends. The cure characteristics were investigated
by gel time determination and dynamic DSC. To disclose Accession no.849739
the structural differences between cured cyanate-novolac
epoxy blends and more traditional cyanate-diglycidyl Item 14
ether systems, FTIR investigations were performed on Polimeros: Ciencia e Tecnologia
the two kinds of blends, and in situ FTIR was used to 11, No.4, Oct./Dec.2001, p.213-21
examine the Bauer mechanism. The effects of epoxy Portuguese
concentration in the blend on the cure kinetics was NEAR-INFRARED SPECTRA OF
investigated using two blends with different molar ratios, POLYSTYRENE, POLY(METHYL
and in situ FTIR. 33 refs. METHACRYLATE) AND POLYCARBONATE
CHINA
De Araujo S C; Kawano Y
Sao Paulo,Instituto de Quimica
Accession no.850546
The near-infrared (NIR) spectra of amorphous polymers
PS, PMMA and polycarbonate (PC) are studied. The
Item 12
tentative assignment of the overtone and combination
Macromolecular Chemistry & Physics
frequencies is made using the curve fitting calculations and
203, No.4, 15th March 2002, p.653-62
the local mode theory. Anharmonicity correction and
MISCIBILITY AND CRYSTALLIZATION
mechanical frequency are determined from a Birge-Sponer
BEHAVIOUR OF POLYETHYLENE
plot. A tentative assignment of stretch overtone frequency
TEREPHTHALATE/POLYVINYLIDENE
of CH2 and CH functional groups of PS; CH3 and CO
FLUORIDE BLENDS
functional groups of PMMA; and CH, CH3 and CO
Rahman M H; Nandi A K
functional groups of PC is made. An anharmonicity
Indian Association for the Cultivation of Science
correction of 57 and 58 cm-1 is obtained for CH2 and CH
The miscibility of PETP and PVDF was studied. The Tg, stretch modes of PS; 59 and 9 cm-1 for CH3 and CO stretch
melting point, the crystallisation temperature and the modes of PMMA; and 53, 59 and 10 cm-1 for CH, CH3
crystallinity values of the blends of different and CO stretch modes of PC, respectively. 21 refs.
compositions, prepared at different conditions were BRAZIL
measured. The polymer-polymer interaction parameter Accession no.849333
Item 15 Item 17
Macromolecules Injection Molding
35, No.7, 26th March 2002, p.2667-75 10, No.1, Jan. 2002, p.40-4
THERMAL PROPERTIES OF CROSS-LINKED THE MATERIALS ANALYST: PART 50. THE
POLYISOPROPYLACRYLAMIDE, CASE OF THE DISAPPEARING CONTAMINANT
POLYMETHACRYLIC ACID, THEIR RANDOM Sepe M
COPOLYMERS, AND SEQUENTIAL Dickten & Masch Mfg.
INTERPENETRATING POLYMER NETWORKS A report is presented on the diagnosis of the failure of a
Diez-Pena E; Quijada-Garrido I; Frutos P; Barrales- component made from a 33% glass-reinforced nylon 66
Rienda J M on the assembly line with the aid of DSC, thermal
CSIC gravimetric analysis, which was utilised to determine filler
The thermal properties of polyisopropyl acrylamide, content and type, X-ray fluorescence and IR spectroscopy.
polymethacrylic acid, isopropyl acrylamide-methacrylic The analytical procedures employed indicated that failure
acid copolymers and their blends were investigated by of the component could be attributed to the presence of
DSC and TGA. The state of the water was studied on the chlorine probably arising from contamination of the
basis of DSC traces of swollen samples. The Tg of the process by PVC.
same series of materials was also measured. 64 refs. USA
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; Accession no.848744
WESTERN EUROPE
Accession no.849122 Item 18
Journal of Polymer Science: Polymer Physics Edition
Item 16 40, No.5, 1st March 2002, p.434-53
Applied Spectroscopy FREE VOLUME, GLASS TRANSITION, AND
56, No.2, Feb.2002, p.187-91 DEGREE OF BRANCHING IN METALLOCENE-
RAMAN MICROSCOPY AND MAPPING AS A BASED PROPYLENE/ALPHA-OLEFIN
PROBE FOR PHOTODEGRADATION IN COPOLYMERS: POSITRON LIFETIME,
SURFACE RELIEF GRATINGS RECORDED ON DENSITY, AND DIFFERENTIAL SCANNING
LAYER-BY-LAYER FILMS OF CONGO RED/ CALORIMETRIC STUDIES
POLYELECTROLYTE Dlubek G; Bamford D; Rodriguez-Gonzalez A;
Constantino C J L; Aroco R F; He J A; Zucolotto Z; Li Bornemann S; Stejny J; Schade B; Alam M A; Arnold M
L; Olveira O N; Kumar J; Tripathy S K Bristol,University; ITA Institut fuer Innovative
Windsor,University; Lowell,Massachusetts University Technologien GmbH; Martin-Luther-Universitat Halle
Raman microscopy, mapping and surface-enhanced Results of the above studies are presented and are
Raman scattering techniques are applied to investigate discussed with particular reference to Tg and degree of
the degradation of Congo Red (CR) in a surface relief branching, local free volume and degree of branching,
grating (SRG) recorded on electrostatically assembled local free volume and Tg, specific volume and degree of
layer-by-layer film of CR alternated with polydimethyl branching, and number density of holes and degree of
diallylammonium chloride (PDAC). Photoinduced branching. 56 refs.
degradation is suggested by a decrease in the Raman bands EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
UK; WESTERN EUROPE
assigned to CR with a concomitant increase in the
background signal. More degradation is observed in the Accession no.848572
valleys of the SRG, which correspond to the most
illuminated areas. In a line mapping across the SRG, the Item 19
Raman intensity of CR bands follows the modulation of Polymer Preprints. Volume 42. Number 2. Fall 2001.
the grating, which indicates that photodegradation of CR Proceedings of a conference held Chicago, Il., 7th-11th
contributes at least partially to the SRG formation. April 2002.
Surface-enhanced resonance Raman scattering (SERRS) Washington, D.C., ACS,Div.of Polymer Chemistry,
indicates that the phenyl ring groups are located at the 2001, p.13-4
film surface. Mapping of the Raman signal over many POSITRON ANNIHILATION SPECTROSCOPY
periods of SRG shows that, within the limits of detection, AS A NOVEL SURFACE PROBE OF POLYMERS
the chromophores appear to be oriented in much the same Jean Y C; Zhang R; Mallon P; Chen H; Huang C-M; Li
way throughout the film. They have no preferred Y; Zhang J; Huang Y Y; Sandreczki T C; Wu Y
orientation in the peaks and valleys of the SRG after the Missouri-Kansas City,University
recording process is completed. 23 refs. (ACS,Div.of Polymer Chemistry)
CANADA; USA Positron annihilation spectroscopy (PAS) is a special non-
Accession no.848921 destructive evaluation (NDE) technique for materials
thermogravimetric analysis techniques. It was concluded state-of-the-art FTIR spectroscopy can be used. From the
that the thermal degradation results varied with both chromatographic and spectroscopic data, contour
atmosphere and test technique with the high resolution diagrams are generated that present the molecular
technique providing more precise data in the inert heterogeneity of the sample in the coordinates molar mass
atmosphere tests but less resolution in air. and chemical composition. 17 refs.
Thermogravimetric analysis data for a number of EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
polyimide polymers is tabulated. The thermoplastic WESTERN EUROPE
polyimide polymer evaluated was more thermally stable Accession no.846265
than many other polyimides. Complete details of the test
techniques are given with full discussion of the results.
Item 26
40 refs.
Polymer
CHINA
43,No.6,2002,p.1835-47
Accession no.846773 THERMAL DEGRADATION OF PET AND
ANALOGOUS POLYESTERS MEASURED BY
Item 24 THERMAL ANALYSIS-FOURIER TRANSFORM
Journal of Applied Polymer Science INFRARED SPECTROSCOPY
83, No.12, 2002, p.2522-7 Holland B J; Hay J N
CRYSTALLIZATION AND CROSSLINKING OF Birmingham,University
POLYAMIDE-1010 UNDER ELEVATED
The thermal degradation of two commercial PET samples
PRESSURE
and two laboratory prepared polyesters, poly(ethylene
Jun Yang; Wenfei Dong; Yucheng Luan; Jingjiang Liu;
isophthalate) and poly(diethylene glycol terephthalate),
Shue Liu; Xingguan Guo; Xudong Zhao; Wenhui Su
was studied using thermogravimetry and thermal analysis-
Changchun,Institute of Applied Chemistry;
FTIR. The commercial PET samples were copolymerised
Jilin,University
with diethylene glycol and isophthalic acid groups in
This study looked at the structural changes to polyamide- different proportions, and their thermal stabilities were
1010 (PA1010) when it was treated at 250 degC for 30 found to differ. Through a study of the thermal degradation
min at a pressure of 0.7-2.5 GPa. Crystals grew when the of poly(diethylene glycol terephthalate) and poly(ethylene
pressure was below 1.0 GPa or above 1.2 GPa. isophthalate), it was found that diethylene glycol and
Crosslinking occurred in the pressure range 1.0-1.2 GPa. isophthalate units promoted thermal degradation through
DSC and wide angle x-ray diffraction showed that PA1010 increased chain flexibility and more favourable bond
lost its crystallisation ability after treatment at pressures angles, respectively. The thermal degradation of all the
of 1.0-1.2 GPa. Crystallised PA1010 had a greater thermal polyesters tested led to the formation of non-volatile
stability than crosslinked PA1010 at 400 degC. 20 refs. residue. IR spectroscopic analysis indicated that the
CHINA residue consisted almost exclusively of interconnected
Accession no.846587 aromatic rings. 21 refs.
EU; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE; WESTERN EUROPE-GENERAL
Item 25
Kautchuk und Gummi Kunststoffe Accession no.846155
55, No.1-2, 2002, p.9-14
German Item 27
ANALYSIS OF TECHNICAL POLYMER BLENDS Progress in Organic Coatings
WITH COUPLING OF LIQUID 43, No.4, Dec.2001, p.226-32
CHROMATOGRAPHY WITH FTIR SIMPLE RAMAN TECHNIQUE TO MEASURE
SPECTROSCOPY THE DEGREE OF CURE IN UV CURABLE
Pasch H; Rode K; Kloninger C; Esser E COATINGS
Deutsches Kunststoff-Institut Nichols M E; Seubert C M; Weber W H; Gerlock J L
Ford Research Laboratory
The coupling of liquid chromatography with FTIR
spectroscopy provides a new and interesting method for The curing of four UV-curable clearcoats was studied by
the detailed analysis of complex polymer systems. The confocal Raman microscopy. The disappearance of the
application of this hyphenated technique to the analysis C:C line near 1636/cm provided the signature for the
of polymer blends shows that it is possible to identify the curing of the samples, but quantification of the degree of
different blend components by their spectral cure by standard peak fitting and baseline subtraction
characteristics. Components of different chemical methods did not work well because of sample
compositions are determined selectively and their fluorescence, baseline shifts and overlapping peaks. A
chemical structure is analysed through well-resolved smoothed second-derivative processing approach
FTIR spectra. For structure elucidation, all facilities of overcame all of these difficulties and provided a simple,
rapid and objective quantification procedure. Steep cure average molec.wts. of the samples, as received and
gradients through the thickness of the clearcoat, due to purified, were determined by VPO in two different
screening of the bottom of the clearcoat by both the UVA solvents, trichloromethane and THF. Viscometric average
and photoinitiator, were observed. Cure gradients at the molec.wts. were obtained in trichloromethane at 25C. Five
top of the clearcoat due to oxygen inhibition were also different equations were used to calculate intrinsic
observed. The most complete cure throughout the film viscosities and viscometric constant values. Relative
thickness was obtained with a mixture of standard and molec.wts. and polydispersities were determined by SEC,
red-shifted photoinitiators. 9 refs. in THF at 35C and in trichlorobenzene at 135C. It was
USA confirmed that the results obtained in the latter solvent
Accession no.846135 were in better agreement with those obtained by the other
techniques. 25 refs.
Item 28 BRAZIL
Polymer Accession no.845967
43, No.5, 2002, p.1587-97
FULL COPOLYMER CHARACTERIZATION BY Item 30
SEC-NMR COMBINED WITH SEC-MALDI Plastics Engineering
Montaudo M S 58, No.2, Feb. 2002, p.40/55
CNR PLASTICS ANALYSIS - THE ENGINEERS
Random copolymers with units of methyl methacrylate, RESOURCE FOR TROUBLESHOOTING
butyl acrylate, styrene and maleic anhydride were studied PRODUCT AND PROCESS PROBLEMS AND
by fractionating the copolymer by size exclusion FOR COMPETITIVE ANALYSIS
chromatography(SEC), collecting 30 to 40 fractions and Ezrin M
then recording both the NMR and MALDI spectra of the Connecticut,University
fractions. In a successive step, bivariate distribution of Methods for competitive analysis, troubleshooting process
chain sizes and composition maps were derived from and product problems, plastics analysis, analysis of failed
knowledge of the molar mass, weight and composition products and analysis of polymeric formulations are
of the copolymer fractions. The compositional distribution discussed. Procedures covered include FTIR spectroscopy,
was obtained by summation of the sections of the bivariate Raman spectroscopy, NMR spectroscopy, surface analysis
distribution which belonged to a narrow compositional by spectroscopy, gas chromatography/mass spectrometry,
range. A model for SEC fractionation of copolymers was atomic force microscopy and techniques for analysing
developed which allowed prediction of the composition unidentified formulations. 47 refs.
and D(x) of the SEC fraction, D(x) being the ratio between
USA
the number-average and the weight-average molar mass,
with x being the fraction number. Off-line SEC-MALDI Accession no.845139
measurements were performed in order to measure D(x)
experimentally for the random copolymers. 31 refs. Item 31
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; Journal of Applied Medical Polymers
WESTERN EUROPE 5, No.2, Autumn 2001, p.77-9
Accession no.846119 NOVEL TECHNIQUE FOR THE DETECTION OF
A HINDERED AMINE LIGHT STABILIZER,
Item 29 BASED ON SILICON TECHNOLOGY
Polymer Testing Narayan S; Lee R E; Hallberg D; Malatesta V
21, No.2, 2002, p.155-61 Great Lakes Chemical Corp.; Great Lakes Chemical
BISPHENOL A-BASED POLYCARBONATES: Italia
CHARACTERIZATION OF COMMERCIAL Details are given of the development of a novel method
SAMPLES to detect the presence of a hindered amine light stabiliser
Delpech M C; Coutinho F M B; Habibe M E S in PP, based on silicon technology. The method consisted
Rio de Janeiro,Universidade Federal; Rio de of extracting the stabiliser from the PP matrix followed
Janeiro,Universidade Estadual; Polialden Petroquimica SA by detection and quantification using proton NMR. 3 refs.
Samples of bisphenol A polycarbonate were characterised EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; USA;
by DSC, TGA, FTIR spectroscopy, size exclusion WESTERN EUROPE
chromatography(SEC), vapour pressure osmometry Accession no.844622
(VPO) and viscometry. The samples exhibited the same
FTIR spectrum profile and almost the same values of Tg Item 32
and initial temp. of degradation. Slight differences were, Adhasion Kleben & Dichten
however, observed in differential TGA curves, which 45, No.12, 2001, p.34-8
could be due to the presence of additives. The number- German
Item 36 Item 38
Revista de Plasticos Modernos Synthetic Metals
81, No.538, April 2001, p.461-6 124, No.2-3, 22nd Oct.2001, p.407-14
Spanish STUDY OF THE SURFACE POTENTIAL AND
APPLICATION OF INFRARED SPECTROSCOPY PHOTOVOLTAGE OF CONDUCTING
AND THERMAL ANALYSIS IN MONITORING POLYMERS USING ELECTRIC FORCE
THE CURE OF THERMOSETTING RESINS MICROSCOPY
USED IN THE AIRCRAFT INDUSTRY Barisci J N; Stella R; Spinks G M; Wallace G G
Sanchez-Blazquez A Wollongong,University
CASA The effect of the polymer composition, preparation
The amine cure of Hexcel 8552 epoxy resin, for use as method and nature of the substrate on the surface potential
the matrix in carbon fibre-reinforced composites for (SP) of conducting polymer films is investigated. Both
application in aircraft construction, was monitored by the average value and the distribution of SP across the
near-infrared spectroscopy. This technique was validated polymer surface are influenced by these factors.
by comparison of the results with those obtained by Polythiophenes, potentially useful for solar energy
modulated DSC. 18 refs. conversion, are used to examine the generation of light-
induced changes in SP. Results suggest the possibility of
HEXCEL COMPOSITES determining the local variations of the surface
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
WESTERN EUROPE photovoltage and the photovoltaic properties of polymer
films intended for use in photovoltaic devices. 16 refs.
Accession no.842573
AUSTRALIA
Accession no.842093
Item 37
Progress in Colloid & Polymer Science
Vol.117, 2001, p.167-71 Item 39
SURFACE CHARACTERISATION OF Polymer Degradation and Stability
POLYLACTIDE/POLYGLYCOLIDE 75, No.1, 2002, p.185-91
COPOLYMERS STUDY ON METHANOLYTIC
Kiss E; Lam C N C; Due T M; Vargha-Butler E I DEPOLYMERIZATION OF PET WITH
Budapest,Eotvos Lorand University; SUPERCRITICAL METHANOL FOR
Toronto,University; Biophy Research CHEMICAL RECYCLING
Yong Yang; Yijun Lu; Hongwei Xiang; Yuanyuan Xu;
The wettability and the surface composition of Yongwang Li
biodegradable polymers used as drug delivery particles Chinese Academy of Sciences
are determined and compared. Films of polylactic acid,
polyglycolic acid and their copolymers with four different Polyethylene terephthalate (PET) was subjected to
lactide, glycolide ratios of 85/15, 75/25, 65/35 and 50; methanolytic depolymerisation with supercritical
50 are formed by solvent-casting on polar (silicone wafer methanol in a stirred stainless steel autoclave at
glass and silica) substrates. Advancing and receding water temperatures of 523-543 deg.C, pressure 8.5-14.0 MPa,
contact angles are measured goniometrically and also by and a 3-8 methanol to PET weight ratio. The solid products
using the automated axisymmetric drop shape analysis obtained, consisting mainly of dimethyl terephthalate and
method. Both the advancing and the receding water small amounts of methyl-(2-hydroxyethyl) terephthalate,
contact angles of the copolymers are higher than expected bis(hydroxyethyl) terephthalate, dimers, and oligomers,
from the values obtained for the two homopolymers were analysed by high performance liquid
considering the increasing glycolide content of the chromatography (HPLC), and the liquid products, mainly
copolymers. Surface analysis of the polyester films is ethylene glycol and methanol were analysed by gas
performed by X-ray photoelectron spectroscopy at various chromatography (GC). The temperature, weight ratio of
take-off angles to get information on the depth distribution methanol to PET, and the reaction time had a very marked
of the components. Surface enrichment of the nonpolar effect on dimethyl terephthalate yield and the degree of
(lactide) component in the outermost layer of the PET depolymerisation, but the effect of pressure was
copolymer films is detected. The wettability behaviour is insignificant above the methanol critical point. The
in accordance with the surface composition, results optimum PET depolymerisation conditions were:
suggesting a surface activity effect resulting in the temperature 533-543 K, pressure 9.0-11.0 MPa, and a
orientation of the nonpolar segments of the copolymer methanol to PET weight ratio of 6-8. The
chains towards the surface of the film and hence producing depolymerisation of several PET wastes from the Chinese
more hydrophobic character for the copolymer films than market was studied under the optimum conditions. 28 refs.
should be due to their bulk composition. 20 refs. CHINA
Accession no.842190 Accession no.841527
PHENYLENECARBONYL-1,4- Item 56
PHENYLENE)(PEEK) Revista de Plasticos Modernos
Kampert W G; Sauer B B 81, No.536, Feb.2001, p.244-8
DuPont Central Research & Development Spanish
PERMEABILITY OF METHANOL, TOLUENE,
The thermal and crystal morphological properties of
FUELS AND OXYGENATED FUELS IN AN
amorphous and melt-crystallised PEEK were investigated.
ETHYLENE-VINYL ALCOHOL COPOLYMER
Two different molec.wts. were studied by temp.-
USED AS A BARRIER COMPONENT TO GASES,
modulated DSC(TMDSC) over a broad range of annealing
AROMAS AND HYDROCARBONS
times and temps. The lower molec.wt. PEEK under all
Lagaron J M; Powell A K
crystallisation conditions was found to exhibit secondary
Jaume I,Universitat; BP Chemicals Ltd.
crystal melting in the low endotherm region, followed by
melting of primary crystals superimposed with a large Measurements were made of the permeation rates of
recrystallisation contribution. Primary crystal melting methanol, toluene, a 50/50 toluene/isooctane fuel (fuel
broadly overlapped with melting of the recrystallised C) and fuel C with 10% ethanol or 15% methanol through
species and contributed to the broad highest endotherm. EVOH films. Large scale methanol and water induced
Recrystallisation contributions and the interpretation of plasticisation was suggested by large solvent uptakes and
TMDSC were partially confirmed by independent rapid confirmed by the observation of considerable decreases
heating rate m.p. determinations and variable heating rate in Tg. The permeability of fuel C increased significantly
DSC. The higher molec.wt. PEEK showed many when methanol was present, while the high barrier
similarities but generally had smaller levels of properties of EVOH to hydrocarbons was maintained for
reorganisation above the annealing temp. under most fuel C containing ethanol. 9 refs.
higher temp. crystallisation conditions. TMDSC provided EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;
good resolution of recrystallisation and related events WESTERN EUROPE
compared with standard DSC. The broad and substantial Accession no.835449
exothermic recrystallisation in amorphous samples was
also examined, showing that recrystallisation continued
Item 57
through the final melting region. 42 refs.
Revista de Plasticos Modernos
USA
81, No.536, Feb.2001, p.236-43
Accession no.836355 Spanish
ETHYLENE-VINYL ALCOHOL COPOLYMERS
Item 55 AND THEIR APPLICATIONS IN FOOD
Macromolecular Symposia PACKAGING
Vol.174, Aug.2001, p.413-34 Cerrada M L
STRATEGIES IN TWO-DIMENSIONAL LIQUID Instituto de Ciencia y Tecnologia de Polimeros
CHROMATOGRAPHIC SEPARATION OF The gas barrier properties of ethylene-vinyl alcohol
COMPLEX POLYMER SYSTEMS copolymers are examined as a function of ethylene and
Berek D vinyl alcohol content, and their use in combination with
Slovak,Academy of Sciences other plastics in films, bottles and other containers for
The separation of complex polymer systems by two- food packaging is discussed. Results are presented of a
dimensional liquid chromatography is discussed. Methods study of the crystal structure of three copolymers having
are reviewed in which the effect of polymer molec.wt. on different compositions. 11 refs.
polymer retention is suppressed. The resulting ‘one EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
WESTERN EUROPE
parameter separation systems’ can be on-line or off-line
connected to another separation system such as size Accession no.835448
exclusion chromatography in order to provide more detailed
characterisation of complex polymers. Selected procedures Item 58
for the re-concentration of diluted polymer solutions are Polymer Preprints. Volume 41. Number 2. Conference
also considered. These could be used for increasing the proceedings.
concentration of sample(s) leaving the first dimension Washington, D.C., 20th-24th Aug.2000, p.1423-4
separation column. Some arrangements for controlled MAPPING CHEMICALLY HETEROGENEOUS
sample re-introduction into the second dimension POLYMER SYSTEM USING CHEMICAL
separation column are outlined. 48 refs. (World Polymer MODIFICATION AND ATOMIC FORCE
Congress, IUPAC MACRO 2000, 38th Macromolecular MICROSCOPY
IUPAC Symposium, Warsaw, Poland, July 2000) Raghavan D; Gu X; VanLandingham M; Nguyen T
SLOVAK REPUBLIC; SLOVAKIA Washington,Howard University; US,National Inst.of
Accession no.836231 Standards & Technology
for periods of time between 30 and 90 seconds on the drinks industry, were studied with and without a
surface of low density polyethylene films were examined compatibiliser. The compatibilising agent was a surlyn
by attenuated total reflectance fourier transform infrared copolymer of ethylene and methacrylic acid partially
spectroscopy, electron spectroscopy for chemical analysis neutralized with zinc, the olefinic segment of which is
(ESCA), scanning electron microscopy and water contact compatible with HDPE, whereas the carboxylic acid
angle. The effect of chromic acid treatment on the tensile groups form hydrogen bonds with the PET carbonyl
strength of the samples was evaluated and tensile strength groups. Infrared spectroscopy, differential scanning
reduced with increasing treatment time. Adhesion of calorimetry, scanning electron microscopy, and the
copper film to the treated surface was evaluated by a mechanical properties were used to assess the
scratch test. It was found that both surface roughness and effectiveness of the compatibiliser. 29 refs.
number of polar groups on the surface increased with MEXICO
increasing treatment times of both chromic acid and Accession no.832040
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 Item 64
initially increased with increasing treatment times, but Polymer Degradation and Stability
optimum adhesion properties consistent with tensile 73, No.3, 2001, p.467-70
strength retention were established with 30 minutes CORRELATION BETWEEN THERMAL
chromic acid treatment followed by 30 seconds oxygen PROPERTIES AND CONFORMATIONAL
plasma treatment. 14 refs. CHANGES IN POLY(ETHYLENE
TEREPHTHALATE)/POLY(ETHER IMIDE)
KOREA
BLENDS
Accession no.834851 Ruvolo-Filho A; de Fatima Barros A
Sao Carlos,Universidade Federal
Item 62
Virgin and recycled polyethylene terephthalate (PET) was
Advanced Materials & Processes
blended with polyether-imide (PEI) in proportions
159, No.10, Oct.2001, p.66-7
between 0 and 50 percent PEI content and samples were
SURFACE ENGINEERING TECHNOLOGIES
examined by differential scanning calorimetry and Fourier
Sudarshan T S
transform infrared spectroscopy. All blends were
Materials Modification Inc.
completely miscible, as indicated by a single glass
The 15th International Conference on Surface transition temperature which is dependent on blend
Modification Technologies will be held in November in composition. Crystallisation rates of PET were retarded
Indianapolis. This article presents a few paper abstracts strongly at 20 percent PEI content and above, but degree
and lists the titles of the sessions. Papers include: structure of crystallinity was easily determined from a linear
and properties of HVOF sprayed amorphous polymer correlation between a structural parameter measured
matrix nanocomposite coatings; field experience with spectroscopically and enthalpy of fusion. Trans conformer
advanced soft-metal surfaces on carbon steel bolting activation energy measurement confirmed the effects of
materials used in gall-prone gasketed joints that operate PEI content on crystallisation of PET. 9 refs.
at elevated temperatures; characterisation of industrial BRAZIL
coatings with atomic force microscopy; characterising Accession no.831829
aluminium pretreatments for structural adhesive bonding;
the Air Force manufacturing technology laser peening
initiative; and iron aluminide based coating deposited by Item 65
high energy density processes. Polymer Degradation and Stability
USA
73, No.3, 2001, p.463-6
EFFECT OF INTERFACE MODIFICATION ON
Accession no.834668
THE PHOTO-STABILITY OF PIGMENTED
POLYETHYLENE FILMS
Item 63 Anna P; Bertalan G; Marosi G; Ravadits I; Maatoug M
Journal of Applied Polymer Science A
82, No.6, 7th Nov.2001, p.1382-90 Budapest,University of Technology & Economics
PROPERTIES AND MORPHOLOGY OF
Examination of the ageing characteristics of high density
POLY(ETHYLENE TEREPHTHALATE) AND
polyethylene films containing phthalocyanine green and
HIGH-DENSITY POLYETHYLENE BLEND
titanium white and other pigments with those of lightly
Guerrero C; Lozano T; Gonzalez V; Arroyo E
stabilised polymer film without pigments was carried out
Nuevo Leon,Universidad Autonoma
using tensile analysis, differential scanning calorimetry
Blends of polyethylene terephthalate (PET) and high and ultraviolet spectroscopy. The early failure of the
density polyethylene (HDPE), widely used in the soft phthalocyanine pigmented sample, and subsequent UV
spectroscopic examination showed that the cause was HIGH RESOLUTION SOLID-STATE CARBON 13
adsorption of stabilisers onto the pigment surface. NMR STUDY OF AS-CURED AND IRRADIATED
Reactive surfactant coating of pigments was shown to EPOXY RESINS
considerably extend the film stability by reducing their Ngono-Ravache Y; Foray M-F; Bardet M
adsorbency. 9 refs. Grenoble,University
EASTERN EUROPE; HUNGARY
Details are given of the effects of strong ionising
Accession no.831828 radiations on the physico-chemical modifications of
epoxy resins. The sensitivity of the epoxy resins to
Item 66 radiation was determined using carbon 13 NMR. 20 refs.
Polymer Degradation and Stability EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
73, No.3, 2001, p.387-92 WESTERN EUROPE
MECHANISM OF PHOTOSTABILIZATION OF Accession no.831124
PERFLUOROPOLYETHER COATINGS BY
HINDERED AMINE STABILISERS Item 69
Luda M P; Camino G; Laurenti E; Novelli S; Applied Spectroscopy
Temtchenko T; Turri S 55, No.8, Aug. 2001, p.984-91
Torino,Universita; Centro Ricerche Ausimont RAMAN AND INFRARED
The mechanism of operation of hindered amine stabilisers MICROSPECTROSCOPIC MAPPING OF
(HAS) against photodegradation in perfluoro polyethers PLASMA-TREATED AND GRAFTED POLYMER
incorporated into a coating material of polyurethane has SURFACES
been studied by infrared spectroscopy, gas Keen I; Rintoul L; Fredericks P M
chromatography-mass spectrometry and electron spin Queensland,University of Technology
resonance spectroscopy. Under curing conditions A section of the surface of a predominantly PP substrate
normally utilised for coil coating (280 degrees Centigrade containing a small amount of PE copolymer and a small
for 1 minute in air), the HAS was found to increase the amount of blended EPM was characterised before and
number of urea bridges in the polyurethane network, and after plasma treatment and after graft copolymerisation
reduce the amount of unreacted isocyanate, giving a with PS by means of Raman and ATR/IR mapping. The
structure which is more resistant to photooxidation. maps constructed indicated variations in crystallinity
Byproducts of the high temperature cure process, caused across the surface, the distribution of EPM and the
by partial transformation of the HAS into -NH derivatives distribution of hydroxy groups introduced onto the surface
act as antioxidants. The unreacted HAS was found to by plasma treatment. 24 refs.
slowly evaporate from the test film, but whilst present AUSTRALIA
acted as a radical scavenger. 8 refs.
Accession no.830453
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
WESTERN EUROPE
Accession no.831816 Item 70
POLYMER PROCESSING ENGINEERING. 01.
Proceedings of a conference held June 2001.
Item 67
London, IOM Communications Ltd., 2001, Paper 5,
Plast’ 21
p.46-58, 012
No.101, April 2001, p.77-9
AT-PROCESS RAMAN SPECTROMETRY OF
Spanish
POLYMER MELTS
INFRARED THERMOGRAPHY: THE COLOURS
Dhamdhere M; Li J; Deshpande B; Patil P; Hansen M G
OF HEAT
Tennessee,University
ASCAMM
(Institute of Materials; Interdisciplinary Research
The use of IR thermography in the study of injection Centre)
moulds and injection moulded plastics parts is discussed,
In-line monitoring of EVA extrusion was carried out using
and details are given of research and development projects
in-line fibre optic Raman spectroscopy. Vinyl acetate
being undertaken by ASCAMM of Spain using this
content in the random copolymer and melt indices of
technique.
various grades of the EVA were determined and vinyl
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
acetate content in the samples correlated using linear least
WESTERN EUROPE
squares and PLS analysis. Hierarchical Cluster analysis was
Accession no.831329 employed as a pattern recognition technique to follow the
natural clustering tendencies of the EVA samples. 10 refs.
Item 68 EUROPEAN COMMUNITY; EUROPEAN UNION; UK; USA;
Polymers for Advanced Technologies WESTERN EUROPE
12, No.9, Sept, 2001, p.515-23 Accession no.830358
LONG-TERM ENERGY EFFICIENCY OF PU- from different wood species was carried out. Studies were
INSULATION FOR REFRIGERATION carried out on Pine (Pino Eliottis), eucaliptus (Eucaliptus
Seifert H; Biedermann A Saligna) and marmelero (Ruprechia Laviflora), a
Elastogran GmbH softwood and two semi-hard woods, respectively. The
(Crain Communications Ltd.; European Isocyanate particles were used untreated and chemically modified
Producers’ Association) with maleic anhydride. For the characterisation of
untreated and treated flours, thermogravimetric analysis
The ageing behaviour of rigid PU foams was investigated
and analytical techniques were utilised. Dispersion of the
using gas chromatographic quantitative evaluation of the
fibrous particles, in addition to maximum fibre
cell gas composition in the foams. The change in thermal
concentration (accompanied by complete wetting of the
conductivity of the foams during ageing was also
wood fibres) was dependent on the treatment and on the
examined as was the dimensional stability of the foams
wood species utilised. Bending and compression tests
under diffusion open conditions and the results obtained
suggested some improvement in the performance of the
correlated with the K x A-values from refrigerator cabinets
composites, if the wood flour was previously esterified.
via the change in cell gas composition. The data obtained
Changes in the fracture surfaces due to maleic anhydride
revealed that the ageing process of appliances could be
treatment of the fibres were observed using scanning
simulated in a tenth of the time by measuring diffusion
electron microscopy. 12 refs.
opened PU foams. 2 refs.
ARGENTINA
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
NETHERLANDS; WESTERN EUROPE Accession no.824162
Accession no.824859
Item 83
Item 81 Polymer Degradation and Stability
International Polymer Science and Technology 73, No.2, 2001, p.251-7
28, No.5, 2001, p.T/79-80 THERMAL CHARACTERISTICS OF ADDITION-
STUDY OF POLYMER-FILLER INTERACTION CURED PHENOLIC RESINS
BY INVERSE GAS CHROMATOGRAPHY Reghunadhan C P; Bindu R L; Ninan K N
Gukasyan S Z Vikram Sarabhai Space Centre
The surface modification of fillers with polymeric The thermal cure characteristics, kinetics of thermal
substances is discussed with reference to improvement degradation and pyrolysis of four different addition cured
of the properties of filled polymers. When the fillers are phenolic resins were investigated using various
modified with polymers, the boundary layer contains not techniques, including DSC, DMA, FTIR spectroscopy,
only the matrix filler, but also the modifying polymer, TGA and X-ray diffraction. Resins investigated were
and when the modifying polymer interacts with the surface propargyl ether resins and phenyl azo-, phenyl ethynyl-
filler, the properties of both the mineral component and and maleimide-functional resins. A comparison of the data
the modifier are altered. One characteristic which reflects obtained for all the phenolic resins was made as a function
the result of polymer-filler interaction is the glass of molecular structure. 12 refs.
transition temperature of the modifier. To determine this INDIA
parameter for a very low content of polymer, the method Accession no.824043
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 Item 84
which were modified with latices of a copolymer of UTECH 2000. Proceedings of a conference held The
styrene and methacrylic acid. 3 refs. (Article translated Hague, Netherlands, 28th-30th March 2000.
from Plasticheskie Massy, No.8, 2000, p.36) London, 2000, Innovations: Flexible Foam
RUSSIA Developments Session, Paper 5, pp.4, 012
VOC DETECTION IN POLYURETHANE
Accession no.824324
FLEXIBLE FOAMS
Occhiello E; Tavan M; Pannocchia P; Fava F
Item 82
EniChem
Molecular Crystals & Liquid Crystals
(Crain Communications Ltd.; European Isocyanate
Vol.353, 2000, p.95-108
Producers’ Association)
COMPOSITES MADE FROM
LIGNOCELLULOSICS AND THERMOSET The detection of volatile organic compounds in polyols
POLYMERS and PU foams using SPME, gas chromatography and gas
Aramguren M I; Marcovich N E; Reboredo M M chromatography-mass spectroscopy is demonstrated.
INTEMA EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
NETHERLANDS; WESTERN EUROPE
Preparation and testing of composites from a styrene/
Accession no.823982
unsaturated polyester thermoset matrix and wood flours
mol.percent ethylene) used in barrier applications was polymers are analysed. The author’s own modification
studied at three temperatures immediately above the of PGC is presented, involving the use of a pyrolysis
melting point using thermogravimetric analysis, DSC and attachment with the mobile reaction zone. Resulting data
FTIR spectroscopy. The weight loss measured by are compared with those obtained by conventional
thermogravimetric analysis was fast at short times and pyrolysis gas chromatography. 34 refs.
slowed down progressively. The weight loss of about 3.6 Accession no.816530
percent measured by thermogravimetric analysis resulted
from chemical alterations in the polymer. DSC showed
small changes in crystallinity, melting point and glass Item 97
transition and broadening of the melting endotherms in New York, John Wiley & Sons, Inc., 1999, pp.xv,752
samples exposed to the more severe thermooxidative CHEMICAL SEPARATIONS- PRINCIPLES,
treatments. FTIR showed a transformation of the vinyl TECHNIQUES, AND EXPERIMENTS
alcohol hydroxyl groups into carbonyl groups and the MELOAN, C E
creation of double bonds. Changes in degradation kinetics, KANSAS STATE UNIVERSITY
and possibly mechanisms, were thought to occur with This combination laboratory manual and reference source
increasing time. FTIR measurements indicated that provides a working knowledge of an array of separation
transformation of the hydroxyl groups led to a weakening methods. In forty-two chapters, it explores all major
of the overall hydrogen bonding strength in the degraded categories of separation. With an emphasis upon everyday
samples so a reduction in the intermolecular cohesion, practice rather that theory, this book explains the
and hence the barrier properties of the copolymer, could principles and parameters of these methods and provides
be anticipated. 19 refs. 59 specific experiments to demonstrate proper procedures.
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; These experiments feature step-by-step protocols for each
WESTERN EUROPE separation scheme, precise instructions on setting up the
Accession no.819207 apparatus, and checklists for essential chemicals and
supplies. Main Headings include Separations involving
Item 95 phase changes; Separations involving extraction;
Polymer Science Series B Separations involving chromatography; Separations
43, Nos. 3-4,March/April 2001, p.105-8 involving ion exchange resins; Separations involving
TRANSFORMATIONS OF ANTIMONY- electric fields; Separations involving flotation;
HALOGEN- AND NITROGEN-PHOSPHORUS- Separations involving membranes; Separations involving
BASED FLAME RETARDANTS IN miscellaneous techniques.
POLYOLEFINS AND THEIR PERFORMANCE USA
Bogdanova V V Accession no.816497
Belorussian,State University
Degradation products from both antimony-halogen based Item 98
and nitrogen-phosphorus based flame retardants were Polymer Bulletin
studied using X-ray diffraction and atomic emission 46, No.2-3, April 2001, p.191-6
analysis. Evidence of the retardation mechanisms in use MISCIBILITY OF POLYETHERIMIDE AND
against combustion was obtained for each system and in POLYBUTYLENE NAPHTHALATE BLENDS
each case emission of volatile combustion inhibitors at Lin C H; Wang C S
the degradation temperature of the polymer matrix was Taiwan,Kung Shan Institute of Technology;
the critical factor. 11 refs Taiwan,National Cheng Kung University
BELARUS; BELORUSSIA DSC, optical microscopy, and SEM were performed to
Accession no.818458 characterise the miscibility of a blend of polybutylene
naphthalate and polyetherimide. Data were compared with
Item 96 theoretical predictions. 6 refs.
Polimery CHINA
45, Nos.11-12, 2000, p.51-8 Accession no.816205
Polish
PYROLYSIS GAS CHROMATOGRAPHY AND Item 99
NEW POSSIBILITIES OF ITS USE IN THE Journal of the National Institute of Materials and
ANALYSIS OF POLYMERS Chemical Research
Hetper J 8, No.4, 2000, p.149-59
Major conditions are formulated to ensure that pyrolysis Japanese
gas chromatography yields reliable and repeatable results, POSITRONIUM FORMATION AND DIFFUSION
particularly when non-volatile substances such as IN POLYMERS
techniques can be used to address topics such as lifetime temperatures and frequencies were used in the
prediction and failure analysis. Questions related to investigation. Results by each technique indicated that
identification, commercialisation, competitiveness, failure the degree of microphase separation of PUR into hard-
and performance. segment (HS) microdomains and soft-segment (SS)
USA microphase increases on addition of SAN. The various
Accession no.811310 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
Item 109 the same temperature are similar for DSC, TSDC and
Journal of Materials Science Letters DMTA and shorter for DRS. The PUR/SAN blends are
20, No.3, 1st Feb.2001, p.257-8 classified as fragile systems. 40 refs.
COMMENTS ON A NEW RAMAN PEAK IN A
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;
HIGH-DENSITY POLYETHYLENE WESTERN EUROPE
Rodriguez A B; Young R J Accession no.810314
Navarra,Universidad Publica; Manchester,University;
UMIST
Item 111
Raman spectroscopy yields information about the Macromolecular Rapid Communications
molecular structure of materials based on the observation 22, No.2, 8th Feb.2001, p.51-67
of scattered light spectra, and has been used extensively EVANESCENT WAVE LIGHT SCATTERING.
in the investigations of polymer structure and FUSION OF THE EVANESCENT WAVE AND
composition: chemical structure and interactions, LIGHT SCATTERING TECHNIQUES TO THE
morphology, crystalline and amorphous structure, STUDY OF COLLOIDS AND POLYMERS NEAR
processing effects and orientation, etc. As an analytical THE INTERFACE
technique, however, it is not free from artefacts, i.e. Matsuoka H
apparent experimental results that are not actually real Kyoto,University
but are due to the experimental methods or conditions.
One factor that may be responsible for the presence of The evanescent wave light scattering technique, which is
artefacts in Raman spectroscopy is external background produced by a fusion of the evanescent wave technique
light. There are numerous potential sources of external and light scattering technique, is a very powerful an useful
background light that lead to sharp spectral peaks. If they tool for investigation of colloidal particles and polymers
are not excluded from the collection optics of the Raman near the surface and interfaces. Two kinds of evanescent
instrument, they can lead to noise, or artefacts, wave light scattering apparatuses are developed. One is
superimposed on the Raman spectrum from the sample. the evanescent wave dynamic light scattering (EVDLS)
This background light can come from either the sample technique and the other is the evanescent wave light
or from the environment around the sample. A study of scattering microscope (EVLSM). By EVDLS, the diffusion
the latter is reported. 14 refs. behaviour of a colloidal particle near the interface can be
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK; extracted quantitatively as a function of the distance from
WESTERN EUROPE the interface. The diffusion coefficient is smaller than those
Accession no.811165 for particles in bulk, reflecting electrostatic and
hydrodynamic interactions. By EVLSM, the interaction
potential profile between a colloidal particle and the surface
Item 110 in dispersion can be directly evaluated. EVLSM will play
Journal of Applied Polymer Science an import role in colloidal interaction studies, especially at
80, No.7, 16th May 2001, p.1071-84 a low ionic strength. It is also shown that a particle dynamics
PHASE BEHAVIOUR AND MOLECULAR study is possible by the EVLSM technique. A new field
MOBILITY IN POLYURETHANE/STYRENE- will be developed in colloid science and polymer science
ACRYLONITRILE BLENDS by application of the evanescent wave light scattering
Vatalis A S; Kanapitsas A; Delides C G; Viras K; Pissis P technique, i.e. fusion of the evanescent light and a scattering
Kozani,Technological Education Institute; techniques. 41 refs.
Athens,University; Athens,Kapodistrian University JAPAN
The molecular mobility and microphase separation in Accession no.809623
blends of crosslinked polyurethane (PUR) and styrene-
acrylonitrile (SAN) copolymer were investigated. The
Item 112
PUR and SAN copolymer were prepared by reactive
Journal of Applied Polymer Science
blending with polymer polyols. DSC, thermally
79, No.6, 7th Feb.2001, p.1101-12
stimulated depolarisation currents (TSDC) techniques,
ULTRASONICATION AND MICROWAVE
dielectric relaxation spectroscopy (DRS) and dynamic
ASSISTED EXTRACTION OF DEGRADATION
mechanical thermal analysis over a wide range of
PRODUCTS FROM DEGRADABLE
STRUCTURE FORMATION DURING THE analytical data, including data on the relation between
ISOTHERMAL CRYSTALLISATION OF retention time and nitrile polarity, and the limiting yield on
ORIENTED AMORPHOUS POLY(ETHYLENE pyrolysis as a function of temperature were obtained. On
TEREPHTHALATE) FILMS the basis of these results, specific applications of PGCA and
Radhakrishnan J; Kaito A the usefulness of this method for studying the thermal
Japan,National Institute of Materials & Chemical degradation of acrylonitrile polymer are indicated. 20 refs.
Research JAPAN
conditions are investigated for four epoxy/amine systems, filter parameters and the most suitable sampling lines in
including commercial RTM6 and F934 resins. Differential terms of flow rate, diameter, construction material and
scanning calorimetry is the thermoanalytical technique operating temperature have been specified. In the large
used to determine the Tg advancement, and rheometry scale, special concern was given to the probe design and
for determination of the chemoviscosity profiles of these the effects of the probe location as well as practical
resin systems. The complex cure kinetics are correlated considerations of the sampling line length. Quantitative
to the Tg advancement via a one-to-one relationship using calibration and prediction methods have been constructed
Di Benedetto’s formula. It is revealed that the three- for different components present in smoke gases.
dimensional network formation follows a single activated Recommendations on how to deal with interferents, non-
mechanism independent of whether the cure kinetics linearities and outliers have been provided and a
follow a single or several activation mechanisms. The verification method for the spectrometer for unexpected
viscosity profiles show the typical characteristics of variations and for the different models have been
epoxy/amine cure. A modified version of the Williams- described. FTIR measurement procedures in different fire
Landel-Ferry equation (WLF) is adequate to model the test scenarios are studied using the recommendations of
viscosity profiles of all the resin systems, in the this project for measurement techniques and analysis and
temperature range 130 to 170 deg.C, with a very good an interlaboratory trial of the FTIR technique in smoke
degree of accuracy. The parameters of the WLF equation gas analysis is carried out to define the repeatability and
are found to vary in a systematic manner with cure reproducibility of the method in connection with a small
temperature. Further correlation between Tg and viscosity scale fire test method, the cone calorimeter. 9 refs.
shows that gelation, defined as the point where viscosity BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
reaches 10 4 Pas, occurs at a unique Tg value for each FINLAND; FRANCE; ITALY; SCANDINAVIA; SWEDEN; UK;
resin system, which is independent of the cure conditions. WESTERN EUROPE
16 refs. Accession no.784096
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
Item 151
Accession no.784172 Polymer
41, No.23, Nov.2000, p.8241-5
Item 150 USE OF RAMAN SPECTROSCOPY TO STUDY
Fire & Materials THE REACTION BETWEEN AN AMINE-
24, No.2, March/April 2000, p.101-12 TERMINATED THERMOPLASTIC AND EPOXY
SMOKE GAS ANALYSIS BY FOURIER RESINS
TRANSFORM INFRARED SPECTROSCOPY - van Overbeke E; Carlier V; Devaux J; Carter J T;
SUMMARY OF THE SAFIR PROJECT RESULTS McGrail P T; Legras R
Hakkarainen T; Mikkola E; Laperre J; Gensous F; Louvain,Universite Catholique; ICI Plc
Fardell P; Le Tallec Y; Bajocchi C; Paul K; Simonson Reactive thermoplastics are often used as toughening
M; Deleu C; Metcalfe E modifiers for epoxy resins. Raman spectroscopy was used
VTT Building Technology; Centexbel; Elf Atochem to follow the reaction of aromatic amines with epoxide
SA; UK,Building Research Establishment; CEMATE; monomers through the evolution of an amine-substituted
LSF SUD srl; Rapra Technology Ltd.; Sweden,National aromatic vibration. A double shift of this peak was correlated
Testing & Research Institute; Ghent,University; with the formation of secondary and tertiary amines. Band
Greenwich,University assignment was confirmed by the study of model
The determination of toxic components from fire gases compounds. Using this method, qualitative observation of
is difficult because the environment is hot, reactions are the reaction between an amine-terminated copolyether-
often temperature dependent, and a lot of soot may be sulphone thermoplastic and epoxide was performed.
produced. Due to the different properties of the gas Unfortunately, in the blend studied containing the curing
components, a different time-consuming procedure for agent, a band appearing upon curing overlapped with the
each species has traditionally been used. The use of FTIR band characterising the end group reaction. 17 refs.
(Fourier transform infrared) spectrometers as a continuous BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
UK; WESTERN EUROPE
monitoring technique overcomes many of the problems
in smoke gas analyses. FTIR offers an opportunity to set Accession no.783075
up a calibration and prediction method for each gas
showing a characteristic spectral band in the infrared Item 152
region of the spectrum. The objective of the SAFIR project Polymer Degradation and Stability
was to further develop the FTIR gas analysis of smoke 68, No.3, 2000, p.437-43
gases to be an applicable and reliable method for the SEMI-QUANTITATIVE ANALYSIS OF
determination of toxic components in combustion gases THERMAL DEGRADATION IN
related to fire test conditions. The optimum probe design, POLYPHENYLENE ETHER
technique used in these experiments was a reliable and conditions. Within this project, optimal working
environmentally-friendly alternative to the commonly- conditions including sampling, calibration and analysis
used liquid extraction and analytical methods. 22 refs. for FTIR fire gas method are defined and verified under
EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN a variety of fire test scenarios. The FTIR method are
EUROPE shown to be a repeatable and reproducible method for
Accession no.770687 the determination of the most important toxic gas
components of real fires. Moreover, the findings of this
Item 172 project concerning sampling techniques are most relevant
Macromolecular Symposia for other methods used for defining fire gases. 5 refs.
Vol.148, Dec.1999, p.463-81 EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN
CHARACTERIZATION OF ACRYLIC DENTAL EUROPE
POLYMERS Accession no.768669
Vera-Graziano R; Martinez-Richa A; Palacios-Alquisira
J; Barcelo-Santana F; Castano-Meneses V Item 174
Mexico,Universidad Nacional Autonoma; Surface Coatings International
Guanajuato,Universidad 83, No.3, March 2000, p.111-8
DETERMINATION OF VOC EMISSIONS FROM
The chemical composition, dimensions and the molecular
LATEX PAINTS DURING AND AFTER
parameters of four dental acrylic polymer materials and
APPLICATION; METHODS, PERFORMANCE
two polyacrylic acids of different molec.wt. used as model
AND PRECISION
compounds were studied by NMR and IR spectroscopies,
Zeh H
GPC, intrinsic viscosity and light scattering
Wacker Polymer Systems GmbH
measurements. Two of the dental polymers were shown
to be mainly polyacrylic acid, while one showed the peak VOC emissions from indoor latex paints during and after
pattern for an acrylic acid/methyl acrylate copolymer of application is determined by four different test methods:
about 2:1 composition and one was an oligomer derived a chamber method in which an emission chamber is
from 2-hydroxyethyl methacrylate. The steric hindrance combined with gas chromatography, two practical
parameter, molecular stiffness and second virial methods in which VOC emitted in a room is measured
coefficient were calculated using different thermodynamic either by the determination of the total organic carbon or
models. The Flory-Fox-Shafgagen and the Stockmayer- by infrared spectroscopy, and an ‘in-can-individual-VOC
Fixman models fitted the experimental data reasonably method’ which determines the VOC of a liquid paint by
well and could be use to describe the molecular parameters the quantitative analysis of each volatile component. VOC
of the acrylic polymers. 18 refs. (7th International emission data gathered by these methods are compared
Conference on Polymer Characterization (POLYCHAR- with calculations from a dynamic computer model
7), Denton, Texas, USA, Jan.1999) describing the time-dependence of the VOC emission in
MEXICO the room atmosphere. This comparison indicates that the
Accession no.770356 ‘in-can-individual-VOC method’ with computer
calculation allows variations in the size of the room, the
Item 173 application rate, VOC content of the paint and the rate of
Flame Retardants 2000. Conference proceedings. air change, without the necessity of additional
London, 8th-9th Feb.2000, p.185-92 experiments, and therefor, offers an approach with a
PRACTICE OF FTIR ANALYSIS FOR FIRE reduction in costs. 10 refs.
GASES (SAFIR) EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Mikkola E WESTERN EUROPE
VTT Building Technology Accession no.768107
(BPF; Interscience Communications Ltd.; APME;
European Flame Retardant Assn.; Fire Retardant Item 175
Chemicals Assn.) Journal of Coatings Technology
72, No.902, March 2000, p.53-61
The use of FTIR (Fourier transform infrared)
ACID ETCH OF AUTOMOTIVE CLEARCOATS.
spectrometers as a continuous monitoring technique
II. COMPARISON OF DEGRADATION
overcomes many of the problems associated in analyses
CHEMISTRY IN LABORATORY AND FIELD
of hot fire gases. FTIR offers an opportunity to set up a
TESTING
calibration and prediction method for each gas showing
Schmitz P J; Holubka J W; Xu L-F
a characteristic spectral band in the infrared region of the
Ford Motor Co.
spectrum. A European project, SAFIR, aims to further
develop the FTIR gas analysis of smoke gases to be an X-ray photoelectron spectroscopy was used to determine
applicable and reliable method for the determination of whether exposure conditions used in the laboratory
toxic components in combustion gases related to fire test gravimetric etch testing of acrylic melamine clearcoats
simulated field degradation pathways. The surface The fibre-matrix interface in carbon fibre-reinforced
chemistry of the field exposed panels was examined and epoxy resin composites was studied by time of flight
the results compared with those for laboratory treated secondary ion mass spectrometry (ToF-SIMS) using novel
powders having identical technologies. Consistency in the preparation techniques. The initial adsorption between
formation of a melamine salt and ammonium sulphate uncured resin or amine curing agent and the fibre was
upon field exposure and laboratory acid treatment investigated by the use of adsorption isotherms obtained
indicated that the laboratory treatment conditions by the analysis of fibre surfaces following immersion in
simulated the field exposure conditions. 7 refs. liquid solutions of the resin. The intact interphase of a
USA composite could be examined by ToF-SIMS following
Accession no.767768 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;
Item 176 WESTERN EUROPE
Journal of Adhesion Science and Technology Accession no.765326
14, No.5, 2000, p.745-64
XPS ANALYSIS OF THE COVERAGE AND
COMPOSITION OF COATINGS ON GLASS Item 179
FIBRES Adhesion ’99. Conference Proceedings.
Thomason J L; Dwight D W Cambridge, UK, 15th-17th Sept.1999, p.347-50
Owens-Corning Science & Technology Center MICRO THERMAL ANALYSIS AT
INTERPHASES
The use of X-ray photoelectron spectroscopy as a method
Hassler R; zur Muhlen E
for characterising different sizings on glass fibres was
Dresden,Institut fuer Polymerforschung; TA
evaluated. A model, based on a patchy sizing overlay
Instruments GmbH
hypothesis, was developed to aid in the reduction of data
(IOM Communications Ltd.)
obtained from the X-ray photoelectron spectroscopic
analysis. It is shown that the spectroscopic results, when Details are given of a thermal analysis technique, referred
combined with the weight fraction of the sizing, provide to as micro thermal analysis, which combines the high
a quantitative value for the coverage of the fibre surface resolution positioning of scanning probe microscopy with
by the sizing. 25 refs. some of the quantitative analysis capabilities of conventional
USA thermal analysis. The application of this technique in
Accession no.767755 characterising the thermal properties of interfaces in
aluminium/epoxy resin adhesive joints and in glass fibre-
reinforced epoxy resin composites is described. 7 refs.
Item 177 EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Polymer News UK; WESTERN EUROPE
25, No.2, Feb.2000, p.56-8 Accession no.765322
POLYMER ANALYSIS AND
CHARACTERISATION
Garbassi F Item 180
EniChem SpA Macromolecules
33, No.1, 11th Jan.2000, p.120-4
Analytical techniques, such as mass spectroscopy, atomic BRANCHING AND CROSSLINKING IN
absorption spectroscopy and atomic emission RADIATION-MODIFIED PTFE. A SOLID-STATE
spectroscopy, for the detection of trace elements, mainly NMR INVESTIGATION
metal trace elements, in polymers, used particularly in Fuchs B; Scheler U
food, are briefly considered. The disadvantages and Dresden,Institute of Polymer Research
suitability of such techniques are summarised. 10 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
High-resolution fluorine 19 NMR was used to investigate
WESTERN EUROPE the structural changes resulting from PTFE electron
Accession no.766702 irradiation under vacuum. A quantitative analysis of the
data was used to establish the density of side groups and
branches. 20 refs.
Item 178 EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Adhesion ’99. Conference Proceedings. WESTERN EUROPE
Cambridge, UK, 15th-17th Sept.1999, p.369-73 Accession no.764731
INTERPHASE CHEMISTRY OF CARBON FIBRE
COMPOSITE MATERIALS
Prickett A C; Vickers P E; Smith P A; Watts J F Item 181
Surrey,University Color and Appearance Retec 1999. Conference
(IOM Communications Ltd.) proceedings.
Nashville, Tn., 27th-29th Sept.1999, p. 178-87 drinking water in contact with PP pipes was studied.
USING MICROSCOPY AS A PROBLEM Austrian, German and International Standard methods
SOLVING TOOL IN PLASTICS were used for water at 23C and 60C. The low molecular
Compton C degradation product 2,4-di-tert-butylphenol, rather than
Sun Chemical Corp. the high molecular antioxidants, was detected in the
(SPE,Color & Appearance Div.) aqueous extracts. In warm water extracts, the
concentration of phenols, the total organic carbon content
Microscopy is a valuable tool for pigment evaluation and
and the effect on odour and flavour were considerably
problem solving in plastics and other applications. The
higher than in cold. Alkaline water extracted higher
organic pigments used in plastic applications are typically
amounts of phenols but acidic drinking water showed no
sub-micron in size. Pigment performance is greatly affected
effect. Thermal loading of PP during the extrusion process
by how well the pigment particles are incorporated in the
significantly increased the extractable phenols, total
polymer medium. Various microscopic evaluation
organic carbon content and flavour number/threshold
techniques that can be used to investigate dispersion quality,
odour. 7 refs.
strength development and thermal stability are reviewed.
AUSTRIA; EUROPEAN UNION; WESTERN EUROPE
In addition, various microscopic techniques for identifying
contaminants are discussed. 7 refs. Accession no.763574
USA
Accession no.764247 Item 184
West Conshohocken, PA, 1999, pp.6. NALOAN.
ASTM D 2124-. METHOD FOR ANALYSIS OF
Item 182
COMPONENTS IN POLY (VINYL CHLORIDE)
Composites Part A: Applied Science and
COMPOUNDS USING AN INFRARED
Manufacturing
SPECTROPHOTOMETRIC TECHNIQUE
31A, No.2, 2000, p.165-71
American Society for Testing & Materials
FAILURE PHENOMENA IN TWO-
ASTM D 2124-
DIMENSIONAL MULTI-FIBRE
MICROCOMPOSITES. PART IV: A RAMAN Version 99. Photocopies and loans of this document are
SPECTRASCOPIC STUDY ON THE INFLUENCE not available from Rapra.
OF THE MATRIX YIELD STRESS ON STRESS USA
CONCENTRATIONS Accession no.760789
van den Heuval P W J; Peijs T; Young R J
Eindhoven,University of Technology; UMIST; Queen
Mary & Westfield College Item 185
Journal of Coatings Technology
Raman spectroscopy is used to study the influence of shear 72, No.900, Jan.2000, p.69-74
yield stress of the matrix on stress situations in carbon ANALYSIS OF EXEMPT PAINT SOLVENTS BY
fibre/epoxy resin composites containing a planar fibre GAS CHROMATOGRAPHY USING SOLID-
array. A mixture of two curing agents, with different PHASE MICROEXTRACTION
functionality and molecular weights, are used to cure the Bodrian R R
epoxy resin in order to obtain a matrix with varying cross- California,Polytechnic University
linked density. The carbon fibres are surface treated to
give good fibre-matrix adhesion. Three matrix systems Acetone, methyl acetate and parachlorobenzotrifluoride
are investigated in the study, each with a different yield have been exempted as VOC solvents by the EPA. In
stress. The mechanical properties of each material are measuring coating VOC content, separate methods for
measured under tension and shear conditions. 35 refs. determining exempt solvents are required. One such
EUROPEAN COMMUNITY; EUROPEAN UNION;
method utilises solid-phase microextraction to sample the
NETHERLANDS; UK; WESTERN EUROPE headspace of solvent-based coatings to which the
Accession no.763633 surrogates acetone-d6, methyl acetate-d3 and/or
metachlorbenzotrifluoride have been added. The sampled
exempt coating solvents are thermally desorbed and
Item 183 analysed using gas chromatography with flame ionisation
Journal of Macromolecular Science A or mass spectral detection. This paper presents the results
A36, No.11, 1999, p.1751-8 obtained for acetone and toluene in a large number of
POLYPROPYLENE PIPES FOR DRINKING aerosol paints. Additionally, the results from a round-robin
WATER SUPPLY study for acetone, methyl acetate and
Hametner C parachlorobenzotrifluoride in commercial solvent-based
Austrian Plastics Institute coatings are reported. 17 refs.
The migration of phenolic antioxidants (which are USA
typically used for the stabilisation of PP pipes) into Accession no.760572
hydroxy propylether). The overall degradation process is mode atomic force microscopy (AFM). The
quantified, and most significant pathways of thermolysis microfibrils feature is observed with an average width
are identified through subsequent spectroscopic analysis of 500 nm, composed of various types of periodical
of products of decomposition. The design and construction units of an average size 50 nm in a pleating appearance.
of a modified vacuum-tight long-path gas IR cell, as an At the less crystalline spot on the Kevlar fibre surface,
interface allowing for the application of Fourier transform the periodical organisations exhibit the skin core-like
infrared spectroscopy (FT-IR) for the online analysis of differentiation. In contrast, at the highly crystalline
volatile products of polymer degradation, is described. spot, the periodicity is more uniformly arranged by a
Proof of concept and application of this new analytical rectangular network manner. Inverse gas
technique, subsequently referred to as TVA/FT-IR, is chromatography (IGC) is used as a tool to investigate
illustrated through the examination of appropriate aspects the surface structure heterogeneity by calculating the
of the thermal degradation of PMMA polymers. 49 refs. surface energy of different types of probes adsorbed
USA on the Kevlar fibre surface. The energy sites
Accession no.760230 distribution plot of n-hexylamine adsorption at finite
dilution exhibits a two-adsorbing-peaks curve. At the
Item 190 higher energy site, a possible hydrogen bonding
Analytical Chemistry interaction is proposed between n-hexylamine and
71, No.21, 1st Nov.1999, p.4793-9 oxygen-containing groups formed at the less crystalline
GEL PERMEATION CHROMATOGRAPHY surface. According to the AFM and IGC results, a
COUPLED TO FOURIER TRANSFORM MASS Kevlar fibre surface organisations model at the
SPECTROMETRY FOR POLYMER nanometer scale is proposed. 19 refs.
CHARACTERIZATION EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
SWITZERLAND; WESTERN EUROPE
Aaserud D J; Prokai L; Simonsick W J
Florida,University Accession no.758987
isophthalate in food simulants. The method consists in proposed and tested liquid chromatographic elution of
extracting DMT and DMIP from the food simulants with homopolymers under limiting conditions of desorption
chloroform and analysing of the compounds by GC with and takes into account the simultaneous effect of
the use of calibration curves and diethyl terephthalate as adsorption and exclusion of macromolecules onto/from
an internal standard. 3 refs. Articles from this journal can the column packing. 17 refs.
be requested for translation by subscribers to the Rapra SLOVAK REPUBLIC; SLOVAKIA
produced International Polymer Science and Technology. Accession no.743327
EASTERN EUROPE; POLAND
Accession no.745025 Item 211
Polymer Recycling
Item 209 3, No.4, 1997/1998, p.263-7
Journal of Applied Polymer Science PROCEDURES FOR THE COMPOSITIONAL
73, No.2, 11th July 1999, p.221-6 ANALYSIS OF REINFORCED POLYESTER
EVALUATION OF EVA-PVAC BLEND RECYCLATE
BEHAVIOUR BY 1-D AND 2-D SOLID-STATE Bream C E; Hornsby P R
NMR Brunel University
De Souza C M G; Pacheco C R; Tavares M I B
In order to consider effective strategies for the recovery
Rio de Janeiro,Universidade Federal; PETROBRAS
and reuse of plastics recyclates, a quantitative method is
Ethylene-co-vinyl acetate and poly(vinyl acetate) blends described for the characterisation of polyester-based
were prepared in different proportions by melting in a moulding compounds. Analytical procedures are
HAAKE Rheomix mixer. The blends were prepared at a described for the quantification of fibre, filler and fire
fixed temperature, rotation rate, and processing time. retardant contents in polyester moulding compounds
High-resolution solid state NMR was used to characterise containing calcium carbonate filler, glass fibre
the blends with respect to structure-mobility-compatibility reinforcement, and aluminium hydroxide flame retardant.
using magic angle spinning with cross-polarisation and 3 refs.
high power hydrogen decoupling and measurements of EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
the proton spin-lattice relaxation time in the rotating WESTERN EUROPE
frame. Miscibility between polymer chains was also Accession no.742796
studied by two-dimensional hydrogen ion/carbon-13 shift
correlation (HETCOR). 21 refs.
Item 212
BRAZIL
High Performance Plastics
Accession no.743489 Aug.1999, p.10
IDENTIFICATION OF PLASTICS IN WASTE
Item 210 A review is presented of the methods used in the
Macromolecules identification of plastics waste prior to recycling
32, No.11, 1st June 1999, p.3671-3 operations, which was published in International Polymer
LIQUID ADSORPTION CHROMATOGRAPHY Science and Technology, and translated from a Polish
OF COPOLYMERS: MOLAR MASS source. Rapid spectroscopic methods are indicated, and
(IN)DEPENDENT RETENTION their use in packaging and automotive recycling are
Berek D discussed.
Slovak Academy of Sciences EASTERN EUROPE; POLAND
Liquid adsorption chromatography with a continuous Accession no.742675
solvent gradient elution was shown by several previous
authors to be capable of separating random and graft
Item 213
copolymers according to their chemical composition, with
Journal of Polymer Science: Polymer Physics Edition
their molar masses not playing an important role. A
37, No.13, 1st July 1999, p.1485-94
tentative explanation of this finding is presented. It is
GLASS TRANSITION AND MISCIBILITY IN
assumed that the copolymer species travel along the
BLENDS OF TWO SEMI-CRYSTALLINE
column with a velocity which exactly corresponds to that
POLYMERS: POLYARYL ETHER KETONE AND
of the eluent composition, exhibiting a displacing power
POLYETHER ETHER KETONE
just necessary to prevent a fast progress of the
Woo E M; Tseng Y C
macromolecules due to their exclusion. Under specific
Taiwan,National Cheng Kung University
conditions, retention of macromolecules at this adsorption
promoting ‘barrier’ depends almost exclusively on the A study was made of the miscibility in the amorphous
copolymer composition and not on its molar mass. This region of melt mixed blends composed of a novel polyaryl
hypothesis is based on the mechanism of the recently- ether ketone (PK99) and PEEK using various methods,
including optical microscopy, DSC, SEM, FTIR Sano K; Shimoyama M; Ohgane M; Higashiyama H;
spectroscopy and wide-angle X-ray diffraction. Samples Watari M; Tomo M; Ninomiya T; Ozaki Y
were physically aged in order to resolve any possible Kwansei-Gakuin,University; Hyogo,Prefectural Police
overlapping Tg’s but only one single Tg was detected over Headquarters; Yokogawa Electric Co.
the entire composition range. No evidence for
FTIR spectra were measured for pellets of sixteen kinds
isomorphism was found and the crystal forms of the
of LLDPE with short branches and one kind of PE without
respective polymers remained distinct and unchanged by
any branch to explore the effects of the branches on the
miscibility in the amorphous region. 14 refs.
physical properties and the Raman spectrum. Partial least
TAIWAN
squares analysis regression was applied to the Raman
Accession no.742306 spectra after multiplicative scatter correction to propose
a calibration model that predicts the density of LLDPE.
Item 214 38 refs.
Applied Spectroscopy JAPAN
53, No.6, June 1999, p.672-81 Accession no.740338
POST-CONSUMER PLASTIC IDENTIFICATION
USING RAMAN SPECTROSCOPY Item 217
Allen V; Kalivas J H; Rodriguez R G Journal of Coatings Technology
Idaho,State University 71, No.893, June 1999, p.53-60
The suitability of Raman spectroscopy, when used with INVERSE GAS CHROMATOGRAPHY, SURFACE
K-nearest neighbours, library searching or cyclic subspace PROPERTIES, AND INTERACTIONS AMONG
regression, for computerised classification of post- COMPONENTS OF PAINT FORMULATIONS
consumer plastics was evaluated. Plastics investigated Ziani A; Xu R; Schreiber H P; Kobayashi T
were PETP, PP, PS, PVC, HDPE AND LDPE. Ecole Polytechnique de Montreal; Nippon Paint Co.
Modifications were made to the original cyclic subspace Inverse gas chromatography analysis at very high dilution
regression algorithm for modelling multiple sample and at finite concentrations of probe injection was carried
properties and the adapted algorithm employed to directly out on a series of polymers and pigments used in paint
compare the mechanisms of principal component formulations. Values of dispersion surface energies, and
regression and the PLS2 form of partial least-squares. It of acid-base interaction parameters were obtained for the
was found that Raman spectroscopy could be used to materials, and pair interaction parameters were calculated
identify both HDPE and LDPE. 33 refs. from the results. The dispersion stability of each pigment/
USA polymer combination was measured and correlated with
Accession no.741260 the acid-base interaction parameters of the materials, and
is shown to justify the availability of fundamental
thermodynamic interaction data to optimise performance
Item 215
aspects of protective coatings. 23 refs.
Applied Spectroscopy
CANADA; JAPAN
53, No.5, May 1999, p.557-64
COMPARISON OF NEAR-INFRARED AND Accession no.739845
RAMAN SPECTROSCOPY FOR THE
DETERMINATION OF CHEMICAL AND Item 218
PHYSICAL PROPERTIES OF NAPHTHA Analytical Chemistry
Min-Sik Ku; Hoeil Chung 71, No.10. 15th May 1999, p.2037-45
SK Corp. ANALYSIS OF POLYMERIC FLAME
RETARDANTS IN ENGINEERING
Near-infrared and FTIR Raman spectroscopy were
THERMOPLASTICS BY PYROLYSIS GAS
compared and evaluated for the quantitative analysis of
CHROMATOGRAPHY WITH AN ATOMIC
naphtha using partial least-squares regression. 19 refs.
EMISSION DETECTOR
SOUTH KOREA
Wang F C Y
Accession no.740339 Dow Chemical Co.
Halogen-containing polymeric flame retardants in
Item 216 engineering thermoplastics were analysed by pyrolysis
Applied Spectroscopy gas chromatography(Py-GC) with an atomic emission
53, No.5, May 1999, p.551-6 detector(AED) and a mass selective detector(MSD). The
FOURIER TRANSFORM RAMAN SPECTRA OF AED was very effective in monitoring halogen-containing
LINEAR LOW-DENSITY POLYETHYLENE AND pyrolysates after Py-GC. The type of polymeric flame
PREDICTION OF THEIR DENSITY BY retardant used in thermoplastics could be identified by
MULTIVARIATE DATA ANALYSIS peak pattern recognition through an AED halogen element
trace. A set of thermoplastic resins containing different were poly(vinyl acetate)/poly(methyl acrylate),
brominated polymeric flame retardants was studied. After poly(phenylene oxide)/PS and two poly(styrene-co-
generation of the pyrogram by Py-GC/AED, those acrylonitrile)/PMMA blends, the last two containing
pyrolysates produced from polymeric flame retardants different acrylonitrile contents. Specific molecular
were identified by MSD analysis of a complex total ion interactions determined whether the glass transition
chromatogram generated by the thermoplastic resins. The temperature and the increment of heat capacity versus
results demonstrated the effectiveness of the AED in the composition showed positive or negative deviations
tasks of specific element monitoring and component from linearity for the blend systems. In the non-
pattern recognition. The advantages and disadvantages interacting system (poly(vinyl acetate)/poly(methyl
of using the AED are also discussed. 11 refs. acrylate)), the glass transition temperature and increment
USA of heat capacity showed linear behaviour with
Accession no.738049 composition. Thermodynamic theories for the observed
results were discussed. 17 refs.
Item 219 EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
ACS, Polymeric Materials Science and Engineering. WESTERN EUROPE
Vol.76. Conference proceedings. Accession no.737361
San Francisco, Ca., Spring 1997, p.128-9. 012
ATOMIC FORCE MICROSCOPY STUDY OF Item 221
INTRAOCULAR LENS IMPLANTS - LCGC International
TOPOGRAPHY AND SURFACE PROPERTIES 12, No.7, July 1999, p.432/6
Kowalewski T; Ravi V N
QUANTITATIVE ANALYSIS OF
Washington,University; St.Louis,Veterans Affairs
POLY(METHYLMETHACRYLATE) IN DRUGS
Medical Center
BY CURIE-POINT PYROLYSIS GAS
(ACS,Div.of Polymeric Materials Science & Engng.)
CHROMATOGRAPHY
Cataracts are one of the most common causes of Muguruma S; Uchino S; Oguri N; Kiji J
worldwide blindness. They are presently corrected by Japan Analytical Industry Co.Ltd.; Tottori,University
surgery in which the natural cataractous lens is replaced
Curie-point pyrolysis gas chromatography was used for
by a synthetic intraocular lens. Successful visual
the quantitative analysis of residual synthetic adsorbent
rehabilitation is not only a function of patients’ health
crosslinked PMMA used in drug purification. Levels of
and the surgical technique, but it also depends on the
PMMA adsorbent below 0.15% in drug substances were
optical, mechanical and bioperformance of the intraocular
successfully measured quantitatively by Py-GC using
lens. Visual deterioration after surgery has been attributed
to cellular debris deposited on the lens surface and characteristic peaks that reflect the structure of the
capsular opacification resulting from inflammation. adsorbent, demonstrating that this analytical technique
Although the exact sequence of events that take place can be used to monitor compliance with the limit of 0.1%
when an implant is exposed to the ocular environment in organic impurity in drug substances stipulated by ICH
vivo is not known, protein adsorption, complement guidelines. 12 refs.
activation and cellular adhesion have been implicated and JAPAN
believed to be influenced by the surface properties of the Accession no.736647
implants. The surface characteristics (surface topography
and viscoelasticity) of intraocular lenses are investigated Item 222
using tapping-mode atomic force microscopy. 9 refs. Journal of Applied Polymer Science
USA 72, No.7, 16th May 1999, p.913-25
Accession no.737604 HIGH-PERFORMANCE LIQUID
CHROMATOGRAPHY-MASS SPECTROMETRY
Item 220 OF EPOXY RESINS
Polymer Fuchslueger U; Rissler K; Stephan H; Grether H J;
40, No.17, 1999, p.4763-7 Grasserbauer M
MODULATED DIFFERENTIAL SCANNING Ciba Specialty Chemicals Inc.; Vienna,Technical
CALORIMETRY: 14. EFFECT OF MOLECULAR University
INTERACTIONS ON GLASS TRANSITION
The application of liquid chromatography coupled to
BEHAVIOUR AND INCREMENT OF HEAT
mass spectrometry for the analysis of epoxy resins was
CAPACITY IN MISCIBLE POLYMER BLENDS
shown in two examples. Electrospray (ESI) and
Song M; Hourston D J; Pollock H M; Hammiche A
atmospheric pressure chemical ionisation (APCI) were
Loughborough,University; Lancaster,University
compared with respect to the ionisation of diglycidyl
Modulated differential scanning calorimetry was used ether of bisphenol A (DGEBA)-based epoxy resins. By-
to study miscible polymer blends. The blends studied products in a typical modified solid DGEBA-based
solution permitted the highly sensitive determination of RAPRA COLLECTION OF INFRARED SPECTRA
terpenic acids, aleuritic acid, several minor fatty acids and OF RUBBERS, PLASTICS AND
the wax components of shellac as their methyl derivatives THERMOPLASTIC ELASTOMERS. SECOND
on the resulting pyrograms with less than 2.0 % relative EDITION
standard deviations without using any cumbersome Sidwell J A
pretreatment. The observed average distributions of each
This book provides a set of transmission and pyrolysate
resin acid component determined by reactive Py-GC for
spectra of a comprehensive range of technically important
shellac samples from India and Thailand showed that the
rubber and plastics materials including copolymers and
average ratios among terpenic acids, aleuritic acid and the
blends which are in current use. Materials are indexed
other fatty acids were about 53:24:14 for Indian shellac
under both polymer and trade name.
and 51:35:14 for Thailand shellac, respectively, suggesting
a slightly significant difference. Clearer discrimination of Accession no.725345
the shellac samples from the two different countries was,
however, achievable by applying principal component Item 235
analysis for the mole percent distributions of all the acidic Polymer
components determined by reactive Py-GC. 24 refs. 40, No.12, 1999, p.3479-85
INDIA; JAPAN; THAILAND INVERSE GAS CHROMATOGRAPHIC
Accession no.727139 CHARACTERIZATION OF POLY(ETHYLENE
OXIDE)
Al-Saigh Z Y
Item 233
Columbus,State University
ACS Polymeric Materials Science and Engineering.
Fall Meeting 1997. Volume 77. Conference The inverse gas chromatography method was used to
proceedings. obtain the thermodynamic properties and the surface
Washington, D.C., 1997, p.594-5 .012 energy of a semicrystalline polymer, PEO. PEO was used
EFFECT OF SECOND DIMENSION SAMPLING as a stationary phase in the chromatographic column and
RATE AND PARTICLE SIZE ON RESOLUTION 16 solutes with a different chemical nature were used as
AND RUN TIME IN TWO DIMENSIONAL eluents. Alkanes showed endothermic interaction
LIQUID CHROMATOGRAPHY FOR THE parameters and the molar heat of mixing in a temp. range
ANALYSIS OF POLYMERS of 70-130C. Acetates and alcohols showed better
Murphy R E; Schure M R; Foley J P interactions with the PEO layer and butanol was found to
Rohm & Haas Co.; Villanova,University be the best solvent for PEO among all solutes used. The
(ACS,Div.of Polymeric Materials Science & Engng.) variation in molec.wt. of PEO above 400 g/mol showed
no apparent effect on the interaction coefficients. The
The optimisation of a two dimensional high performance
dispersive contribution of the surface energy of PEO was
liquid chromatography (HPLC) (reverse phase liquid
measured as a function of temp., which ranged from 8.00
chromatography/gel permeation chromatography (GPC))
and 13.00 mJ/sq m, indicating a poor surface energy of
system for the analysis of low molecular weight polymers
PEO. 43 refs.
is described. A test mixture of polyethylene glycols and a
USA
commercial surfactant was used. The analysis time of the
second dimension, GPC, was varied by using different Accession no.721885
columns. The columns had different particle sizes and
lengths, and the two dimensional resolution was compared Item 236
by varying the run time in the second dimension. Journal of Adhesion
Following the optimisation, it was possible to complete a 68, Nos.1-2, 1998, p.117-42
two dimensional analysis in the time normally taken for QUANTIFICATION OF COATING ADHESION
a normal gradient HPLC run. It was established that USING LASER INDUCED DECOHESION
conventional columns could be run with higher flow rates SPECTROSCOPY
without a significant loss of resolution. The combination Meth J S; Sanderson D; Mutchler C; Bennison S J
of shorter and smaller particle GPC columns resulted in DuPont Co.
lower sampling periods at lower flow rates than
conventional columns. The highest sampling rate into the A new technique, laser induced decohesion spectroscopy,
second dimension gave the best resolution. 7 refs. is presented, which is capable of measuring the practical
work of adhesion between a transparent polymer coating
USA
or substrate. A laser pulse directed onto the sample creates
Accession no.726180 a blister at the transparent/opaque interface. The blister’s
internal pressure depends on the laser pulse energy, and
Item 234 at a critical pressure the sample fractures, creating an
Shawbury, Rapra Technology Ltd., 1997, pp.315. annular debond similar to that obtained in the standard
220.00. 30cms. 9922 blister test. By measuring physical variables such as the
curvature of the blister, and its radius and thickness, it is Kuo C; Grieser M D; Robinson D
possible to deduce the practical work of adhesion. 19 refs. Henkel Corp.
USA (ACS,Div.of Polymeric Materials Science & Engng.)
Accession no.721348 Applications are given of the use of size exclusion
chromatography and high performance liquid
Item 237 chromatography for the characterisation of coatings
Journal of Adhesion Science and Technology systems which either use water as the major solvent or
13, No.3, 1999, p.379-91 utilise low molecular weight polymers, oligomers, and
DETERMINATION OF THE ADHESION reactive additives which are then reacted to produce high
PROPERTIES OF AN ALKYD PIGMENTED molecular weight and crosslinked films. 6 refs.
COATING BY ELECTROCHEMICAL USA
IMPEDANCE SPECTROSCOPY Accession no.720838
Gonzalez J E G; Rosca J C M
Gran Canaria,University
Item 240
Impedance measurements were performed in different ACS Polymeric Materials Science and Engineering.Fall
frequency ranges at open circuit potential for an alkyd Meeting 1997.Volume 77.Conference proceedings.
coating with titanium dioxide as a mineral pigment in Washington, D.C., 1997, p.35-6 012
3% sodium chloride. The most probable impedance LIQUID CHROMATOGRAPHY OF
equivalent circuit method was considered for data MACROMOLECULES UNDER LIMITING
analysis. The interpretation of the impedance spectra CONDITIONS OF SOLUBILITY: FIRST
permitted the determination of water permeation, the EXPERIMENTAL OBSERVATIONS
formation of blisters, swelling of the coating, and the loss Bartkowiak A; Hunkeler D; Murgasova R; Berek D
of adhesion. 17 refs. Szczecin,Technical University; Swiss Federal Institute
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; of Technology; Slovak Academy of Sciences
WESTERN EUROPE (ACS,Div.of Polymeric Materials Science & Engng.)
Accession no.721335 Liquid chromatography at the critical adsorption point
(LC LCS) was investigated. The solubility of
Item 238 macromolecules, the sensitivity of LC LCS to such
ACS Polymeric Materials Science and Engineering.Fall variables as the injection volume, concentration injected,
Meeting 1997.Volume 77.Conference proceedings. mobile phase flow rate and mixing between the injection
Washington, D.C., 1997, p.48-9 012 zone, were investigated, using polymethyl methacrylate
QUANTITATION IN THE ANALYSIS OF (PMMA) and polyacrylamide standards. It is proposed
OLIGOMERS BY HPLC WITH ELSD that using tetrahydrofuran and n-hexane as eluents for
Trathnigg B; Kollroser M; Maier B; Berek D; Janco M PMMA, at the LC LCS, limited polymer insolubility or
Graz,Karl-Franzens-Universitat; Slovak Academy of even local precipitation is combined with the size
Sciences exclusion of macromolecules. 12 refs.
(ACS,Div.of Polymeric Materials Science & Engng.) EASTERN EUROPE; POLAND; SLOVAK REPUBLIC;
SLOVAKIA; SWITZERLAND; WESTERN EUROPE
The influence of the operating parameters used when
Accession no.720833
operating evaporative light scattering detectors in
conjunction with high performance liquid
chromatography for the characterisation of oligomers was Item 241
investigated, using polyether samples. It was concluded ACS Polymeric Materials Science and Engineering.Fall
that the instrument was useful because it provided gradient Meeting 1997.Volume 77.Conference proceedings.
elution, however, very careful calibration was required Washington, D.C., 1997, p.31-2 012
to obtain reliable quantitative data. 16 refs. LIQUID CHROMATOGRAPHY OF
AUSTRIA; WESTERN EUROPE MACROMOLECULES AT THE CRITICAL
Accession no.720839 ADSORPTION POINT: PROBLEMS AND
PITFALLS
Berek D; Janco M
Item 239 Slovak Academy of Sciences
ACS Polymeric Materials Science and Engineering.Fall (ACS,Div.of Polymeric Materials Science & Engng.)
Meeting 1997.Volume 77.Conference proceedings.
Washington, D.C., 1997, p.46-7 012 The role of column packing pore size in liquid
APPLICATION OF SEC AND HPLC TO THE chromatography at the critical adsorption point was
CHARACTERIZATION OF POLYMERS, investigating using three silica gels and a series of
OLIGOMERS, AND SMALL MOLECULES USED polymethyl methacrylates (PMMA), using toluene,
IN COATINGS AND INKS tetrahydrofuran (THF) or their mixtures as eluents.
Toluene strongly promotes adsorption of PMMAs on the Dallas, Tx., Spring 1998, p.102-3. 012
silica surface, whereas THF suppresses adsorption. It was COUPLED PROGRAMMED PYROPROBE-MASS
established that the pore size of the column packings SPECTROMETRY AND
played an important role in liquid chromatography at the THERMOGRAVIMETRIC-MASS
critical adsorption point. The column with the smallest SPECTROMETRY
pores largely determined the behaviour of the whole set. Carraher C E; Molloy H M; Louda J W; Baker E
The feasibility of using silica gel as column packings for Florida,Atlantic University; Florida,Center for
liquid chromatography at the critical adsorption point is Environmental Studies; Midwest Research Institute
questioned. 14 refs. (ACS,Div.of Polymeric Materials Science & Engng.)
SLOVAK REPUBLIC; SLOVAKIA In 1977, a thermogravimetric analysis unit was
Accession no.720831 successfully coupled with a mass spectrophotometer, TG-
MS. More recently, a coupled programmed pyroprobe-
Item 242 mass spectrophotometry system, also utilising IR
ACS Polymeric Materials Science and Engineering.Fall spectroscopy, was employed as a means of describing
Meeting 1997.Volume 77.Conference proceedings. degradation sequences as a function of temperature. The
Washington, D.C., 1997, p.22-3 012 application of these tools as a means to define polymer
2D-LC OF FUNCTIONAL POLYETHERS structure and degradation products is described. 9 refs.
Trathnigg B; Kollroser M; Parth M USA
Graz,Karl-Franzens-Universitat Accession no.719193
(ACS,Div.of Polymeric Materials Science & Engng.)
A combination of liquid chromatography under critical Item 245
conditions using coupled density and RI detection in one ACS Polymeric Materials Science & Engineering,
dimension, and gradient high performance liquid Spring Meeting 1998. Volume 78. Conference
chromatography in the second dimension, was used in proceedings.
the two-dimensional chromatographic analysis of the Dallas, Tx., Spring 1998, p.219-20. 012
oligomers present in fatty alcohol ethoxylates. Full SECONDARY TRANSITIONS IN POLYMERS
resolution was achieved. 6 refs. PROBED BY DIFFERENTIAL SCANNING
CALORIMETRY
AUSTRIA; WESTERN EUROPE
Bertolucci P R H; Harmon J P
Accession no.720827 South Florida,University
(ACS,Div.of Polymeric Materials Science & Engng.)
Item 243
The use of differential scanning calorimetry to identify
ACS Polymeric Materials Science and Engineering.Fall
secondary transitions in thermoplastics is studied. The
Meeting 1997.Volume 77.Conference proceedings.
temperature and breadth of the secondary transition are
Washington, D.C., 1997, p.20-1 012
related to the those of the alpha transition in a variety of
MOLECULAR CHARACTERIZATION OF
methacrylate, acrylate and styrene polymers, as well as
COMPLEX POLYMERS BY COUPLED LIQUID
polycarbonate. The effect of thermal history and the
CHROMATOGRAPHIC PROCEDURES
position and sharpness of these endothermic transitions
Berek D is discussed. Some comparisons are made between this
Slovak Academy of Sciences technique and results obtained via dielectric analysis and
(ACS,Div.of Polymeric Materials Science & Engng.) dynamic mechanical analysis obtained in the laboratory.
Size exclusion chromatography alone cannot characterise 7 refs.
the constituents of complex polymer systems. Separation USA
selectivity and characterisation of complex systems may Accession no.718740
be enhanced with liquid chromatographic (LC) methods
utilising combinations of different separation
Item 246
mechanisms. These are termed coupled LC procedures.
Macromolecular Chemistry & Physics
The applications of a variety of coupled LC procedures
200, No.2, Feb.1999, p.413-21
are discussed. 16 refs.
THERMAL PROPERTIES AND
SLOVAK REPUBLIC; SLOVAKIA
CRYSTALLISATION BEHAVIOUR OF
Accession no.720826 POLYHYDROXYBUTYRIC ACID IN BLENDS
WITH CHITIN AND CHITOSAN
Item 244 Ikejima T; Yagi K; Inoue Y
ACS Polymeric Materials Science & Engineering, Tokyo,Institute of Technology
Spring Meeting 1998. Volume 78. Conference Films of blends of polyhydroxybutyric acid with chitin
proceedings. and chitosan were prepared as completely biodegradable
polyester-polysaccharide composites. Crystallisation was systems under elongational interactions in polymer bilayer
examined using DSC. Data are given from FTIR and systems under elongational deformations and changes in
carbon 13 NMR. 31 refs. potential energy, leading to determination of the work of
JAPAN adhesion. This research expands the scope of previous
Accession no.716972 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
Item 247 the interfacial forces responsible for adhesion. 39 refs.
Journal of Biomedical Materials Research (Applied
USA
Biomaterials)
48, No.1, 1999, p.5-8 Accession no.715972
EXTRACTABLE FREE MONOMERS FROM
SELF-CURED DENTAL SEALANTS RESULTING Item 250
FROM DISPENSING ERRORS Analytical Chemistry
Vaubert V M; Moon P C; Love B J 71, No.2, 15th Jan.1999, p.468-75
Virginia,Polytechnic Institute IDENTIFICATION AND DETERMINATION OF
CROSSLINKERS IN CROSSLINKED
HPLC experiments were performed on a series of self-
POLYVINYLPYRROLIDONE(PVP) BY
curing polybisglycidyl methacrylate dental sealants that
PYROLYSIS-GAS CHROMATOGRAPHY(GC)/
were deliberately mismixed. The amount of extractable
MASS SPECTROMETRY(MS)
sealant under conditions of nonideal processing was
Cheng T M H; Malawer E G
measured. 13 refs.
International Specialty Products
USA
Accession no.716163 Pyrolysis-GC and pyrolysis-GC/MS were used to identify
and quantify specific nitrogen-containing crosslinker
compounds incorporated into the structures of crosslinked
Item 248 PVP polymers which appeared to be identical by FTIR
Macromolecular Rapid Communications spectroscopy. The pyrolyser regenerated and volatilised
20, No.2, Feb. 1999, p.95-7 specific crosslinkers which could be distinguished from
CURING OF MONOMER COMPOSITES. II. USE other pyrolysate compounds by either peak retention time
OF NMR TO MONITOR REAL TIME CURING or mass spectral release. Individual compounds studied
DYNAMICS included 3-ethylidene-1-vinyl-2-pyrrolidone, 3,3'-
Martin S J; McBrierty V J; Dowling J; Douglass D C ethylidenebis(1-vinyl-2-pyrrolidone) and N,N’-
Dublin,Trinity College; Bausch & Lomb Inc. divinylimidazolidone. In general, the level of specific
Details are given of a method for monitoring the real- crosslinkers in various commercial products ranged from
time curing dynamics of composite monomers, exploiting 1.8 to 2.5% w/w. The effect of pyrolysis temp. on this
site specific information provided by high resolution level varied with the crosslinkers studied. The crosslinker
NMR. Data using polyvinylpyrrolidone, polyhydroxy- content obtained by this technique correlated with the
ethyl methacrylate and polybutylhydroxycyclohexyl swell volume data for a specific series of crosslinked PVP
methacrylate are compared with results from a computer samples made with a single crosslinker and having similar
simulation based on a multicomponent kinetic model. particle size distributions. The pyrolysis methodology
7 refs. could not distinguish the level of crosslinker which was
EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND; incorporated as a pendant functionality from that portion
WESTERN EUROPE which was incorporated through both vinyl groups. 26
Accession no.716161 refs.
USA
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Details are given of the range of physical and chemical
WESTERN EUROPE properties of flame-sprayed ethylene-methacrylic acid
Accession no.711133 copolymer following different processing conditions.
Coatings were produced at a range of specific
Item 257 temperatures by varying the propane flow rate and gun
Applied Spectroscopy traverse rate. Coatings were scanned using dielectric
52, No.12, Dec.1998, p.1498-504 relaxation spectroscopy. 24 refs.
MEASUREMENT OF ORIENTATION AND AUSTRALIA; USA
CRYSTALLINITY IN UNIAXIALLY DRAWN Accession no.709520
POLY(ETHYLENE TEREPHTHALATE) USING
POLARISED CONFOCAL RAMAN
Item 260
MICROSCOPY
Polymer Journal (Japan)
Everall N J
30, No.10, 1998, p.771-4
ICI Wilton Research Centre
CRYSTALLITE SIZES AND LATTICE
Polarised confocal Raman microscopy was used to DISTORTIONS OF GEL-SPUN ULTRA-HIGH
measure molecular orientation in uniaxially drawn PETP MOLECULAR WEIGHT POLYETHYLENE
films, prepared with draw ratios from 1 to 3.5. The FIBRES
orientation of both polarised Raman microscopy and Xiao-Ping Hu; You-Lo Hsieh
polarised attenuated total reflection IR spectroscopy. California,University
Crystallinity profiles were measured through the thickness
A detailed method is reported for deriving the lattice
of the film samples and compared with the orientation
distortions and crystallite sizes of UHMWPE fibres using
gradients existing in the films. This procedure was to
a full wide angle X-ray diffraction patterns. The
determine whether the intuitive assumption that
instrumental broadening and the background scattering
orientation and crystallinity would be positively correlated
is represented by a binomial. A discussion is included
actually holds true on the microscopic scale for these
about the diffraction trace, peak assignments, and unit
samples. 18 refs.
cell dimensions. 26 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
USA
WESTERN EUROPE
Accession no.711041 Accession no.709342
surfaces were analysed using ATR FTIR spectroscopy. The use of NMR to probe the in-situ curing of monomer
Surface reactions on PVC were heavily dependent on a prior mixtures commonly encountered in the manufacture of
thermal history of the PVC substrate. A mechanism for the contact lenses was studied. Spectral lines were identified
PVC-imidazole reactions was also presented. The PVC was which monitored curing with time of individual
useful as an implant for biomedical applications. 10 refs. components in the monomer mix. This information can
USA aid in gaining an understanding of the overall curing
Accession no.709309 dynamics and provide important guidance in establishing
suitable protocols in the manufacturing process. As a
precursor to this goal, several commonly-used component
Item 263 materials were characterised by high resolution proton
Applied Spectroscopy and carbon-13 NMR spectroscopies. The efficacy of the
52, No.11, Nov.1998, p.1483-7 overall procedure is demonstrated. 20 refs.
SAMPLING CONSIDERATIONS FOR FT- EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;
RAMAN SPECTROSCOPY OF POLYMERS AND WESTERN EUROPE
SOLUTIONS Accession no.706520
Barrerra B A; Sommer A J
Miami,University
Item 266
Details are given of the determination of apparent Polimeros: Ciencia e Tecnologia
absorption coefficients and optimal sample thickness of 8, No.1, Jan./March 1998, p.46-53
PE, PETP, cellulose, and cyclohexane by FT-Raman Portuguese
analysis. A relationship was developed that permits the THERMAL STABILITY OF POLYETHYLENE
optimal sample thickness for FT-Raman measurements TEREPHTHALATE PACKAGING:
to be determined by measuring the absorbance spectrum DETERMINATION OF OLIGOMERS
of a sample whose thickness is known. Results are Freire M T de A; Reyes F G R; Castle L
discussed in the context of scattering theory, sampling Campinas,Universidade Estadual; UK,Min.of
considerations, and spectral artifacts. 9 refs. Agriculture,Fisheries & Food
USA
PETP food packaging materials were subjected to
Accession no.709038 different heating conditions (50 minutes at 120-230C),
and oligomers were identified by HPLC coupled with
Item 264 mass spectrometry and used as a parameter for evaluating
Journal of Applied Polymer Science the thermal stability of PETP. Small changes in oligomer
71, No.3, 18th Jan.1998, p.371-5 distribution were observed only for samples heated at
PROPYLENE OLIGOMERS: EXTRACTION 230C, suggesting that PETP was thermally stable under
METHODS AND CHARACTERISATION BY the heating conditions employed. The results also
FTIR, HPLC, AND SEC suggested the suitability of PETP as a food packaging
El Mansouri H; Yagoubi N; Scholler D; Feigenbaum A; material for use in conventional and microwave ovens,
Ferrier D and for secondary recycling under controlled conditions.
INRA 28 refs.
BRAZIL; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Details are given of the isolation of propylene oligomers WESTERN EUROPE
from polymer matrix by dissolution precipitation and
Accession no.706082
Soxhlet methods. Characterisation was undertaken by
FTIR, UV spectroscopy, HPLC, and GPC. Data were used
to explain their behaviour toward packaged food products Item 267
in PP packaging. 18 refs. Journal of Thermal Analysis and Calorimetry
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; 52, No.2, 1998, p.261-74
WESTERN EUROPE THERMAL ANALYSIS OF SOME
Accession no.708984 ENVIRONMENTALLY DEGRADABLE
POLYMERS
Day M; Cooney J D; Shaw K; Watts J
Item 265 Canada,National Research Council
European Polymer Journal
34, No.12, Dec.1998, p.1817-28 The thermal characteristics of a series of degradable
CURING OF POLYMER COMPOSITES. I. NMR polymers for use in commercial composting facilities was
CHARACTERIZATION OF COMPONENT investigated using TGA and DSC. Phase changes
MONOMERS associated with some of the polymers investigated may
Martin S J; O’Brien J E; Dowling J; McBrierty V J cause problems in the interpretation of data from
Dublin,Trinity College; Bausch & Lomb Inc. composting degradation studies. Several biodegradable
All materials examined were effective thermal insulators. Popovici D; Sacher E; Meunier M
18 refs. Montreal,Ecole Polytechnique
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Teflon, type AF1600, which contains perfluorinated
WESTERN EUROPE
dioxole rings, was found to suffer significant degradation
Accession no.702142 when exposed to X-rays whilst undergoing investigation
by X-ray photoelectron spectroscopy. The degradation
Item 277 mechanism was significantly different to that of
Journal of Materials Science fluoropolymers which contain only carbon and fluorine.
33, No.14, 15th July 1998, p.3511-7 It was established that oxygen was at least as twice as
MOLECULAR ORGANISATION IN susceptible as fluorine, and that the amounts of oxygen
STRUCTURAL PVDF loss were equal to those of fluorine. Oxygen could be
Glennon D; Cox P A; Nevell R T; Nevell T G; Smith J degraded by the breaking of only one bond, the oxygen
R; Tsibouklis J; Ewen R J then forming a free radical. The free radicals produced
Portsmouth,University; West of England,University by scission of carbon-carbon bonds participated in
reactions leading to degradation and crosslinking. 9 refs.
Poly(vinylidene fluoride) containing 10% dibutyl sebacate
CANADA
plasticiser, as used in the construction of flexible oil and
gas pipelines, was exposed to raised temperatures for Accession no.700200
prolonged periods of time, to acid etching and to various
tensile deformation regimes. The effects of these Item 280
treatments on crystallinity and surface properties of this Polymer International
material were examined in the light of analytical data 47, No.1, Sept.1998, p.72-5
obtained by FTIR, DSC, X-ray diffraction, X-ray TEMPERATURE-MODULATED DIFFERENTIAL
photoelectron spectroscopy, goniometry and a variety of SCANNING CALORIMETRY. II.
microscopy techniques. 36 refs. DETERMINATION OF ACTIVATION ENERGIES
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Zhong Jiang; Hutchinson J M; Imrie C T
WESTERN EUROPE Aberdeen,University
Accession no.701984
Alternating differential scanning calorimetry (ADSC), a
commercial development of temperature-modulated
Item 278 differential scanning calorimetry, was used to determine the
Food Additives and Contaminants activation energy associated with the relaxation processes
15, No.3, 1st April 1998, p.346-54 in polycarbonate in the region of the glass transition. In this
PARTS-PER-TRILLION DETERMINATION OF procedure the frequency of the temperature modulation is
STYRENE IN YOGHURT BY PURGE-AND-TRAP varied over a range of approximately one decade, and the
GAS CHROMATOGRAPHY WITH MASS mid-point of the step change in the complex heat capacity is
SPECTROMETRY DETECTION evaluated. In these experiments, two different amplitudes
Nerin C; Rubio C; Cacho J; Salafranca J of temperature modulation were employed. The results were
Zaragoza,University in agreement with each other, and in good agreement with
Headspace sampling methods prior to capillary gas published values. Ripples seen on the Fourier-transformed
chromatography are widely used for the determination signals are attributed to the mode of the data analysis, and
of volatile compounds present in very different types of not to noise on the data. 7 refs.
samples. An automated and rapid system for EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
determination of volatiles from yoghurt was developed.
Thirty-five volatile organic compounds(VOCs) were Accession no.700165
identified in PS cups used for yoghurt packaging and 42
VOCs from yoghurt samples. Quantitative analysis of Item 281
styrene in several samples from the Spanish retail market Materials World
was carried out. 16 refs. 6, No.10, Oct.1998, p.617-9
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; THROWING LIGHT ON FIBRES AND
WESTERN EUROPE COMPOSITES
Accession no.700270 Young B
Manchester,University
Item 279 The use is discussed of Raman spectroscopy to monitor
Journal of Applied Polymer Science the stresses and strains on individual fibres in composite
70, No.6, 7th Nov.1998, p.1201-7 materials. New instrumentation has caused rapid growth
PHOTODEGRADATION OF TEFLON AF1600 in the use of Raman spectroscopy for materials
DURING XPS ANALYSIS characterisation, including the introduction of charged-
coupled device cameras which offer significant London, Chapman & Hall, 1997, p.181-233. 9
improvements in sensitivity and very low noise, and also INFRARED DICHROISM, POLARISED
holographic notch filters which are used to remove the laser FLUORESCENCE AND RAMAN
line and allow single monochromators to be used. Both SPECTROSCOPY
these developments are incorporated in the Raman imaging Bower D I
microscope developed by Renishaw in collaboration with Leeds,University
Leeds University Physics Department. Its use is described Edited by: Ward I M
with reference to aramid fibre reinforced PP. 5 refs. (Leeds,University)
RENISHAW PLC
The three spectroscopic techniques for studying
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE molecular orientation in polymers described in detail
Accession no.699334 use polarised electromagnetic radiation. The principles
of the techniques are outlined, relevant theory and
Item 282 experimental details described, and a selection of results
Farbe und Lack presented. 79 refs.
104, No.10, 1998, p.93/8 EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
German
MODULATED DIFFERENTIAL SCANNING Accession no.697738
CALORIMETRY
Haessler R Item 285
Dresden,Institut fuer Polymerforschung Polymer
The use of modulated DSC for improved interpretation 39, No.20, 1998, p.4973-6
of product characteristics under thermal effects was EFFECTS OF SUBSTRATE INTERACTIONS IN
investigated. Tgs, for example, which are masked by post- THE LIQUID CHROMATOGRAPHY OF
curing or enthalpy relaxation, could be detected in a single POLYMERS
measurement and compared. The separation of complex Kosmas M K; Bokaris E P; Georgaka E G
transitions in multicomponent systems into individual Ioannina,University
parts such as melts, transition temps. and relaxations was The elution behaviour of PMMA samples was studied
shown to be feasible. The potential for use of modulated through two liquid chromatographic columns, one
DSC in the field of epoxy resins was demonstrated using
containing a substrate of silica covered with trimethylsilyl
examples of the determination of Tg near the regions of
groups and the other a substrate of pure silica. Both
enthalpy relaxation, melt and post-curing. 7 refs.
substrates had the same pore size and the solvent was the
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE
same for both columns. The results were discussed and
they showed that the polymer-surface interactions
Accession no.699054
changed when the nature of the substrate was changed.
14 refs.
Item 283
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;
Structure and properties of Oriented Polymers. Second WESTERN EUROPE
Edition.
Accession no.696588
London, Chapman & Hall, 1997, p.234-68. 9
NUCLEAR MAGNETIC RESONANCE
Speiss H W Item 286
Max-Planck-Institut fuer Polymerforschung Food Additives and Contaminants
Edited by: Ward I M 15, No.1, 1st Jan.1998, p.93-9
(Leeds,University) SYSTEMATIC STUDY ON THE STABILITY OF
SELECTED POLYMER ANTIOXIDANTS IN EU
The basics of solid state NMR are outlined and the site-
OFFICIAL AQUEOUS AND ALTERNATIVE
selective information available from multi-dimensional
FOOD SIMULANTS USING HPLC
NMR spectra about molecular order and dynamics in
Demertzis P G; Franz R
oriented polymers is illustrated with specific experimental
examples. 55 refs. Fraunhofer Institute for Food Technol. & Packag.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Details are given of the stability of five commercial
WESTERN EUROPE antioxidants in food simulants and in an alternative fat
Accession no.697739 simulant. Analysis was performed using a rapid HPLC
method with UV detection. 23 refs.
Item 284 EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE
Structure and properties of Oriented Polymers. Second
Edition. Accession no.695963
about 20 min., and were compared with similar parameters Item 295
obtained using more conventional DSC, small angle X-ray Macromolecular Chemistry & Physics
scattering (including synchrotron), and solution-state NMR 199, No.8, 1998, p.1623-9
measurements, with good agreement. 23 refs. THERMAL STABILITY AND
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; USA; CRYSTALLISATION KINETICS OF PEEK
WESTERN EUROPE Chen J-Y; Chen M; Chao S-C
Accession no.694867 Taiwan,National Sun Yat-Sen University
TGA, dynamic rheological analysis and polarised light
Item 292 microscopy were used to assess thermal stability of PEEK.
Smart Materials & Structures Emphasis is given to the effect of melting temperature on
7, No.4, Aug. 1998, p.557-68 thermal stability. 23 refs.
IN SITU CURE MONITORING USING OPTICAL CHINA
FIBRE SENSORS. A COMPARATIVE STUDY Accession no.694246
Powell G R; Crosby P A; Waters D N; France C M;
Spooncer R C; Fernando G F Item 296
Brunel University; Cranfield,University Injection Molding
A comparative study is presented for different types of 6, No.8, Aug. 1998, p.56/9
optical fibre sensor developed to monitor the cure of an MATERIALS ANALYST: PART 13.
epoxy resin system. The sensors were based on PERFORMANCE PROBLEMS: WHEN THE
transmission spectroscopy, evanescent wave spectroscopy PELLETS DON’T MATCH THE PARTS
and refractive index monitoring. 19 refs. Sepe M
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Dickten & Masch Mfg.
WESTERN EUROPE The use of differential scanning calorimetry and
Accession no.694840 thermogravimetric analysis as analytical tools in part
failure determination is applied. Problems are examined
Item 293 in part performance of moulded 30% glass-reinforced,
Polymer Testing ’97. Day 3: Chemical Analysis. low-viscosity PEI and a second part moulded from PPS
Conference proceedings. with proprietary additives to improve wear resistance. The
Shawbury, 7th-11th April 1997, Paper 4. 9T importance of checking the composition of the basic
RAMAN SPECTROSCOPY OF POLYMERS material is stressed.
Williams K P J; Wilcock I C USA
Renishaw plc Accession no.693205
(Rapra Technology Ltd.; Plastics & Rubber Weekly;
European Plastics News) Item 297
Raman spectroscopy is now coming of age as a routine Journal of Applied Polymer Science
analytical method. Advances in Raman technology have 69, No.11, 12th Sept.1998, p.2175-85
meant that robust, user-friendly equipment can be IR SPECTROSCOPY AS A QUANTITATIVE AND
manufactured at a reasonable cost. These advances are PREDICTIVE ANALYSIS METHOD OF
described, together with applications of Raman imaging PHENOL-FORMALDEHYDE RESOL RESINS
microscope systems to polymer analysis. 11 refs. Holopainen T; Alvila L; Rainio J; Pakkanen T T
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Joensuu,University; Dynoresin Oy
WESTERN EUROPE A set of resin samples was characterised by IR and carbon-
Accession no.694712 13 NMR spectroscopy. The suitability of IR spectroscopy
for the quantitative analysis of resins was evaluated by
Item 294 statistical methods using the NMR reference data as
International Polymer Processing calibration. The values of interesting properties, e.g. the
13, No.2, July 1998, p.142-8 amount of free phenol and the formaldehyde-to-phenol
PEROXIDE INDUCED CROSSLINKING AND molar ratio, of the resins being similar to the calibration
DEGRADATION OF POLYAMIDE resins were predicted from the IR spectra. The predicted
Yu Q; Zhu S results were compared with those observed by carbon-13
McMaster University NMR spectroscopy. 15 refs.
FINLAND; SCANDINAVIA; WESTERN EUROPE
Peroxide-induced crosslinking and degradation of nylon
12 were investigated using ESR. Various reaction Accession no.692990
mechanisms are proposed. 20 refs.
Item 298
CANADA
Journal of Materials Science
Accession no.694268 33, No.13, 1st July 1998, p.3245-9
Item 306
Item 304 Antec ’98. Volume II. Conference proceedings.
Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.2215-8. 012
Atlanta, Ga., 26th-30th April 1998, p.2101-5. 012 PRACTICAL ANALYSIS TECHNIQUES OF
TEMPERATURE GRADIENT INTERACTION POLYMER FILLERS BY FOURIER
CHROMATOGRAPHY OF POLYMERS TRANSFORM INFRARED SPECTROSCOPY
Chang T; Lee W; Lee H C; Mays J W; Harville S; (FTIR)
Frater D J Coles B J; Hall C J
Pohang,University of Science & Technology; Hauser Inc.
Alabama,University at Birmingham (SPE)
(SPE)
The identification of polymers by FTIR is often
Temperature gradient interaction chromatography (TGIC) complicated by the presence of fillers. However for kaolin
is a conventional reversed phase BPLC technique, but the clay, an FTIR analysis should be able to identify the filler
column temperature is varied during elution. A very fine and predict its concentration using a standard curve. The
and reproducible control of interaction between polymer resulting percentage is more reliable than a simple ash,
chains and the stationary phase can be achieved by changing which may change the chemical composition of the filler.
the column temperature. Under a suitable temperature 2 refs.
programming, this method provides a far superior resolution
USA
to conventional size exclusion chromatography. In addition,
elution in TGIC is more sensitive to molecular weight alone. Accession no.687418
Thus it provides an excellent route to separating branched
polymer molecules of similar hydrodynamic volume but Item 307
differing molecular weight. 8 refs. Polymer Engineering and Science
KOREA; USA 38, No.6, June 1998, p.922-5
Accession no.687496 IDENTIFICATION OF OFF-FLAVOUR
COMPOUNDS IN HDPE WITH DIFFERENT
AMOUNTS OF ABSCENTS
Item 305 Villberg K; Veijanen A; Gustafsson I
Antec ’98. Volume II. Conference proceedings. Jyvaskyla,University; Borealis AB
Atlanta, Ga., 26th-30th April 1998, p.2037-41. 012
MODULATED DIFFERENTIAL SCANNING Details are given of the addition of zeolite to HDPE
CALORIMETRY TO STUDY REACTING drinking water pipes in an attempt to eliminate odours
POLYMER SYSTEMS and to remove odour-causing compounds. The system
Van Mele B; Van Assche G; Van Hemelrijck A used for analysis of volatile organic compounds was a
Brussels,Free University gas chromatographic/mass spectrometric sniffing system.
(SPE) Purge and trap techniques were used to introduce the
volatile, off-flavour components into the gas
Modulated (temperature) differential scanning calorimetry chromatograph. 16 refs.
(MTDSC or MDSC) is used to simultaneously study the
FINLAND; SCANDINAVIA; SWEDEN; WESTERN EUROPE
evolution of heat flow and heat capacity for the isothermal
and non-isothermal reactions of polymer systems. An Accession no.686400
Montpellier,Ecole Nationale Superieure de Chimie; composites. The interaction and chemical reaction of
Talcs de Luzenac SA functional groups in the matrix with functional groups at
the fibrer surface contribute to the adhesion. Direct
By using combined TGA/FTIR thermogravimetric
analysis of the fibre/matrix interface by surface analytical
analysis, accurate real time qualitative and quantitative
methods such as X-ray photoelectron spectroscopy is not
data can be obtained for thermal decomposition of
trivial due to the thickness of a matrix layer over fibres
polymers. It was used to study interactions between an
and the complexity of the matrix system. Indirect analysis
additive and a filler (talc), highlighting a degradation
of the matrix/fibre interface is possible using model
phenomenon of additive by talc, and this phenomenon
compounds which represent functional groups where
depended on the structure and chemical composition of
differences in results are indicative of reaction between
talc. This procedure also applied to analysis of degradation
fibre and matrix. The matrix functional groups that may
of other additives by talc. Thus, polymer formulations
chemically react with the fibre surface can be separated
will rapidly be optimised in various areas of filled
and investigated individually. Mixtures of model
polymers. 12 refs.
compounds can be used to investigate functional groups
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE
reactions between the components, and with the fibre
surface. Model compounds based on epoxy, polyimide,
Accession no.681630
polyphenylene sulphide and vinyl ester matrices are
investigated to characterise the chemical reactions at the
Item 319 fibre/matrix interface. XPS is used to characterise both
Journal of Polymer Science : Polymer Chemistry the carbon fibre surfaces and the reacted carbon fibre
Edition surfaces. The model compounds representative of each
36, No.9, 15th July 1998, p.1363-71 of these matrices demonstrate the range of possible
LIQUID CHROMATOGRAPHY OF reactions and interactions possible between the fibre and
MACROMOLECULES AT THE CRITICAL matrix, ranging from no reaction to distinct chemical
ADSORPTION POINT. II. ROLE OF COLUMN reactions. 4 refs.
PACKING: BARE SILICA GEL USA
Berek D; Janco M; Meira G R Accession no.681439
Slovak,Academy of Sciences; INTEC CONICET
Data are presented manifesting the role of column Item 321
packings from the point of view of both their pore size Cleanrooms
and surface chemistry. Bare silica gels that are the most 12, No.5, Suppl. May 1998, p.S13/20
commonly used LC CAP column packings and model APPLICATION OF FTIR FOR MONITORING
macromolecules, viz. narrow PMMA, were investigated. CLEANROOM AIR AND PROCESS EMISSIONS
20 refs. Zazzera L; Reagen W
ARGENTINA; SLOVAK REPUBLIC; SLOVAKIA 3M Co.
Accession no.681599
The use of FTIR monitoring methods for HAP, VOC, PFC
and HFC emissions for identification and quantification
Item 320 in process exhaust and in clean room air, is discussed. A
20th Annual Anniversary Meeting of the Adhesion summary is included of the various protocols, test methods
Society. Conference proceedings. and references for the use of FTIR spectroscopy to
Hilton Head Island, S.C., 23rd-26th Feb.1997, p.519- generate verifiable data. Results of field trials and
21. 8(10) laboratory study trials are presented, which demonstrate
USING XPS TO INVESTIGATE FIBRE/MATRIX its value as a monitoring method in the semiconductor
CHEMICAL INTERACTIONS AT THE industry
INTERFACE IN CARBON FIBRE REINFORCED USA
COMPOSITES Accession no.679498
Weitzsacker C L; Xie M; Drzal L T
Michigan,State University
Edited by: Drzal L T; Schreiber H P Item 322
(US,Adhesion Society) Analytical Chemistry
70, No.8, 15th April 1998, p.1563-8
With composites expanding into areas from aerospace to POLYMER ANALYSIS BY MICRO-SCALE SIZE-
recreation, different matrices are being investigated to EXCLUSION CHROMATOGRAPHY(SEC)/
tailor composites to specific uses. The degree of adhesion MALDI TIME-OF-FLIGHT MASS
between the fibre and matrix, influenced by chemical SPECTROMETRY WITH A ROBOTIC
reactions, mechanical interactions and topography at the INTERFACE
fibre/matrix interface, has been recognised as a critical Nielen M W F
factor in determining the performance of fibre-reinforced Akzo Nobel Central Research
A report is presented on the development of a micro-scale greatest improvement, while fine grades and talc had little
SEC system in which the MALDI matrix solution is effect. Micrographs revealed the level of interparticle
coaxially added to the column effluent and directly spotted contact and alignment of anisotropic particles which gave
onto the MALDI targets in a robotic interface. Each spot rise to the observed differences. Filler type and content
corresponds to the 10-s elution window from the micro- did not significantly influence shear rheology at the shear
SEC column, thus yielding a narrow polymer distribution rates associated with film extrusion. 17 refs.
which is amenable to characterisation by MALDI mass CANADA; EUROPEAN COMMUNITY; EUROPEAN UNION;
spectroscopy. The performance of the system is UK; USA; WESTERN EUROPE
demonstrated by the characterisation of a polybisphenol Accession no.677503
A carbonate and a complex dipropoxylated bisphenol A/
adipic acid/isophthalic acid copolyester resin. 29 refs. Item 325
EUROPEAN COMMUNITY; EUROPEAN UNION; TAPPI 1997 Polymers, Laminations and Coatings
NETHERLANDS; WESTERN EUROPE Conference. Conference Proceedings. Book 1.
Accession no.679150 Toronto, Ontario, 24th-28th Aug.1997, p.35-44. 012
EFFECT OF TITANIUM DIOXIDE ON
Item 323 EXTRUSION STABILITY
Polymer Engineering and Science Merkley J H
38, No.2, Feb.1998, p.265-73 Eastman Chemical Co.
DSC STUDIES ON THE CRYSTALLISATION (TAPPI)
CHARACTERISTICS OF POLY(ETHYLENE Rheological techniques for following the degradation and
TEREPHTHALATE) FOR BLOW MOULDING changes in molecular weight and MWD of titanium
APPLICATIONS dioxide-filled polyolefins during extrusion coating are
Daw-Ming Fann; Huang S K; Jiunn-Yih Lee examined. These include measurements of the crossover
Taiwan,National University of Science & Technology point between loss modulus and storage modulus and the
The crystallisation behaviour of blow moulded PETP variation in complex viscosity versus frequency curves
bottles, which helps determine the product’s transparency, seen in the rotational mechanical spectrometer curves,
was investigated by DSC dynamic cooling experiments variations in viscosity versus shear rate seen in the
that simulated the cooling that occurs in the injection blow capillary extrusion rheometer curves, and shifts in the
moulding manufacturing process. DSC measurements DMTA curves.
were used to obtain information on related aspects, such CANADA; USA
as the ease of crystallisation from glassy and molten states Accession no.677489
and crystallinity in the products. An Avrami equation was
used for calculation of the crystallisation kinetic Item 326
parameters. 40 refs. Journal of Polymer Science : Polymer Chemistry
TAIWAN Edition
Accession no.678858 36, No.5, 15th April 1998, p.851-60
PEROXIDE INDUCED CROSSLINKING AND
DEGRADATION OF PVC
Item 324
Yu Q; Zhu S; Zhou W
TAPPI 1997 Polymers, Laminations and Coatings
McMaster University
Conference. Conference Proceedings. Book 1.
Toronto, Ontario, 24th-28th Aug.1997, p.173-82. 012 Peroxide induced crosslinking and degradation of PVC
INFLUENCE OF MINERAL FILLERS ON THE were investigated using an on-line ESR technique. The
PROCESSING OF LLDPE FILMS reaction variables included temperature, peroxide type and
Ansari D M; Higgs R P concentration. The mechanism involved in the reaction
ECC International Ltd. was determined base on the radical information. The gel
(TAPPI) content and swelling ratio were also measured. 38 refs.
A study was made of the thermal properties and melt CANADA
rheology of linear LDPE masterbatches filled with Accession no.674965
calcium carbonate, talc and calcined clay. Films were
prepared by extrusion blowing and temperature changes Item 327
were monitored along the bubble. Filler distribution within Journal of Materials Science Letters
the films was assessed by optical and electron microscopy. 17, No.6, 15th March 1998, p.511-3
Rheological properties of the diluted masterbatches were EVIDENCE OF MOLECULAR ORIENTATION IN
evaluated over four decades of shear rate. The mineral POLY(3-BUTYLTHIOPHENE) FILMS BY
fillers increased cooling rates and improved bubble ELECTRON SPIN RESONANCE
stability. Coarser calcium carbonate grades gave the MEASUREMENTS
reported. Depth profiling was carried out using confocal Item 345
Raman microspectroscopy to study polyacrylonitrile/ Applied Spectroscopy
polyvinyl alcohol and polyacrylonitrile/polyacrylic acid 51, No.11, Nov.1997, p.1668-77
laminates. The laminates were annealed at 65, 75 and 90C. RAPID-SCAN TWO-DIMENSIONAL FT-IR: AN
It was demonstrated that the degree of hydrogen bonding EFFICIENT APPROACH TO DYNAMIC
interaction between the nitrile and alcohol groups near INFRARED SPECTROSCOPY
the interfacial region changes between laminates annealed Steeman P A M
at different temperatures. For comparison, Raman DSM Research
mapping of a polyacrylonitrile-polyvinyl alcohol blend
A new and efficient mode of operation is presented that
was used to study the interactions between the polymers
involves a continuous rapid-scan FTIR spectrometer, the
in this (disordered) system. 29 refs.
measurement technique relying completely on the
EUROPEAN COMMUNITY; EUROPEAN UNION;
utilisation of the digital signal processor for data
NETHERLANDS; UK; WESTERN EUROPE
acquisition and manipulation. Experimental and
Accession no.665697 mathematical details were discussed. Application of the
rapid-scan technique was illustrated with some results for
Item 343 a styrene-acrylonitrile/butadiene copolymer. 17 refs.
Applied Spectroscopy EUROPEAN COMMUNITY; EUROPEAN UNION;
51, No.11, Nov.1997, p.1741-4 NETHERLANDS; WESTERN EUROPE
CHARACTERISATION OF DENTURE ACRYLIC Accession no.665692
RESIN SURFACES MODIFIED BY GLOW
DISCHARGES
Item 346
Suzer S; Ozden N; Akaltan F; Akovali G
Applied Spectroscopy
Bilkent,University; Ankara,University; Middle
51, No.11, Nov.1997, p.1593-6
East,Technical University
RAMAN IMAGING OF DENTAL ADHESIVE
Resin samples prepared by compression moulding using DIFFUSION
a PMMA denture base material were exposed to radio Wieliczka D M; Kruger M B; Spencer P
frequency glow discharges to improve the wettability of Missouri,University
the material. FTIR reflectance, X-ray photoelectron
Using micro-Raman spectroscopy, chemical and
spectroscopy and contact angle measurements were used
morphological information on the dentin/adhesive
to characterise the changes introduced by the glow
interface was collected with minimal sample preparation.
discharge plasma. 18 refs.
Results provided direct evidence of an adhesive
TURKEY
preparation and demineralisation depth for two adhesive
Accession no.665695 systems. 17 refs.
USA
Item 344 Accession no.665691
Applied Spectroscopy
51, No.11, Nov.1997, p.1736-40
Item 347
GENERALISED TWO-DIMENSIONAL FOURIER
Injection Molding
TRANSFORM INFRARED PHOTOACOUSTIC
5, No.12, Dec. 1997, p.44-5
SPECTRAL DEPTH-PROFILING ANALYSIS
MATERIALS ANALYST: PART 3. LOT-TO-LOT
Jiang E Y; McCarthy W J; Drapcho D L; Crocombe R
VARIATION
A
Sepe M
Bio-Rad Laboratories Inc.
Dickten & Masch Mfg.Co.
A new application of generalised two-dimensional
The use is examined of thermogravimetric analysis as an
correlation spectroscopy in photoacoustic depth-profiling
analytical tool for the diagnosis of part failure in injection
analysis. Both rapid-scan and step-scan photoacoustic
moulding. The consistent performance of an ethylene
spectroscopy (obtained by using the software-based
vinyl acetate copolymer was evaluated and the need to
digital signal processing technique) of multilayer samples
separate the component parts of the material to test for
were used to calculate generalised two-dimensional
the amount of vinyl acetate in the compound is discussed
correlation maps. Advantages of this unambiguous
in order to develop a thermal history. Once this history is
analysis method in enhancing spectral as well as depth
established, a customer can institute an incoming QC test
resolutions, over conventional two-dimensional
on the material’s composition rather than by adjusting
correlation and other spectral depth-profiling methods,
the process for each new lot and performing product
were discussed. 31 refs.
testing after the parts have been produced.
USA
USA
Accession no.665694
Accession no.664180
the different chemical bondings in agreement with X-ray OF POLYETHYLENE AND N-ALKANES
absorption near-edge spectroscopy experiments is Parker S F
proposed. 14 refs. Rutherford Appleton Laboratory
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
High quality inelastic neutron scattering (INS) spectra of
WESTERN EUROPE
randomly oriented polycrystalline PE, polydeutero-
Accession no.653745
polyethylene and highly oriented polyethylene are
presented and a number of new features described. 9 refs.
Item 359 EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Macromolecular Symposia WESTERN EUROPE
Vol.119, July 1997, p.309-15 Accession no.653736
CARBON-13, MAGNESIUM-25 AND BORON-11
SOLID STATE NMR STUDY OF A FIRE
Item 362
RETARDED ETHYLENE-VINYL ACETATE
Macromolecular Symposia
COPOLYMER
Vol.119, July 1997, p.157-64
Pecoul N; Bourbigot S; Revel B
INFRARED ABSORPTION SPECTRA OF
Ecole Nationale Superieure de Chimie de Lille; Centre
POLYMERS FROM CLASSICAL MOLECULAR
Commun de Mesures RMN
SIMULATION
Flame retardance of ethylene-vinyl acetate copolymer can Soldera A; Dognon J P
be achieved using magnesium hydroxide incorporated in CEA/Le Ripault
the polymeric matrix. The adduct of a small amount of
A method is proposed to predict the IR spectra of
zinc borate as synergistic agent in the formulation
amorphous polymers. Based on classical molecular
increases the fire-proofing properties. Multinuclei solid-
state NMR appears as a means to characterise materials simulation and Kramers-Kronig relations, it allows the
before and after combustion. It was shown that computations of absorption and transmittance spectra of
endothermic dehydration, water vapour evolved and polymer films in near and middle infra-red domains with
formation of a glassy coating provided the flame good agreement with experimental data. 22 refs.
retardancy of interest to the polymer matrix. 12 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE Accession no.653730
Accession no.653744
Item 363
Item 360 Macromolecular Symposia
Macromolecular Symposia Vol.119, July 1997, p.79-87
Vol.119, July 1997, p.269-76 CREEP RATE SPECTROSCOPY USING A LASER
QUANTITATIVE ATR-FTIR SPECTROSCOPY AT INTERFEROMETER AS ULTRA-HIGH
POLYMER SURFACES: SORPTION AND RESOLUTION TECHNIQUE FOR STUDY OF
MOLECULAR CONFORMATION RELAXATIONS
Mueller M; Schmitt F J Peschanskaya N N; Yakushev P N; Sinani A B;
Dresden,Institute of Polymer Research Bershtein V A
Russian Academy of Sciences
Adsorption and diffusion phenomena at or within polymer
systems were investigated by surface sensitive ATR-FTIR An original laser interferometry creep rate spectroscopy
spectroscopy. For a systematic description, a study was (CRS) method was developed and used as the low-
made of (1) the competitive adsorption and desorption frequency and high-resolution technique for studying
behaviour of proteins on polymer surfaces, (2) swelling microplasticity and relaxations in different materials
of hydrophilic polymers by water molecules, which can including brittle ones. New possibilities for CRS for
be accompanied by conformational changes, and (3) polymers are demonstrated. 13 refs.
induced orientational changes of hydrophobically RUSSIA
modified polypeptides by apolar solvents. 10 refs. Accession no.653722
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE
Item 364
Accession no.653740 Macromolecular Symposia
Vol.119, July 1997, p.49-63
Item 361 POTENTIAL OF TWO-DIMENSIONAL NEAR-
Macromolecular Symposia INFRARED CORRELATION SPECTROSCOPY
Vol.119, July 1997, p.227-34 IN STUDIES OF PRE-MELTING BEHAVIOUR OF
INELASTIC NEUTRON SCATTERING STUDIES NYLON 12
MOLECULAR WEIGHT OF POLYETHYLENE interpretation methods were applied to the data. The wide
GLYCOLS BY VAPOR PRESSURE temperature range used in this work (45-580C)
OSMOMETRY: AN ALTERNATIVE DATA encompassed a change in the decomposition mechanism
TREATMENT and this greatly limited the utility of the methods. To
Sabadini E; Assano E M; Atvars T D Z accommodate this mechanism change, the data were
Campinas,Universidade Estadual treated as a pseudo-first order reaction. The lower
activation energy occurring at lower degradation
The number-average molec.wt. of some polyethylene
temperatures was attributed to scission of the ‘weak links’
glycols was analysed using vapour pressure osmometry.
in the polymer. The higher activation energy was similar
This technique generally worked with a plot of the
to the carbon-carbon dissociation energy and was
difference in electrical resistance/concentration versus
associated with random scission throughout the polymer.
concentration and the molec.wt. was determined by the
47 refs.
calibration constant obtained from the curve intercept. It
CANADA
was demonstrated that this method induced a high
dispersion of the data, which could be minimised using a Accession no.645116
plot of difference in electrical resistance versus
concentration.. More precise values of molec.wt. could Item 381
thus be obtained and the number-average molec.wt. of Polymer Degradation and Stability
several polyethylene glycols could be directly obtained 57, No.2, 1997, p.113-25
from the ratio between the curve slopes obtained for a THERMAL DEGRADATION KINETICS OF
standard and the polymer sample. 10 refs. POLYPROPYLENE. I. MOLECULAR WEIGHT
BRAZIL DISTRIBUTION
Accession no.645677 Chan J H; Balke S T
Toronto,University
Item 379 A kinetic model for the thermal degradation of PP was
Speciality Chemicals developed and fitted to MWD data obtained by high
17, No.5, June/July 1997, p.165/70 temperature size exclusion chromatography. In a series
MAKING LIQUID CHROMATOGRAPHY MORE of ampoule experiments, reaction temperatures of 275-
ACCESSIBLE 315C were examined with reaction times of up to 48 h. A
Kuehler T C; Sellen M; Lavold T; Batt J; Langridge J; single-parameter version of the model, containing an
Raso R; Rontree J A apparent rate constant, was found to provide excellent
Astra Hassle AB; Micromass AB; Micromass UK Ltd. fits of all MWDs. Values of the parameter varied with
Until recently, mass spectrometry was regarded as a highly both temperature and reaction time. 35 refs.
sophisticated technique requiring careful use of the CANADA
instrument by a sole operator, and demanding meticulous Accession no.645114
sample preparation by the chemist. However, moves
towards open-access, chemist-operated systems have been
Item 382
reported on mass spectrometers equipped with a variety
Analytical Chemistry
of ionisation modes. The reliability and robustness of
69, No.13, 1st July 1997, p.2485-95
atmospheric pressure ionisation, the ease and speed of
MASS SPECTROMETRIC INVERSE GAS
source tuning, the fact that it is unnecessary to optimise
CHROMATOGRAPHY: INVESTIGATION OF
the source conditions for each sample individually and
POLYMERIC PHASE TRANSITIONS
the reproducibility of results have made API techniques
Panda S; Bu Q; Huang B; Edwards R R; Liao Q; Yun K
the ionisation methods of choice. Details are given. 5 refs.
S; Parcher J F
EUROPEAN COMMUNITY; EUROPEAN UNION;
SCANDINAVIA; SWEDEN; UK; WESTERN EUROPE Mississippi,University
Accession no.645281 An improved inverse gas chromatographic method
involving the use of a mass-specific detector for
Item 380 determination of the Tg of polymeric materials is
Polymer Degradation and Stability described. This new method allows the use of several
57, No.2, 1997, p.135-49 probe solutes simultaneously with an automated, closed-
THERMAL DEGRADATION KINETICS OF loop injector and stepped temperature programming. The
POLYPROPYLENE. III. result is a single continuous chromatogram for each probe
THERMOGRAVIMETRIC ANALYSIS solute over a range of temperatures encompassing the Tg.
Chan J H; Balke S T Several different methods for the exact determination of
Toronto,University Tg from the chromatogram were investigated. Two new
methods were also proposed for the evaluation of Tg from
Thermogravimetric data were obtained for the pyrolysis
either the temperature dependence of the second moments
of polypropylene, and several previously published
of the elution peaks for probe solutes or simple inspection When coupled with an automated mapping stage, it can
of the variation of elution peak height (width) with offer unique evaluation capabilities. A number of
temperature. 51 refs. applications of FTIR spectroscopy mapping to the vinyl
USA siding industry are described. Examples focus on
Accession no.645093 determining, in single sample mapping experiments, the
compositional changes associated with capstock to
substrate transition and evaluating the degradation species
Item 383 and level observed during weathering exposure
Analytical Chemistry throughout the thickness of the siding panel. 4 refs.
69, No.12, 15th June 1997, p.15R-28R
USA
COATINGS
Anderson D G Accession no.639927
Witco Corp.
Item 386
A review is presented of analytical techniques applicable
Antec 97. Volume II. Conference proceedings.
to the examination of coatings, raw materials and
Toronto, 27th April-2nd May 1997, p.2310-4. 012
substrates since 1995. The most highly referenced areas
QUANTITATIVE ANALYSIS OF LDPE/LLDPE
were found to be IR spectroscopy, NMR, HPLC, thermal
BLEND USING DSC AND FTIR METHODS
analysis and gas chromatography. 704 refs.
Prasad A; Mowery D
USA
Quantum Chemical Co.
Accession no.640310 (SPE)
A blend of LDPE and LLDPE is widely used for blown
Item 384 film applications. For quality control an accurate and rapid
Polymer Bulletin method is required to identify the type and composition
38, No.6, June 1997, p.681-8 of alpha-olefin in an LDPE/LLDPE blend. A rapid,
SEPARATION OF BLOCK COPOLYMERS FROM accurate and new test method is developed which utilises
PARENT HOMOPOLYMERS BY MEANS OF DSC and FTIR techniques. The melting point of LDPE
LIQUID CHROMATOGRAPHY AT THE varies with density and usually is in the range of 106 deg.C
CRITICAL ADSORPTION POINT to 112 deg.C for film grade resins. The DSC thermogram
Janco M; Berek D; Onen A; Fischer C H; Yagci Y; of LLDPE is characterised by a broad range of melting
Schnabel W with a lower melting peak around 106 deg.C to 110 deg.C
Slovak Academy of Sciences; Istanbul,Technical and a higher one in the range of 120 deg.C to 124 deg.C.
University; Hahn-Meitner-Institut Berlin GmbH In the blend with LDPE, the ratio of the two endothermic
The principle underlying the above method is described peak heights changes. At a given weight percent of LDPE,
and results of its application to block copolymers this ratio depends on the type of LLDPE. The separate
consisting of methyl methacrylate and tetrahydrofuran calibrations for butene-1, hexene-1, and octene-1 LLDPEs
blocks are presented and discussed. The technique is are developed to quantify the blend composition from
shown to be suitable for characterisation of block DSC thermograms provided the alpha-olefin type is
copolymers with regard to the presence of homopolymer identified by a rapid method such as FTIR. 17 refs.
and multiblock (triblock) fractions. 5 refs. USA
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; Accession no.638387
SLOVAK REPUBLIC; SLOVAKIA; TURKEY; WESTERN
EUROPE
Accession no.640169 Item 387
Shawbury, Rapra Technology Ltd., 1992, pp.112. 12ins.
30/6/97. Rapra Review Rept. No.61, Vol.6, No.1, 1992.
Item 385 FOOD CONTACT POLYMERIC MATERIALS
Antec 97. Volume III. Conference proceedings. Sidwell J
Toronto,27th April-2nd May 1997,p.3588-92. 012 Rapra Technology Ltd.
FOURIER TRANSFORM INFRARED MICRO Edited by: Dolbey R
SPECTROSCOPY MAPPING. APPLICATIONS (Rapra Technology Ltd.)
TO VINYL SIDING INDUSTRY Rapra Review Report No.61
Garcia D; Black J
Elf Atochem North America Inc. A review is presented of the current and proposed
(SPE) European legislation on materials in contact with food,
as well as the latest technological advances. With
Fourier transform IR (FTIR) spectroscopy is a powerful reference to legislation, details are given of EC directives
analytical technique capable of yielding high quality issued, their implementation, FDA regulations, recycling
information with a spacial resolution as low as 10 microns. and waste management legislation. Technical
developments in food contact materials cover barrier 5, No.3, March 1997, p.97-102
polymers in multilayer packaging films, migration of CHARACTERISATION OF POLYMER BLENDS
species from food contact materials, and methods of BY INVERSE GAS CHROMATOGRAPHY
analysis of multilayer food contact materials. 485 refs. Al-Saigh Z Y
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Ohio,State University
WESTERN EUROPE
A brief review is presented of the use of inverse gas
Accession no.637749 chromatography to characterise polymer blends.
Comparisons between data from inverse gas
Item 388 chromatography and DSC are discussed. 23 refs.
Polymer
USA
38, No.12, 1997, p.3035-43
CHARACTERIZATION OF POLYETHYLENE Accession no.632110
TEREPHTHALATE AND POLYETHYLENE
TEREPHTHALATE BLENDS Item 391
Fox B; Moad G; van Diepen G; Willing I; Cook W D Polymer News
CSIRO,Div.of Chemicals & Polymers; 22, No.1, Jan.1997, p.15
Monash,University POLYMER ANALYSIS AND
CHARACTERISATION. SOLID STATE NMR: IS
A method was developed for direct determination of the
IT BECOME TRULY POPULAR?
molec.wt. of the PETP component in PETP/ABS blends
Garbassi F
by GPC. The technique was used to demonstrate that an
EniChem SpA
observed deterioration in the mechanical properties, e.g.
Izod impact strength, of PETP/ABS blends on processing A very brief review is presented of specific areas where
could be correlated with a decrease in the molec.wt. of solid state NMR can contribute to polymer analysis.
the PETP component. Various methods for evaluating the Mention is made of polymer morphology, interactions,
molec.wt. and the chemical microstructure of PETP were dynamics and polymer reactions. 10 refs.
examined. The use of NMR spectroscopy as a means of EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
quantitatively identifying end groups and comonomers WESTERN EUROPE
that were present at the 1-4% level in commercial PETP Accession no.632071
was critically evaluated with reference to the stability of
PETP and PETP end groups in various NMR solvents.
Item 392
New proton NMR chemical shift assignments for
Analytical Chemistry
cyclohexanedimethanol units are presented and the
69, No.4, 15th Feb.1997, p.618-22
reactivity of hydroxy end groups in trifluoroacetic acid
COMPOSITION AND MICROSTRUCTURE
mixtures is examined. 34 refs.
ANALYSIS OF CHLORINATED
AUSTRALIA
POLYETHYLENE BY PYROLYSIS GAS
Accession no.636573 CHROMATOGRAPHY AND PYROLYSIS GAS
CHROMATOGRAPHY/MASS SPECTROMETRY
Item 389 Cheng-Yu Wang F; Smith P B
Polymer Testing Dow Chemical Co.
16, No.2, 1997, p.193-8 A pyrolysis gas chromatography method was developed
NMR CARBON-13 HIGH RESOLUTION STUDY to determine the composition and microstructure of
OF POLY(ETHYLENE-CO-VINYL ACETATE) chlorinated PE (CPE). The method used specific aromatic
Stael G C; Tavares M I B compounds which were formed through
CCT/UENF dehydrochlorination of trimers after pyrolysis of CPE
EVA was analysed by carbon-13 high-resolution using polymers at elevated temperatures. The composition and
NMR employing solution and solid state techniques. The microstructure calculation was based on the difference
analyses of this copolymer by solution NMR permitted between the levels of ethylene and vinyl chloride trimers
the copolymer composition to be obtained, and using formed. The composition of CPE polymers used in this
solid-state NMR, a study of molecular mobility was study was corroborated with carbon-13 NMR results and
carried out. Both studies were made to correlate the the manufacturers product specification. 23 refs.
structure and properties. 9 refs. USA
BRAZIL Accession no.629089
Accession no.634101
Item 393
Item 390 Biomaterials
Trends in Polymer Science 18, No.5, March 1997, p.415-9
DETECTION OF PEROXY SPECIES IN ULTRA- compared for THF/carbon dioxide and other common liquid
HIGH MOLECULAR WEIGHT mixtures. As enhanced-fluid liquids were highly
POLYETHYLENE BY RAMAN SPECTROSCOPY compressible, it was possible to reach the critical condition
Chenery D H by changing the pressure of the THF/carbon dioxide
Smith & Nephew Group Research Centre mixture. Approaching the critical condition by pressure
variation was compared with that possible with temp.
Samples of gamma-sterilised UHMWPE were examined
changes. Pressure variation was a more accurate and
using infra-red and Raman spectroscopies. The purpose
reproducible means of reaching the critical condition than
of this study was to detect the peroxy intermediates by
temp. variation. Finally, THF/carbon dioxide mixtures were
the novel use of Raman spectroscopy to confirm that
used as mobile phases at the critical condition for PS to
oxidation proceeded by this mechanism. 16 refs.
characterise styrene-methyl acrylate copolymers. 25 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE USA
Item 396
Item 394 Shawbury, Rapra Technology Ltd., 1995, pp.108. 12ins.
Polymer 18/7/95. Rapra Review Rept. Vol.7, No.11, 1995,
38, No.1, 1997, p.1-7 MOLECULAR WEIGHT CHARACTERISATION
MODULATED DIFFERENTIAL SCANNING OF SYNTHETIC POLYMERS
CALORIMETRY: 6. THERMAL Holding S R; Meeham E
CHARACTERISATION OF MULTICOMPONENT Rapra Technology Ltd.; Polymer Laboratories Ltd.
POLYMERS AND INTERFACES Edited by: Dolbey R
Hourston D J; Song M; Hammiche A; Pollock H M; (Rapra Technology Ltd.)
Reading M Rapra Review Report No. 83
Loughborough,University of Technology;
Lancaster,University; ICI Paints Techniques are examined for the determination of the
molecular weight distribution and molecular weight averages
A quantitative thermal method, based on the differential of synthetic polymers. The use is discussed of gel permeation
of heat capacity signal from modulated temperature chromatography in combination with other techniques such
differential scanning calorimetry, was described for as light scattering and viscometry to provide information
determining the weight fraction of interface and the extent about the molec.wt. of a polymer and potentially significant
of phase separation in polymer materials. The interface information on the composition of copolymers and blends.
was modelled as discrete fractions, each with its own The use of solution viscosity is also examined as a valuable
characteristic increment of heat capacity. The materials quality control technique. 411 refs.
used to demonstrate the range of the method were PS
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
blended with poly(phenylene oxide) (PPO), pure PS, pure WESTERN EUROPE
PPO, a styrene-isoprene-styrene triblock copolymer (SIS),
Accession no.556661
SIS blended with PPO, PMMA/poly(vinyl acetate) blends
and PVC sandwiched with poly(n-butyl acrylate). Two-
Item 397
phase and four-phase systems were used. The calculated
Analytical Chemistry
results agreed well with experimental results for two- and
60,No.9,1st May 1988,p.932-7
four-phase systems. 20 refs.
IDENTIFICATION OF DYES IN SOLID
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
POLYMETHYL METHACRYLATE BY MEANS
OF LASER DESORPTION FOURIER
Accession no.621625
TRANSFORM ION CYCLOTRON RESONANCE
MASS SPECTROMETRY
Item 395 Hsu A T;Marshall A G
Analytical Chemistry OHIO STATE,UNIVERSITY
69, No.1, 1st Jan.1997, p.66-71
It is demonstrated that the above technique can detect and
LIQUID CHROMATOGRAPHY AT THE
identify (by chemical formulae) dyes in solid PMMA
CRITICAL CONDITION USING ENHANCED-
commercial plastics at concentrations at least on order of
FLUIDITY LIQUID MOBILE PHASES
magnitude lower (0.1% vs 1-2wt%) than those obtained
Souvignet I; Olesik S V
by the best currently-available alternative method (ATR
Ohio,State University
Fourier transform IR spectrometry). Both untreated and
The use of enhanced-fluidity liquid mixtures of THF and redissolved PMMA can be characterised, in the presence
carbon dioxide for liquid chromatography at the critical and absence of up to three dyes in a single sample. 44 refs.
condition was examined. For PS polymers, the molec.wt. USA
range that could be analysed at the critical condition was Accession no.357996
Item 398 processing aids are presented. Over 1300 IR spectra and
Oxford, Pergamon Press Ltd., 1984, pp.ix,445. 60 UV spectra are included. The functions and
LS.24.50. 9ins. 2copies. 12/7/85. Analytical Chemistry compositions as well as the physical and chemical
Vol.8. 91T methods of identification of the following materials are
ANALYSIS OF PLASTICS discussed: plasticisers, fillers, pigments, antioxidants, UV
Crompton T R stabilisers, optical brighteners, antistatic agents,
biostabilisers, flame retardants, lubricants, accelerators,
This book covers all aspects of the analysis of plastics by
hardeners and blowing agents. 608 refs.
chemical and physical methods. It is divided into eight
chapters which each deal with a particular polymer or Accession no.211056
group of polymers:- polyolefins, polypropylene, higher
alkene polymers, styrene polymers, chlorine-containing Item 400
polymers, methacrylates, polybutadienes, polyesters and Members Rept.49 Shawbury, 1980, pp.12. 12ins.
polyethers. The techniques discussed include 2copies. 26/6/80. 91T
spectroscopy, chromatography, fractionation,, X-ray HIGH PERFORMANCE LIQUID
diffraction, autoradiography, DTA, TGA and DSC. CHROMATOGRAPHY - ANALYTICAL
UK APPLICATIONS IN THE RUBBER AND
Accession no.280400 PLASTICS INDUSTRIES
Sidwell J A
Rubber & Plastics Research Assn.of Gt.Britain
Item 399
RUBBER & PLASTICS RA.MEMBERS REPT.049
Weinheim, Verlag Chemie GmbH, 1981, pp.XV,687.
12ins. 22/3/82. R.ROOM. 91T This report details some of the high-performance liquid
ATLAS OF POLYMER AND PLASTICS chromatography work carried out at RAPRA and reviews
ANALYSIS. VOL.3....ADDITIVES AND reported in the literature. 11 refs.
PROCESSING AIDS: SPECTRA AND METHODS RUBBER & PLASTICS RESEARCH ASSN.OF
OF IDENTIFICATION. 2ND REV.EDN. GT.BRITAIN
Scholl F Accession no.154074
The spectroscopic and chromatographic data that are
required for the identification of plastics additives and
Subject Index
A ALKYD RESIN, 237 BAND STRUCTURE, 262
ALPHA TRANSITION, 245 290 BARIUM SULPHATE, 40
ABS, 160 164 207 225 345 365 388 328 BARRIER PROPERTIES, 56 57 86
398 ALUMINIUM, 126 168 179 223 266 94 168 387
ABSORPTION, 56 226 297 306 374 ALUMINIUM HYDROXIDE, 211 BENZENE, 382
382 ALUMINIUM OXIDE, 6 BETA RELAXATION, 325
ABSORPTION SPECTRA, 274 AMINE, 36 48 130 151 161 178 272 BIAXIALLY ORIENTED, 104
ABSORPTION SPECTROSCOPY, AMMONIUM PYRROLIDONE BIOCOMPATIBLE, 42
358 362 DITHIOCARBAMATE, 351 BIODEGRADABLE, 37 112 267
ACCELERATOR, 399 AMMONIUM SALT, 258 387
ACCURACY, 131 AMORPHOUS, 14 54 74 78 99 117 BIODETERIORATION, 5 37 112
ACETIC ACID, 76 266 141 170 207 213 274 283 340 246 267 387
ACETONE, 185 224 266 311 362 367 BIOMATERIAL, 42 46 246 262
ACETONITRILE, 21 266 ANISOTROPY, 13 256 324 BIOMEDICAL APPLICATION,
ACID, 277 288 ANNEALING, 24 54 74 101 135 262
ACOUSTIC MICROSCOPY, 126 136 277 308 338 342 BIREFRINGENCE, 257 284
ACRYLATE, 269 ANTI-STICK AGENT, 6 BISPENTAMETHYLPIPERIDYL
ACRYLIC, 199 ANTIMONY, 95 SEBACATE, 66
ACRYLIC ACID COPOLYMER, ANTIOXIDANT, 65 86 93 107 132 BISPHENOL A, 200 222 272 356
172 217 348 171 183 195 286 288 366 368 BISPHENOL A COPOLYMER,
ACRYLIC POLYMER, 33 172 255 372 387 399 189
299 314 335 371 384 397 ANTISTATIC AGENT, 399 BISPHENOL A DIGLYCIDYL
ACRYLIC-MELAMINE RESIN, 44 AQUEOUS, 46 198 223 232 ETHER, 178
175 ARAMID FIBRE, 281 BISPHENOL A EPOXY RESIN,
ACRYLONITRILE, 119 AROMA, 56 57 11
ACRYLONITRILE COPOLYMER, AROMATIC, 48 125 192 278 288 BISPHENOL A
57 299 392 POLYCARBONATE, 4 29 78
ACRYLONITRILE-STYRENE ATMOSPHERIC PRESSURE, 50 135 159 322 367
COPOLYMER, 72 110 220 345 206 222 BISPHENOL DIGLYCIDYL
ACTIVATION ENERGIES, 49 75 ATOMIC ABSORPTION ETHER, 178
146 169 280 288 317 328 380 SPECTROSCOPY, 177 BLEND, 11 12 15 25 47 58 60 63
381 ATOMIC EMISSION 64 69 72 77 91 98 107 110 112
ADDITIVE, 29 36 71 89 99 107 108 SPECTROSCOPY, 95 177 218 125 137 139 146 147 151 156
112 124 128 132 151 161 171 273 351 186 188 193 209 213 220 228
178 181 199 201 206 225 226 ATOMIC FORCE MICROSCOPY, 234 246 309 331 340 347 348
250 272 288 289 302 306 318 30 38 44 58 59 62 108 115 118 363 367 375 377 386 388 390
324 325 353 366 372 377 387 142 145 154 167 179 191 219 391 394
391 397 399 277 BLOCK COPOLYMER, 127 193
ADHESION, 32 61 62 145 157 167 ATTENUATED TOTAL 274 354 370 384 394
176 202 223 231 236 237 247 REFLECTANCE BLOW MOULDING, 313 323
249 312 316 341 346 SPECTROSCOPY, 43 61 69 126 BLOWING AGENT, 302 399
ADHESIVE, 9 20 62 167 168 179 257 262 301 360 BLOWN FILM, 324 386
272 346 AUGER ELECTRON BODY ARMOUR, 281
ADSORPTION, 46 56 65 93 103 SPECTROSCOPY, 13 BOILING POINT, 120 185 266
178 203 210 221 241 285 319 AUTOMATION, 46 50 212 278 382 BONDING, 32 168 202
339 360 384 AUTOMOTIVE APPLICATION, 44 BONDING AGENT, 168 179
ADSORPTION 56 62 67 175 202 212 236 329 BONNET, 329
CHROMATOGRAPHY, 105 210 AUTOOXIDATION, 169 BOTTLE, 57 131 212 266 313 323
AEROPLANE, 36 62 121 BOUND WATER, 51
AFFINITY CHROMATOGRAPHY, BOUNDARY LAYER, 81
50 97
B BRANCHING, 18 35 60 102 200
AGEING, 66 80 86 88 112 148 152 BACKSCATTERED ELECTRON 216
274 288 298 309 338 377 IMAGING, 289 BRITTLE, 41 62 271 289 357 363
ALCOHOL, 56 235 288 BAG, 266 BROMINE CONTAINING
ALCOHOLYSIS, 39 BAGASSE, 100 COPOLYMER, 273
FILLER, 17 43 45 65 81 90 93 184 FRACTURE, 67 82 98 178 236 149 155 161 163 164 170 179
207 211 226 289 306 307 318 271 289 207 213 220 249 261 269 280
324 325 399 FRACTURE MORPHOLOGY, 2 282 287 290 305 308 309 323
FILLER CONTENT, 81 90 324 13 54 61 98 115 191 319 346 328 338 357 367 377 382 390
FILLER DISTRIBUTION, 289 324 391 394 394
FILM, 1 3 16 27 37 38 40 41 49 56 FREE ENERGY, 339 GLOW DISCHARGE, 343
57 61 62 65 86 92 102 104 106 FREE RADICAL, 45 266 GLOW DISCHARGE
115 117 118 135 142 148 156 FREE VOLUME, 18 56 99 338 SPECTROSCOPY, 202
167 168 186 205 246 257 262 367 382 GRAVIMETRIC ANALYSIS, 23
266 269 288 289 308 324 327 FREEZING POINT, 324 82 85 93 94 152 189 196 211
349 351 362 373 374 386 387 FREQUENCY, 78 118 179 255 256 244 258 296 317 347 377 380
FINITE ELEMENT ANALYSIS, 287 309 325 336
108 FUEL TANK, 56
FIRE RETARDANT, 359 FUNCTIONAL GROUP, 36 83 274
H
FLAME IONISATION, 185 331 HEADSPACE ANALYSIS, 311
FLAME RETARDANT, 95 152 FUNGUS, 5 HEADSPACE
211 218 273 FURAN RESIN, 199 CHROMATOGRAPHY, 185
FLAMMABILITY, 150 173 273 FURNITURE, 274 HEAT CAPACITY, 20 74 78 125
359 161 179 220 253 261 276 280
FLASH CHROMATOGRAPHY,
97
G 287 290 309 324 336 394
HEAT DEGRADATION, 23 26 29
FLASH PYROLYSIS, 4 GAMMA-IRRADIATION, 4 99 75 76 83 152 160 163 189 192
FLAVOUR, 183 133 393 194 196 244 266 273 318 325
FLEXIBLE, 84 277 283 353 GAS, 67 80 277 311 380 381
FLOATATION, 97 GAS BARRIER, 56 57 168 HEAT FLOW, 36 155 245 252 261
FLOW INJECTION ANALYSIS, GAS CHROMATOGRAPHY, 3 4 276 309 324
50 30 34 39 53 56 66 71 72 75 76 HEAT INSULATION, 80 276
FLOW MICROCALORIMETRY, 80 81 84 87 90 96 107 112 119 HEAT RESISTANCE, 11 24 26 57
93 120 124 128 132 141 143 160 85 126 163 196 228 266 267
FLOW RATE, 50 143 233 324 372 174 183 185 186 191 194 195 269 295 317 377
FLUORESCENCE, 17 293 198 208 217 218 221 232 235 HEAT STABILITY, 146 196
FLUORESCENCE 250 270 273 278 303 307 311 HEAT TREATMENT, 57 119
SPECTROSCOPY, 108 116 157 339 349 353 373 382 383 390 HEATING, 36 179 187 244 266
FLUOROPOLYMER, 279 387 392 398 309 323 348 354
FOAM, 80 84 97 302 GAS DIFFUSION, 274 HEATING RATE, 36 54 144 179
FOOD-CONTACT GAS LIQUID 309 328 332 348 380
APPLICATION, 124 177 195 CHROMATOGRAPHY, 97 HELIUM, 57
208 264 286 387 GAS-PHASE, 67 80 277 311 HETEROGENEITY, 25 217 268
FOOD PACKAGING, 57 124 168 GAS PIPE, 277 HETEROGENEOUS, 129 146 170
195 266 278 311 GAS TRANSMISSION, 311 HEXANE, 240 319
FORMULATION, 30 108 164 174 GEL, 46 319 326 HIGH DENSITY
217 312 GEL ELECTROPHORESIS, 97 POLYETHYLENE, 52 56 57 63
FOURIER TRANSFORM GEL PERMEATION 87 91 102 109 112 128 132 143
INFRARED SPECTROSCOPY, CHROMATOGRAPHY, 50 107 164 195 212 214 307 357 372
1 3 6 8 11 24 25 26 29 30 34 36 113 137 152 169 172 190 200 392
40 41 60 63 64 72 77 83 88 92 233 259 264 295 310 325 334 HIGH IMPACT PS, 48
93 94 98 102 107 108 113 117 356 376 383 388 396 399 HIGH PERFORMANCE LIQUID
126 135 136 150 153 156 160 GELATION, 7 73 134 161 294 CHROMATOGRAPHY, 21 35
161 163 165 169 170 173 181 GLASS, 145 167 276 351 39 46 76 97 165 171 183 195
189 190 213 215 216 226 228 GLASS CONTENT, 296 200 222 233 238 239 242 247
246 249 250 252 259 262 264 GLASS FIBRE, 76 176 197 264 266 286 304 337 366 375
271 274 275 277 288 300 306 GLASS FIBRE-REINFORCED 383 399 400
309 316 318 321 328 341 343 PLASTIC, 17 179 202 211 231 HIGH TEMPERATURE, 62 107
344 345 352 360 364 374 381 271 288 296 333 277 381
385 386 397 GLASS TRANSITION HIGH RESOLUTION, 179 209
FRACTION, 35 170 204 394 TEMPERATURE, 12 15 18 20 289 340 354 363 389
FRACTIONATION, 28 52 97 107 29 36 49 51 56 74 77 81 85 94 HINDERED AMINE, 3 31 66 123
113 337 370 398 101 106 110 114 117 122 135 225
HINDERED PHENOL, 41 250 256 257 259 262 264 269 KEVLAR, 191
HIP JOINT, 42 271 274 275 277 284 294 297 KINETIC, 8 10 45 73 83 125 377
HOMOGENEITY, 100 289 340 301 306 316 318 321 328 341 KINETICS, 3 23 52 73 75 94 144
HOT STAGE MICROSCOPY, 2 343 344 345 353 360 362 364 149 302 317 323 332 363 380
181 365 371 374 381 383 385 386 381
HUMIDITY, 44 56 57 309 387 393 399
HYDROFLUOROCARBON, 321 INFRARED THERMOGRAPHY,
HYDROGEN BONDING, 77 94 67
L
99 114 342 364 INJECTION MOULDING, 67 160 LAC RESIN, 352
HYDROGEN CHLORIDE, 34 48 231 296 357 LACQUER, 185
194 228 INK, 239 LAMELLAE, 78 139
HYDROLYSIS, 34 58 59 165 319 INSULATION, 80 276 LAMINATE, 56 57 168 182 266
341 352 INTERACTION, 90 167 178 235 342
HYDROPHILICITY, 46 51 360 249 285 311 318 341 342 364 LAMINATED FILM, 57 168 266
HYDROPHOBICITY, 37 46 360 INTERACTION PARAMETER, 293
375 220 235 285 LANGIVIN EQUATION, 3 46 50
HYDROXYBENZENE, 75 297 INTERCHAIN PACKING, 135 60 75
300 INTERFACE, 178 179 182 206 229 LASER, 62 212 236 298 351 397
HYDROXYETHYL 236 322 341 342 346 367 394 LASER INDUCED
METHACRYLATE INTERFACIAL ADHESION, 333 DECOHESION
COPOLYMER, 46 INTERFACIAL DEBONDING, 167 SPECTROSCOPY, 236
HYDROXYL GROUP, 36 69 INTERFACIAL INTERACTION, LASER INTERFEROMETRY, 363
90 167 178 LASER IONISATION MASS
INTERFACIAL PROPERTIES, 81
I 90 111 141 167 178 249 320 342
SPECTROMETRY, 6
LASER LIGHT SCATTERING, 35
IDENTIFICATION, 30 79 121 128 INTERFEROMETRY, 13 275 363 200
132 212 214 353 370 397 INTERNAL MOULD RELEASE, LASER RAMAN
ILLUMINATION, 311 202 SPECTROSCOPY, 168
IMAGING, 13 67 88 168 179 275 INTRINSIC VISCOSITY, 29 172 LATERAL FORCE
289 346 266 330 MICROSCOPY, 308
IMIDAZOLE, 262 INVERSE GAS LATEX, 46 156 174 193 198
IMIDISATION, 8 355 CHROMATOGRAPHY, 81 90 LEACHING, 183
IMMERSION, 178 223 237 141 143 191 217 235 339 382 LEAD, 201
IMMISCIBLE, 188 367 394 390 LEAST-SQUARES ANALYSIS,
IMMUNOELECTROPHORESIS, ION CHROMATOGRAPHY, 97 70 214 345
97 218 LENS, 219 265
IMPACT PROPERTIES, 56 63 231 ION CYCLOTRON RESONANCE, LIFETIME PREDICTION, 108
370 388 397 255 377
IMPLANT, 219 262 393 ION EXCHANGE, 50 97 351 LIGHT ABSORPTION, 229 274
IMPURITY, 221 IONISATION, 46 50 206 222 379 LIGHT DEGRADATION, 3 40 129
INDUCTION PERIOD, 41 88 IRON OXIDE, 112 153 196 274 288
INDUCTIVELY COUPLED IRRADIATION, 4 40 92 153 358 LIGHT MICROSCOPY, 181 295
PLASMA SPECTROMETRY, IRRADIATION DEGRADATION, LIGHT SCATTERING, 111 116
351 133 117 172 203 238 260 310 396
INELASTIC NEUTRON ISOELECTRIC POINT, 46 333 LIGHT STABILISER, 3 31 123
SCATTERING, 361 ISOMERISATION, 11 288 132 288
INFRARED ABSORPTION, 36 ISOPHORONE DIISOCYANATE, LIGHT STABILITY, 3 288
274 362 121 LIGNOCELLULOSE, 82
INFRARED CAMERA, 67 ISOTACHOPHORESIS, 46 LINEAR LOW DENSITY
INFRARED DICHROISM, 284 ISOTACTIC, 129 133 274 314 POLYETHYLENE, 57 92 107
INFRARED SPECTROSCOPY, 1 3 ISOTHERM, 67 178 309 339 139 186 216 225 324 386
8 11 14 17 24 26 29 33 34 36 39 ISOTHERMAL, 36 78 117 125 276 LINEAR REGRESSION
41 43 51 60 63 66 69 72 77 79 317 338 348 375 ANALYSIS, 144
85 88 92 93 94 98 108 113 126 ISOTROPY, 117 LIQUID CHROMATOGRAPHY,
135 142 150 153 156 160 161 21 25 35 39 46 50 55 76 97 103
163 164 165 169 172 173 181 K 105 108 124 159 165 171 183
184 186 188 189 207 215 216 195 200 203 206 210 222 229
225 226 228 230 244 246 249 KAOLIN, 226 306 233 238 239 240 241 242 243
247 264 266 285 286 299 304 325 288 387
319 337 353 355 366 375 379 MEDICAL APPLICATION, 42 262 MINERAL FILLER, 45 288 289
383 384 395 MELAMINE-FORMALDEHYDE 324
LIQUID CRYSTAL POLYMER, RESIN, 159 365 MISCIBILITY, 12 64 77 98 125 146
309 367 387 MELT, 54 170 254 282 290 354 209 213 220 309 367 390 391
LIQUID NITROGEN, 358 MELT TRANSITION, 267 394
LOW DENSITY MELTING, 2 24 54 78 79 136 155 MOBILE PHASE, 50 375 395
POLYETHYLENE, 3 57 86 87 179 209 252 309 332 MODEL, 28 105 149 152 172 216
139 143 164 168 186 207 214 MELTING POINT, 12 52 56 63 94 290 311 319 336 341 360 381
266 324 325 348 372 373 386 114 164 266 295 324 382 394
LOW FREQUENCY, 126 363 MELTING TEMPERATURE, 20 57 MODULATED DIFFERENTIAL
LOW MOLECULAR WEIGHT, 179 207 309 323 332 370 SCANNING CALORIMETRY,
128 375 MEMBRANE OSMOMETRY, 396 10 36 74 125 131 135 161 220
METAL, 177 179 298 341 261 282 309 377 394
METAL ADHESION, 62 223 341 MODULATED TEMPERATURE
M METAL COATING, 62 255 THERMOMECHANICAL
MAGIC ANGLE, 209 268 283 291 METAL SALT, 352 ANALYSIS, 20
300 340 METALLISED FILM, 168 266 387 MOISTURE CONTENT, 6 51 148
MAGNESIUM-25, 359 METHACRYLATE COPOLYMER, 266 309
MALDI-TOF SPECTROSCOPY, 190 MOLAR MASS, 25 35 102 103 107
28 103 127 137 158 159 166 204 METHACRYLIC ACID 140 159
310 322 335 356 376 COPOLYMER, 15 63 259 MOLECULAR
MALEIC ANHYDRIDE, 82 METHACRYLIC ESTER CONFIGURATION, 117 130
MALEIC ANHYDRIDE COPOLYMER, 190 135 168 328 338 355 367
COPOLYMER, 28 341 METHACRYLIC ESTER MOLECULAR INTERACTION,
MAPPING, 69 275 289 339 342 POLYMER, 45 245 178 220 342 375
344 METHANOL, 39 56 76 171 266 MOLECULAR MOBILITY, 26 268
MASS SELECTIVE DETECTOR, METHANOLYSIS, 39 301 389
76 218 METHYL ACETATE, 185 MOLECULAR ORIENTATION,
MASS SPECTROMETRY, 4 6 13 METHYL ACRYLATE 257 281 284 327 360
28 30 50 75 103 107 112 127 COPOLYMER, 33 172 299 395 MOLECULAR STRUCTURE, 1 8
132 178 186 192 194 204 222 METHYL ETHYL KETONE, 285 12 16 25 31 47 49 51 53 56 66
229 266 278 307 311 376 379 METHYL METHACRYLATE, 288 68 72 73 77 80 83 89 93 98 101
382 392 396 397 398 METHYL METHACRYLATE 102 103 107 114 130 133 140
MASS SPECTROSCOPY, 28 66 72 COPOLYMER, 28 33 166 198 146 152 158 159 164 166 168
84 86 103 121 124 127 128 137 308 384 172 180 197 198 200 211 213
153 158 159 166 177 185 190 METHYLBENZENE, 56 185 241 222 228 229 232 243 264 268
195 202 204 206 244 250 270 261 269 274 275 277 283 284 286
273 303 310 312 322 335 356 METHYLENE CHLORIDE, 266 289 291 300 301 308 310 317
376 399 MICROANALYSIS, 179 231 289 318 328 331 334 337 355 356
MATRIX, 36 82 141 178 182 351 MICROBIAL DEGRADATION, 5 364 365 368 370 376 382 391
359 MICROCALORIMETRY, 154 MOLECULAR WEIGHT, 1 28 29
MATRIX-ASSISTED LASER MICRODIELECTROMETRY, 9 42 46 50 52 54 55 62 73 89 102
DESORPTION, 28 103 127 137 MICROEXTRACTION, 71 185 112 113 114 116 120 127 128
158 159 166 204 310 322 335 MICRORAMAN 130 158 164 166 172 185 190
356 376 SPECTROSCOPY, 168 346 200 204 210 222 224 235 239
MDI, 9 MICROSCOPY, 2 13 16 27 38 41 243 285 310 314 319 322 323
MECHANICAL DEGRADATION, 58 59 61 98 111 125 126 142 325 330 332 334 337 355 356
266 145 168 179 181 213 231 256 375 376 378 381 382 388 395
MECHANICAL PROPERTIES, 9 257 277 289 295 308 324 387 396
40 41 56 61 62 63 65 67 82 84 MICROSTRUCTURE, 13 58 60 MOLECULAR WEIGHT
86 91 114 115 126 151 163 168 168 170 198 274 370 388 392 DISTRIBUTION, 102 116 190
178 179 182 207 231 249 256 MICROTOMY, 168 200 204 224 310 314 319 322
269 271 277 281 288 289 296 MICROWAVE, 112 128 262 325 356 375 381 396
309 315 316 324 325 333 353 MICROWAVEABLE, 266 387 MONITORING, 5 70 149 174 188
365 370 388 MID-INFRARED 223 261 272 298 311 321 348
MECHANICAL RECYCLING, 195 SPECTROSCOPY, 362 MONOETHYLENE GLYCOL, 39
MECHANICAL SPECTROSCOPY, MIGRATION, 46 65 183 264 266 266
MONOMER, 124 229 269 270 387 OIL, 194 277 PERMITTIVITY, 338
MORPHOLOGY, 2 13 54 61 63 98 OLIGOMER, 26 46 103 124 172 PEROXIDE, 294 326
115 118 136 191 213 256 309 190 192 238 242 264 266 335 PEROXY COMPOUND, 393
319 346 367 391 394 ON-LINE MEASUREMENT, 314 PESTICIDE, 373
MOULDING, 134 225 343 OPTICAL FIBRE, 36 188 292 PH, 46 50 130 183
MULTI-ANGLE LASER LIGHT OPTICAL MICROSCOPY, 2 13 41 PHARMACEUTICAL
SCATTERING, 35 200 98 125 142 181 213 289 324 APPLICATION, 46 221
MULTILAYER, 168 266 344 387 387 PHASE BEHAVIOUR, 267 340
MULTILAYER FILM, 57 168 OPTICAL PROPERTIES, 1 3 47 365
MULTIPLE PULSE NMR, 291 57 162 181 199 200 206 263 PHASE SEPARATION, 110 125
MULTIVARIATE ANALYSIS, 216 274 288 292 293 323 332 350 156 391 394
MUNICIPAL WASTE, 128 362 375 PHENOL, 75 297 300
OPTIMISATION, 50 102 105 171 PHENOL-FORMALDEHYDE
233 318 373 RESIN, 73 297 300
N ORGANOLEPTIC PROPERTIES, PHENOLIC ANTIOXIDANT, 183
N-METHYL-2-PYRROLIDONE, 57 183 PHENOLIC RESIN, 83 199 300
355 ORIENTED, 104 117 283 284 361 PHOSPHORUS, 95 312 373
NANOCOMPOSITE, 62 387 PHOTOACOUSTIC
NAPHTHA, 215 ORTHOPAEDIC APPLICATION, SPECTROSCOPY, 249 288 344
NATURAL FIBRE, 82 393 PHOTOCALORIMETRY, 377
NATURAL FIBRE-REINFORCED OSCILLATING DIFFERENTIAL PHOTOCHEMICAL
PLASTIC, 141 SCANNING CALORIMETRY, DEGRADATION, 288
NATURAL POLYMER, 232 352 7 PHOTOCROSSLINKING, 45 187
NEAR-INFRARED OSMOMETRY, 29 46 200 378 PHOTODEGRADATION, 16 19
CORRELATION OVEN STABILITY, 266 65 66 274 279
SPECTROSCOPY, 364 OXIDATION, 40 41 61 66 88 94 PHOTOELECTRON
NEAR-INFRARED 104 129 152 153 205 266 269 SPECTROSCOPY, 13 37 48
SPECTROSCOPY, 14 36 215 274 288 325 329 348 381 393 100 104 121 167 175 176 196
225 362 371 OXYGEN, 57 104 153 262 274 197 202 205 277 279 298 308
NITROCELLULOSE, 46 79 185 311 312 316 320 333 343
NITROGEN, 57 76 95 OXYGEN ABSORPTION, 104 PHOTOINITIATOR, 27 312
NITROGEN-CONTAINING 387 PHOTOISOMERISATION, 288
POLYMER, 250 OXYGEN BARRIER, 56 57 168 PHOTOLYSIS, 153
NON-DESTRUCTIVE TEST, 19 PHOTON CORRELATION
SPECTROSCOPY, 224
32 67 106 126 157 327 P PHOTOOXIDATION, 40 129 153
NOVOLAC RESIN, 73 300
NUCLEAR MAGNETIC PACKAGING, 5 57 128 131 168 274 288
RESONANCE, 1 22 28 30 31 212 264 266 278 323 387 PHOTOVOLTAIC PROPERTIES,
32 34 57 60 68 73 77 100 108 PACKAGING FILM, 57 168 266 38
113 114 123 130 138 148 162 387 PHTHALATE, 288
169 172 180 189 193 201 209 PAINT, 62 174 185 217 255 298 PHTHALOCYANINE GREEN, 65
212 246 248 251 265 268 272 PAPER, 266 387 PHYSICAL AGEING, 101 135 213
283 291 297 300 314 331 334 PAPER CHROMATOGRAPHY, 97 309 338
340 350 359 370 372 376 383 PARACRYSTALLINE, 102 207 PHYSICAL PROPERTIES, 12 42
388 389 391 392 213 315 52 56 63 94 114 164 188 215
NUMBER-AVERAGE PARTIAL LEAST SQUARES, 215 216 236 259 266 295 324 353
MOLECULAR WEIGHT, 130 216 382
375 378 PARTICLE BEAM ANALYSIS, PIGMENT, 65 121 181 217 225
NYLON, 33 56 57 79 125 164 168 206 236 237 325 399
192 199 207 225 231 309 331 PARTICLE PACKING, 324 PIPE, 52 183 277 307 329
NYLON 1010, 24 PARTICLE SIZE, 13 45 50 81 225 PLANT FIBRE, 82
NYLON-12, 294 364 233 319 324 372 375 PLASMA TREATMENT, 61 69
NYLON-6, 33 56 57 132 207 387 PARTICLE SIZE 106 230 262 298 343
NYLON-6,6, 17 33 57 130 231 329 DISTRIBUTION, 62 324 PLASTICISATION, 36 56 301 348
PEAK INTENSITY, 168 178 260 PLASTICISER, 33 34 120 184 258
289 392 277 353 387 399
O PELLET, 216 266 296 373 PLASTICS WASTE, 87 211 212
PERMEABILITY, 56 57 168 237 PLATE-OUT, 6
ODOUR, 57 183 307
POLARISATION, 256 257 284 POLYCYANATE, 11 207 212 214 257 261 263 266
POLARISED CONFOCAL POLYCYANURATE, 317 269 283 293 309 323 336 357
RAMAN MICROSCOPY, 257 POLYDEUTEROPOLYETHYLENE, 358 382 388 398
POLARISED FLUORESCENCE, 361 POLYFLUOROETHYLENE, 79
284 POLYDICYANATE, 11 164 180 279 296
POLARISED LIGHT POLYDIMETHYLPHENYLENE POLYHYDROXYBUTYRATE, 59
MICROSCOPY, 181 OXIDE, 356 POLYHYDROXYBUTYRIC
POLARISED OPTICAL POLYDIMETHYLSILOXANE, ACID, 246
MICROSCOPY, 13 140 POLYHYDROXYETHYL
POLARISING MICROSCOPY, POLYDISPERSITY, 29 35 127 137 METHACRYLATE, 172 248
168 204 224 325 335 356 POLYHYDROXYKETONE, 349
POLARITY, 50 203 339 POLYEPICHLOROHYDRIN, 390 POLYHYDROXYSTYRENE, 77
POLYACETAL, 164 POLYEPOXIDE, 10 20 32 36 47 367
POLYACRYLAMIDE, 46 240 62 68 144 145 149 151 157 161 POLYIMIDE, 5 23 79 196 199 320
POLYACRYLATE, 245 269 178 179 182 199 200 222 249 355
POLYACRYLIC, 249 343 255 269 272 282 292 305 309 POLYIONENE, 57 276
POLYACRYLIC ACID, 46 172 342 312 320 POLYISOCYANATE, 9
POLYACRYLIC IMIDE, 387 POLYESTER RESIN, 199 204 288 POLYKETONE, 54
POLYACRYLONITRILE, 33 79 POLYESTER-URETHANE, 114 POLYLACTIC ACID, 267
119 342 POLYESTERIMIDE, 355 POLYMERIC FLAME
POLYALPHA- POLYETHER, 54 66 158 235 238 RETARDANT, 218 273
METHYLSTYRENE, 153 242 384 398 POLYMERIC MOULD RELEASE
POLYAMIC ACID, 355 POLYETHER SULPHONE, 75 AGENT, 202
POLYAMIDE, 33 56 57 79 125 125 151 356 POLYMETHACRYLATE, 45 245
164 168 192 199 207 225 231 POLYETHER-ETHERKETONE, 398
309 331 54 79 126 213 295 315 POLYMETHACRYLIC ACID, 15
POLYAMIDE-1010, 24 POLYETHER-URETHANE, 90 141
POLYAMIDE-12, 159 POLYETHERETHERKETONE, 79 POLYMETHACRYLONITRILE,
POLYAMIDE-6, 33 56 57 132 165 126 141
207 387 POLYETHERIMIDE, 64 79 98 192 POLYMETHYL
POLYAMIDE-6,6, 17 130 296 367 387 METHACRYLATE, 14 21 116
POLYAMIDE-IMIDE, 316 POLYETHERSULPHONE, 75 125 132 137 141 159 166 178 204
POLYAMINE, 46 272 151 356 219 220 221 224 229 240 241
POLYANILINE, 46 115 POLYETHYL ACRYLATE, 58 284 285 289 299 301 304 314
POLYARAMIDE, 191 339 POLYETHYL METHACRYLATE, 319 335 338 343 363 375 382
POLYARYL ETHER KETONE, 390 384 394 397 398
213 POLYETHYLENE, 42 52 56 57 60 POLYMETHYLENE OXIDE, 79
POLYARYLATE, 367 61 63 65 79 87 91 92 99 102 POLYOL, 84 110
POLYBENZIMIDAZOLE, 79 107 109 112 128 132 139 143 POLYOXYETHYLENE, 154
POLYBENZYL 146 148 154 157 164 168 181 POLYOXYMETHYLENE, 79
METHACRYLATE, 35 186 188 195 199 207 212 214 POLYPHENYLENE, 398
POLYBIBENZOATE, 309 216 225 249 256 260 263 266 POLYPHENYLENE ETHER, 79
POLYBISGLYCIDYL 267 283 293 307 315 324 325 152 220 367
METHACRYLATE, 247 344 348 357 361 365 366 368 POLYPHENYLENE OXIDE, 79
POLYBUTYL ACRYLATE, 156 370 372 373 386 392 393 398 152 220 357 367 394
394 400 POLYPHENYLENE SULPHIDE,
POLYBUTYL METHACRYLATE, POLYETHYLENE GLYCOL, 46 79 170 296 320 328
21 376 233 310 369 378 POLYPHENYLENE
POLYBUTYL THIOPHENE, 327 POLYETHYLENE GLYCOL TEREPHTHALAMIDE, 339
POLYBUTYLENE TEREPHTHALATE, 26 POLYPHENYLMETHACRYLATE,
NAPHTHALATE, 98 POLYETHYLENE 367
POLYBUTYLENE NAPHTHALATE, 387 POLYPHENYLSULPHONE, 79
TEREPHTHALATE, 164 273 POLYETHYLENE OXIDE, 125 POLYPROPYLENE, 31 41 57 59
POLYCAPROLACTONE, 147 267 154 235 337 79 87 88 91 102 104 109 112
390 POLYETHYLENE 118 123 128 129 132 133 168
POLYCARBONATE, 14 57 62 72 TEREPHTHALATE, 2 12 26 171 183 188 205 206 207 212
79 99 101 199 207 245 273 280 39 40 57 63 64 74 76 79 106 214 249 264 281 284 289 293
309 340 356 363 367 382 398 117 118 131 136 157 164 168 329 330 370 380 381 398
223 230 262 277 298 343 371 133 134 144 147 149 154 155 THIN LAYER
SURFACTANT, 46 65 233 170 179 186 187 189 207 245 CHROMATOGRAPHY, 97 399
SURGICAL APPLICATION, 219 252 258 267 269 270 305 309 TIE LAYER, 168
393 313 324 325 367 377 383 386 TIME, 54 61 94 135 209 223 253
SWELLING, 15 237 250 326 360 394 261 268 277 289 317 338 354
SYNCHROTRON RADIATION, THERMAL CONDUCTIVITY, 80 394
291 179 309 324 377 TIME DEPENDENCE, 125 196
SYNTHETIC FIBRE- THERMAL DEGRADATION, 23 360
REINFORCED PLASTIC, 281 26 29 75 76 83 85 152 160 163 TIME OF FLIGHT, 103 127 137
189 192 194 196 244 258 266 158 159 166 178 202 204 229
273 318 325 380 381 310 312 322 335 356 376
T THERMAL DIFFUSIVITY, 179 TIME RESOLVED
TALC, 65 318 324 324 394 SPECTROSCOPY, 170
TAPE, 284 THERMAL FIELD-FLOW TITANIUM DIOXIDE, 40 65 217
TAPPING MODE ATOMIC FRACTIONATION, 35 237 325
FORCE MICROSCOPY, 58 THERMAL HISTORY, 57 135 136 TOLUENE, 56 185 241 261 319
TASTE, 57 207 245 254 262 287 309 TOTAL ORGANIC CARBON, 183
TEMPERATURE DEPENDENCE, THERMAL IMAGING, 67 TOXICITY, 173 195
49 99 135 146 147 170 196 259 THERMAL INSULATION, 80 276 TRACE ELEMENT, 177
269 308 336 354 364 382 THERMAL MECHANICAL TRANSITION PHENOMENA,
TEMPERATURE GRADIENT ANALYSIS, 196 377 254
INTERACTION THERMAL RELAXATION, 282 TRANSITION PROPERTIES, 203
CHROMATOGRAPHY, 304 290 269 340 354
375 THERMAL RESISTANCE, 196 TRANSITION TEMPERATURE,
TEMPERATURE MODULATED THERMAL STABILITY, 11 24 26 179
DIFFERENTIAL SCANNING 57 85 126 163 196 228 266 267 TRANSMISSION ELECTRON
CALORIMETRY, 54 78 136 269 295 317 377 MICROSCOPY, 2 5 13 59 63
252 253 280 287 290 309 336 THERMAL TRANSITION, 56 78 82 108 129 181 213 289 331
TEMPERATURE PROFILE, 67 220 282 290 309 358
324 THERMAL VOLATILISATION TRANSMISSION
TEMPERATURE ANALYSIS, 189 SPECTROSCOPY, 234 292 362
PROGRAMMED THERMALLY STIMULATED TRANSPARENCY, 57 236 323
ANALYTICAL PYROLYSIS, CURRENT, 323 377 TRANSPORT PROPERTIES, 56
273 THERMOANALYTICAL, 348 115
TEMPERATURE RANGE, 207 THERMODYNAMIC TRIAZINE, 40
317 364 380 382 PROPERTIES, 21 90 122 155 TRICHLOROBENZENE, 29
TEMPERATURE RISING 169 172 220 235 290 339 TRICHLOROMETHANE, 29
ELUTION FRACTIONATION, THERMOGRAM, 36 67 323 348 TRIETHYLAMINE, 298
370 396 370 TRIFLUOROACETIC ACID, 388
TENSILE PROPERTIES, 40 41 61 THERMOGRAVIMETRIC TROUBLESHOOTING, 30 181
63 65 86 114 115 231 277 315 ANALYSIS, 2 8 12 15 17 23 24 296 303
333 26 29 48 82 83 85 93 94 98 146 TWO-DIMENSIONAL, 55 58 209
TEREPHTHALIC ACID, 76 152 163 164 189 192 194 196 233 242 275 283 344 345 364
TERTIARY AMINE, 36 151 211 228 231 244 258 267 269 365
TEST SPECIMEN, 236 346 351 295 296 316 317 318 326 330
347 348 377 380 381 398
358
THERMOLYSIS, 189
U
TESTING, 19 43 58 59 62 71 79
96 108 112 120 123 124 134 THERMOMECHANICAL UHMWPE, 260 393
145 174 182 183 184 185 195 DEGRADATION, 266 ULTRA-HIGH RESOLUTION
206 208 254 255 270 288 293 THERMOMECHANICAL SPECTROSCOPY, 363
304 315 321 329 332 345 347 PROPERTIES, 179 269 ULTRASONIC, 112 126 272
357 363 365 379 382 398 THERMOOXIDATIVE ULTRAVIOLET ABSORPTION,
TETRAHYDROFURAN, 29 35 DEGRADATION, 41 94 152 229 274
240 241 319 395 269 348 ULTRAVIOLET CURING, 27 269
TEXTILE APPLICATION, 371 THERMORHEOLOGICAL 349
THERMAL AGEING, 88 152 PROPERTIES, 338 ULTRAVIOLET DEGRADATION,
THERMAL ANALYSIS, 7 20 26 THICKNESS, 27 56 62 67 168 179 16 19 196
36 54 56 67 78 83 92 95 110 236 255 257 263 ULTRAVIOLET IRRADIATION,
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