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ADDITIVES IN POLYMERS
Industrial Analysis and Applications
Additives In Polymers: Industrial Analysis And Applications
J. C. J. Bart
2005 John Wiley & Sons, Ltd
ISBN: 0-470-85062-0
ADDITIVES IN POLYMERS
Industrial Analysis and Applications
Jan C.J. Bart
DSM Research, The Netherlands
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Copyright
2005
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Library of Congress Cataloging-in-Publication Data
Bart, Jan C. J.
Additives in polymers : industrial analysis and applications / Jan C.J. Bart.
p. cm.
Includes bibliographical references and index.
ISBN 0-470-85062-0 (acid-free paper)
1. Polymers – Additives. 2. Polymers – Analysis. I . Title.
TP1142.B37 2005
668.9 – dc22
2004015411
British Library Cataloguing in Publication Data
A catalogue record for this book is available from the British Library
ISBN 0-470-85062-0
Typeset in 9/11pt Times by Laserwords Private Limited, Chennai, India
Printed and bound in Great Britain by Antony Rowe Ltd, Chippenham, Wiltshire
This book is printed on acid-free paper responsibly manufactured from sustainable forestry
in which at least two trees are planted for each one used for paper production.
The author and publishers wish to thank C. Gerhardt, GmbH & Co. KG for providing the cover image:
‘Soxtherm’ an original painted by Douglas Swan (1997).
Contents
FOREWORD .........................
ix
2.6.2 Deformulation of rubbers ......
48
2.6.3 Deformulation of polymers .....
48
PREFACE ...........................
xi
2.7 References .......................
48
ABOUT THE AUTHOR .................
xiii
CHAPTER 3
Sample Preparation
Perspectives ..............
51
ACKNOWLEDGEMENTS ................
xv
3.1 Solvents ........................
54
3.1.1 Polymer solubility criteria ......
55
CHAPTER 1
Introduction ..............
1
3.1.2 Solubility parameters ..........
55
3.1.3 Polymer solutions ............
56
1.1 Additives ........................
2
3.2 Extraction strategy .................
57
1.1.1 Additive functionality .........
3
3.3 Conventional extraction technologies ...
59
1.2 Plastics formulations ...............
5
3.3.1 Liquid–liquid extraction .......
60
1.2.1 Supply forms ...............
7
3.3.2 Liquid–solid extraction ........
60
1.2.2 Additive delivery ............
9
3.3.3 Classical solvent extractions of
additives from polymers .......
1.3 Economic impact of polymer additives ..
9
61
1.4 Analysis of plastics ................
11
3.3.4 Sonication .................
75
1.4.1 Regulations and standardisation ..
15
3.4 High-pressure solvent extraction methods
81
1.4.2 Prior art ...................
17
3.4.1 Supercritical fluid technology ...
81
1.4.3 Databases ..................
19
3.4.2 Analytical SFE ..............
85
1.4.4 Scope .....................
20
3.4.3 Subcritical water extraction .....
100
1.4.5 Chapter overview ............
22
3.4.4 Microwave technology ........
101
1.5 Bibliography .....................
23
3.4.5 Microwave-assisted extractions ..
104
1.5.1 Plastics additives .............
23
3.4.6 Pressurised fluid extraction .....
117
1.5.2 Processing technologies ........
23
3.5 Sorbent extraction .................
123
1.5.3 Instrumental analysis ..........
23
3.5.1 Solid-phase extraction .........
124
1.5.4 Polymer analysis .............
24
3.5.2 Solid-phase microextraction .....
129
1.5.5 Polymer/additive analysis ......
24
3.5.3 Stir bar sorptive extraction .....
133
1.6 References .......................
24
3.6 Methodological comparison of extraction
methods .........................
134
CHAPTER 2 Deformulation Principles ....
3.6.1 Experimental comparisons ......
136
29
3.6.2 Extraction selectivity ..........
138
3.6.3 ‘Nonextractable’ additive analysis
140
2.1 Polymer identification ..............
30
2.2 Additive analysis of rubbers: ‘Best
Practice’ ........................
3.7 Polymer/additive dissolution methods ...
146
32
3.8 Hydrolysis .......................
152
2.3 Polymer extract analysis .............
42
3.9 Bibliography .....................
155
2.4 In situ polymer/additive analysis ......
46
3.9.1 Sampling and sample preparation
155
2.5 Class-specific polymer/additive analysis .
47
3.9.2 Solvents/solubility ............
155
2.6 Bibliography .....................
48
3.9.3 Extraction methods ...........
156
2.6.1 Polymer identification .........
48
3.10 References .......................
156
vi
CONTENTS
CHAPTER 4
Separation Techniques ......
171
6.1.2 Modes of detection ...........
353
6.1.3 Mass resolution ..............
354
4.1 Analytical detectors ................
177
6.1.4 Isotope distributions ..........
354
4.2 Gas chromatography ...............
181
6.1.5 Accurate mass measurements ....
355
4.2.1 High-temperature gas
chromatography .............
6.2 Ion sources ......................
357
200
6.2.1 Electron impact ionisation ......
360
4.2.2 Headspace gas chromatography ..
202
6.2.2 Chemical ionisation ...........
362
4.3 Supercritical fluid chromatography .....
205
6.2.3 Metastable atom bombardment ..
367
4.4 Liquid chromatography techniques .....
217
6.2.4 Fast atom bombardment .......
367
4.4.1 Planar chromatographies .......
218
6.2.5 Field ionisation ..............
372
4.4.2 Column chromatographies ......
230
6.2.6 Field desorption .............
374
4.5 Capillary electrophoretic techniques ....
273
6.2.7 Thermospray ionisation ........
376
4.6 Bibliography .....................
278
6.2.8 Atmospheric pressure ionisation
techniques .................
4.6.1 General texts ...............
278
378
4.6.2 Detectors ..................
279
6.2.9 Desorption/ionisation methods ...
383
4.6.3 Gas chromatography ..........
279
6.2.10 Photoionisation techniques ......
385
4.6.4 Supercritical fluid chromatography
279
6.3 Mass analysers ...................
386
4.6.5 Thin-layer chromatography .....
279
6.3.1 Sector analysers .............
387
4.6.6 Liquid chromatography ........
280
6.3.2 Quadrupole mass spectrometers ..
389
4.6.7 Size-exclusion chromatography ..
280
6.3.3 Time-of-flight mass spectrometry .
390
4.6.8 Ion chromatography ..........
280
6.3.4 Quadrupole ion trap ..........
393
4.6.9 Capillary electrophoretic
techniques .................
6.3.5 Fourier-transform ion-cyclotron
resonance mass spectrometry ....
280
395
4.7 References .......................
281
6.3.6 Tandem mass spectrometry .....
398
6.4 Direct mass-spectrometric polymer
compound analysis .................
407
CHAPTER 5
Polymer/Additive Analysis:
The Spectroscopic Alternative
6.5 Ion mobility spectrometry ...........
415
299
6.6 Bibliography .....................
417
6.6.1 Mass spectrometry (General) ....
417
5.1 Ultraviolet/visible spectrophotometry ...
302
6.6.2 Mass spectrometers ...........
417
5.2 Infrared spectroscopy ...............
311
6.6.3 Ionisation modes .............
417
5.3 Luminescence spectroscopy ..........
318
6.7 References .......................
418
5.4 High-resolution nuclear magnetic
resonance spectroscopy .............
323
CHAPTER 7 Multihyphenation and
Multidimensionality in
Polymer/Additive Analysis ...
5.4.1 Multidimensional NMR
spectroscopy ................
336
5.5 Bibliography .....................
342
425
5.5.1 General spectroscopy .........
342
7.1 Precolumn hyphenation .............
428
5.5.2 Ultraviolet/visible
spectrophotometry ............
7.1.1 Chromatographic sampling
methods ...................
342
432
5.5.3 Infrared spectroscopy .........
342
7.2 Coupled sample
preparation – spectroscopy/spectrometry .
5.5.4 Luminescence spectroscopy .....
342
449
5.5.5 Nuclear magnetic resonance
spectroscopy ................
7.3 Postcolumn hyphenation .............
452
342
7.3.1 (Multi)hyphenated GC techniques
456
5.6 References .......................
342
7.3.2 (Multi)hyphenated SFC
techniques .................
475
CHAPTER 6 Organic Mass-Spectrometric
Methods ................
7.3.3 (Multi)hyphenated HPLC
techniques .................
349
489
7.3.4 Hyphenated SEC techniques ....
527
6.1 Basic instrumentation ...............
351
7.3.5 Hyphenated TLC techniques ....
530
6.1.1 Inlet systems ................
352
7.3.6 Hyphenated CE techniques .....
543

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