Polymer Reference Book

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Polymer Reference Book

T. R. Crompton

rapraTECHNOLOGY

Polymer Reference Book

T.R. Crompton

Rapra Technology LimitedShawbury, Shrewsbury, Shropshire, SY4 4NR, United Kingdom Telephone: +44 (0)1939 250383 Fax: +44 (0)1939 251118 http://www.rapra.net

First Published in 2006 by

Rapra Technology LimitedShawbury, Shrewsbury, Shropshire, SY4 4NR, UK

2006, Rapra Technology Limited

All rights reserved. Except as permitted under current legislation no part of this publication may be photocopied, reproduced or distributed in any form or by any means or stored in a database or retrieval system, without the prior permission from the copyright holder. A catalogue record for this book is available from the British Library. Every effort has been made to contact copyright holders of any material reproduced within the text and the authors and publishers apologize if any have been overlooked.

ISBN: 1-85957-526-9

Typeset by Rapra Technology Limited Printed and bound by Lightning Source UK Limited

Contents

Preface ......................................................................................................................... 1 1. Determination of Metals ....................................................................................... 7 1.1 Destructive Techniques ................................................................................ 7 1.1.1 1.1.2 1.1.3 1.1.4 1.1.5 1.1.6 1.1.7 1.1.8 1.1.9 Atomic Absorption Spectrometry .................................................... 7 Graphite Furnace Atomic Absorption Spectrometry ........................ 8 Atom Trapping Technique............................................................... 9 Vapour Generation Atomic Absorption Spectrometry ................... 10 Zeeman Atomic Absorption Spectrometry .................................... 11 Inductively Coupled Plasma Atomic Emission Spectrometry ......... 14 Hybrid Inductively Coupled Plasma Techniques............................ 22 Inductively Coupled Plasma Optical Emission Spectrometry Mass Spectrometry........................................................................ 23 Pre-concentration Atomic Absorption Spectrometry Techniques ... 25

1.1.10 Microprocessors............................................................................ 26 1.11 Autosamplers ............................................................................................. 26 1.1.12 Applications: Atomic Absorption Spectrometric Determination of Metals....................................................................................... 26 1.1.13 Visible and UV Spectroscopy......................................................... 34 1.1.14 Polarography and Voltammetry .................................................... 34 1.1.15 Ion Chromatography .................................................................... 36 1.2 Non-destructive Methods .......................................................................... 43 1.2.1 1.2.2 X-ray Fluorescence Spectrometry .................................................. 43 Neutron Activation Analysis ......................................................... 49

References ........................................................................................................... 53 i

Polymer Reference Book 2. Non-metallic Elements ........................................................................................ 57 2.1 Instrumentation: Furnace Combustion Methods ........................................ 58 2.1.1 2.1.2 2.1.3 2.1.4 2.1.5 2.1.6 2.1.7 2.2 Halogens ....................................................................................... 58 Sulfur ............................................................................................ 58 Total Sulfur/Total Halogen ............................................................ 58 Total Bound Nitrogen ................................................................... 59 Nitrogen, Carbon, and Sulfur ....................................................... 59 Carbon, Hydrogen, and Nitrogen ................................................. 60 Total Organic Carbon ................................................................... 61

Oxygen Flask Combustion Methods .......................................................... 61 2.2.1 2.2.2 2.2.3 2.2.4 2.2.5 Total Halogens .............................................................................. 61 Sulfur ............................................................................................ 62 Oxygen Flask Combustion: Ion Chromatography ......................... 62 Instrumentation ............................................................................ 63 Applications .................................................................................. 63

2.3

Acid and Solid Digestions of Polymers ....................................................... 64 2.3.1 2.3.2 2.3.3 2.3.4 Chlorine ........................................................................................ 64 Nitrogen ....................................................................................... 65 Phosphorus ................................................................................... 65 Silica ............................................................................................. 66

2.4 2.5

X-ray Fluorescence Spectroscopy ............................................................... 66 Antec 9000 Nitrogen/Sulfur Analyser ........................................................ 67

References ........................................................................................................... 68 3. Functional Groups and Polymer Structure ........................................................... 71 3.1 Infrared and Near-Infrared Spectroscopy ................................................... 71 3.1.1 3.1.2 3.2 Instrumentation ............................................................................ 71 Applications .................................................................................. 71

Fourier Transform Near-Infrared Raman Spectroscopy ............................. 80 3.2.1 Theory .......................................................................................... 80

ii

Contents 3.2.2 3.2.3 3.3 Instrumentation ............................................................................ 82 Applications .................................................................................. 82

Fourier Transform Infrared Spectroscopy .................................................. 85 3.3.1 3.3.2 Instrumentation ............................................................................ 85 Applications .................................................................................. 86

3.4

Nuclear Magnetic Resonance (NMR) Spectroscopy .................................. 89 3.4.1 3.4.2 Instrumentation ............................................................................ 89 Applications .................................................................................. 89

3.5

Proton Magnetic Resonance (PMR) Spectroscopy ..................................... 96 3.5.1 3.5.2 Instrumentation ............................................................................ 96 Applications .................................................................................. 97

3.6

Reaction Gas Chromatography ................................................................. 99 3.6.1 3.6.2 Instrumentation ............................................................................ 99 Applications .................................................................................. 99

3.7

Pyrolysis Gas Chromatography ............................................................... 108 3.7.1 3.7.2 3.7.3 Theory ........................................................................................ 108 Instrumentation .......................................................................... 108 Applications ................................................................................ 109

3.8

Pyrolysis Gas ChromatographyMass Spectrometry ................................ 122 3.8.1 3.8.2 Instrumentation .......................................................................... 122 Applications ................................................................................ 125

3.9

Pyrolysis Gas ChromatographyFourier Transform NMR Spectroscopy.... 126 3.10 High-Performance Liquid Chromatography ................................ 126

3.11 Mass Spectrometric Techniques ............................................................... 127 3.11.1 Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) .... 127 3.11.2 XPS ............................................................................................. 130 3.11.3 Tandem Mass Spectrometry (MS/MS) ......................................... 132 3.11.4 Fourier Transform Ion Cyclotron Mass Spectrometry ................. 132 3.11.5 MALDI-MS ................................................................................ 133 3.11.6 Radio Frequency Glow Discharge Mass Spectrometry ................ 134 iii

Polymer Reference Book 3.12 Microthermal Analysis ............................................................................ 135 3.13 Atomic Force Microscopy ........................................................................ 136 3.13.1 Applications ................................................................................ 136 3.14 Scanning Electron Microscopy and Energy Dispersive Analysis using X-rays ............................................................................................ 139 R