Atlas Of Plastics Additives - Analysis by Spectrometric Methods.pdf - Polymers(1) - ziolek6661

Dietrich O. Hummel

Atlas of Plastics Additives

Analysis by Spectrometric Methods

With 62 tables and 772 FTIR spectra

Springer

Prof. Dr. Dietrich O. Hummel

Im Lindenhof 15

D-53773 Hennef

ISBN 3-540-42414-8 Springer-Verlag Berlin Heidelberg New York

Library of Congress Cataloging-in-Publication-Data

Hummel, Dieter O.

Atlas of plastics additives : analysis by spectrometric methods / Dieter Hummel.

p.cm.

Includes bibliographical references and index.

ISBN 3540424148 (alk. paper)

1. Plastics--Additives--Analysis. 2. Plastics--Additives--Spectra. I. Title.

TP1142.H86 2002

668.4 c n--dc2i

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Preface

Twenty years ago the 2nd edition of the text and spectra volume of Friedrich Scholl on the analysis of plastics additives

was published, it can be found in most laboratories. He deceased shortly after his retirement, and my coworkers and I took

over his heritage. Collecting samples of additives of all kind as well as the measurement of their FTIR spectra was done by

Sigrun Wittmann, Liu Min, Mark Amberg, Vera Brunne, Astrid Baum and myself; my wife Doris digitised the structures. 752

spectra of the more important additives were selected from a total of 1630. To facilitate access for the analyst, the "triplets"

(spectrum with peak table, structure, legend) were arranged according to a decimal system (technological class, chemical

composition). Registers (chemical and trade name, empirical formula) help one to find the desired spectrum.

Literature on (predominantly) spectroscopic methods in the analysis of plastics additives was evaluated until 2001.

Methods and experiments were critically reported; wherever possible the results were compressed in tables. In order to keep

the volume of the book within limits only elementary methods for the separation of additives and matrices were described

(2nd chapter). The chromatographic separation of mixtures had to be omitted; it is amply described in the book of Scholl

and in later monographs. The reason why chapters 3 and 7 are so large is very simple: (FT)IR and mass spectrometries are

by far the most important methods for identification and quantitative determination of additives. They are also suitable for

combination with chromatographic and other analytical methods.

I owe gratitude to my coworkers for their zeal as well as to Stiftung Industrieforschung for generous support of our

research, to many chemical companies for providing samples and to numerous colleagues sending reprints. Many thanks

go to my colleagues B. Schrader (Uni. Essen), K.-W. Brzezinka (BAM, Berlin-Adlershof), K.-J. Eichhorn and D. Fischer (IPF

Dresden) for measuring the Raman spectra of problematic samples. Finally, many thanks go to the editorial staff of Springer

Verlag and to medio Technologies (producer) for skill and carefulness and for their patience with the author.

Dietrich O. Hummel

Summer 2002

Contents

Preface .............................................................................................................................

Part A. Theory und Practical Applications

1. Introduction ..............................................................................................................................

2. Extraction, Solution Precipitation and Separation of Additives ...............................................

2.1 Extraction ..............................................................................................................

2.2 Solution Precipitation .............................................................................................

2.3

Separation of Additive Mixtures into Components ..................................................

3. Infrared Spectrometry ..............................................................................................................

3.1 Fundamentals ........................................................................................................

3.2

Sample Preparation and Measurement ..................................................................

3.3

Conventional and Computer-Supported Interpretation of IR Spectra ......................

3.4 Some Aspects of FTIR Spectrometry .....................................................................

3.4.1

Storage of Spectra in the Computer ...............................................................

3.4.2

The Search for Similarity and Equality (“Identity”) ..........................................

3.5 Recent Work in IR Spectrometry of Additives ........................................................

3.5.1

Additives with Preventive or Curative Properties ............................................

3.5.1.1 Empirical IR Band Assignments ........................................................

3.5.1.2 Separation of Additives and Identification by (FT)IR

Spectrometry .....................................................................................

3.5.1.3 Solubility of Stabilizers and Antioxidants in Polymers .......................

3.5.1.4 ATR Investigation of Rubber Surfaces ..............................................

3.5.1.5 Quantitative IRS Analysis of Additives ..............................................

3.5.2

Pigments and Fillers .......................................................................................

3.5.2.1 Organic Pigments ..............................................................................

3.5.2.2 Inorganic Pigments and Fillers ..........................................................

3.5.2.3 Pigments and Other Components in Fine Art and Historical

Objects .............................................................................................. 25

3.5.3 Plasticizers ..................................................................................................... 26

This page has been reformatted by Knovel to provide easier navigation.

vii

viii Contents

4. Raman Spectrometry ............................................................................................................... 55

4.1 Fundamentals ........................................................................................................ 55

4.2 Applications of RS in the Field of Plastics Additives ...............................................

4.3 RS Combined with Information-Enhancing Techniques for the Identification

of Dyes and Pigments ............................................................................................ 61

4.3.1 Subtracted Shifted Resonance RS ................................................................. 61

4.3.2 RS Combined with Light Microscopy .............................................................. 61

5. Spectrometry in the Ultraviolet and Visible Regions ............................................................... 65

5.1 Fundamentals ........................................................................................................ 65

5.2 Antioxidants ........................................................................................................... 65

5.3 Light Stabilizers ..................................................................................................... 67

5.4 Pigments ................................................................................................................ 67

5.5 Plasticizers ............................................................................................................ 68

6. Nuclear Magnetic Resonance Spectrometry .......................................................................... 71

6.1 Fundamentals ........................................................................................................ 71

6.2 Applications ........................................................................................................... 71

7. Mass Spectrometry .................................................................................................................. 73

7.1 Fundamentals ........................................................................................................ 73

7.1.1 Mass Separation ............................................................................................ 73

7.1.2 Ionization ........................................................................................................ 73

7.1.3

Ion Detection ..................................................................................................

7.2

Mass Spectrometry with Electron Impact Ionization (EIMS) ...................................

7.3

Mass Spectrometry with Low-Fragmentation Ionization .........................................

7.3.1

(Pyrolysis-) Field Ionization (FI) and Field Desorption Mass

Spectrometry (Py-FIMS, FDMS) .....................................................................

7.3.2

Chemical Ionization Mass Spectrometry (CIMS) ............................................

7.3.3

Fast-Atom Bombardment Mass Spectrometry (FAB-MS) ..............................

7.3.4

Laser-Desorption Mass Spectrometry ............................................................

7.3.4.1 Matrix-Assisted Laser-Desorption Ionization Time-of-Flight

(MALDI-TOF) Mass Spectrometry ....................................................

7.3.4.2 Laser-Desorption FT-Ion Cyclotron Resonance (LD/FT-ICR)

Mass Spectrometry ...........................................................................

7.4

Mass Spectrometry with Pre-Separated Mixtures (GC-, HPLC-, TLC-MS) .............

7.4.1

On-Line Coupling of GC with Mass Spectrometry (GC-MS) ..........................

7.4.2

On-Line Coupling of Separation Techniques for Non-Volatile

Substances with Mass Spectrometry .............................................................

7.4.3

A Typical Investigation ...................................................................................

This page has been reformatted by Knovel to provide easier navigation.

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