9781574446418

Applied Pyrolysis Handbook

by ;
  • ISBN13:

    9781574446418

  • ISBN10:

    157444641X

  • Edition: 2nd
  • Format: Hardcover
  • Copyright: 2006-12-13
  • Publisher: CRC Press

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Summary

Analytical pyrolysis allows scientists to use routine laboratory instrumentation for analyzing complex, opaque, or insoluble samples more effectively than other analytical techniques alone. Applied Pyrolysis Handbook, Second Edition is a practical guide to the application of pyrolysis techniques to various samples and sample types for a diversity of fields including microbiology, forensic science, industrial research, and environmental analysis.This second edition incorporates recent technological advances that increase the technique's sensitivity to trace elements, improve its reproducibility, and expand its applicability. The book reviews the types of instrumentation available to perform pyrolysis and offers guidance for interfacing instruments and integrating other analytical techniques, including gas chromatography and mass spectrometry. Fully updated with new sample pyrograms, figures, references, and real-world examples, this edition also highlights new areas of application including surfactants, historical artifacts, and environmental materials.This book illustrates how the latest advances make pyrolysis a practical, cost-effective, reliable, and flexible alternative for increasingly complex sample analyses. Applied Pyrolysis Handbook, Second Edition is an essential, one-stop guide for determining if pyrolysis meets application-specific needs as well as performing pyrolysis and handling the data obtained.

Table of Contents

Chapter 1 Analytical Pyrolysis: An Overview 1
Thomas P. Wampler
1.1 Introduction
1
1.2 Degradation Mechanisms
2
1.2.1 Random Scission
2
1.2.2 Side Group Scission
5
1.2.3 Monomer Reversion
6
1.2.4 Relative Bond Strengths
6
1.2.4.1 Polyolefins
7
1.2.4.2 Vinyl Polymers
8
1.2.4.3 Acrylates and Methacrylates
8
1.3 Examples and Applications
9
1.3.1 Forensic Materials
9
1.3.2 Fibers and Textiles
11
1.3.3 Paper, Ink, and Photocopies
13
1.3.4 Art Materials and Museum Pieces
16
1.3.5 Synthetic Polymers
18
1.3.6 Natural Materials and Biologicals
19
1.3.7 Paints and Coatings
22
1.3.8 Trace-Level Analyses
22
References
24
Chapter 2 Instrumentation and Analysis 27
Thomas P. Wampler
2.1 Introduction
28
2.2 Pyrolysis Instruments
28
2.2.1 General Considerations
28
2.3 Analytical Pyrolysis at Rapid Rates
29
2.3.1 Furnace Pyrolyzers
29
2.3.1.1 Design
30
2.3.1.2 Sample Introduction
30
2.3.1.3 Temperature Control
31
2.3.1.4 Advantages of Furnace Pyrolyzers
31
2.3.1.5 Disadvantages of Isothermal Furnaces
32
2.3.2 Heated Filament Pyrolyzers
32
2.3.3 Inductively Heated Filaments: The Curie-Point Technique
33
2.3.3.1 Design
33
2.3.3.2 Sample Introduction
34
2.3.3.3 Temperature Control
35
2.3.3.4 Advantages of Curie-Point Systems
35
2.3.3.5 Disadvantages of Curie-Point Systems
35
2.3.4 Resistively Heated Filaments
36
2.3.4.1 Design
36
2.3.4.2 Sample Introduction
37
2.3.4.3 Interfacing
38
2.3.4.4 Temperature Control
38
2.3.4.5 Advantages of Resistively Heated Filament Pyrolyzers
39
2.3.4.6 Disadvantages of Resistively Heated Filament Pyrolyzers
39
2.4 Pyrolysis at Slow or Programmed Rates
40
2.4.1 Programmable Furnaces
40
2.4.2 Resistively Heated Filaments at Slow Rates
40
2.5 Off-Line Interfacing
41
2.6 Multistep Analyses
42
2.7 Autosamplers
43
2.7.1 Furnace Autosamplers
43
2.7.2 Curie-Point Autosamplers
43
2.7.3 Resistive Heating Autosamplers
43
2.8 Sample Handling and Reproducibility
44
2.8.1 Sample Size and Shape
44
2.8.2 Homogeneity
44
References
46
Chapter 3 Pyrolysis Mass Spectrometry: Instrumentation, Techniques, and Applications 47
C.J. Maddock and T.W. Ottley
3.1 Introduction
48
3.1.1 History
48
3.1.2 Instrument Design
48
3.1.2.1 Direct Insertion Probes
48
3.1.2.2 Modified GC/MS for Pyrolysis-MS
49
3.1.2.3 Py-MS Instruments
52
3.2 Data Analysis
55
3.2.1 Multivariate Statistics
55
3.2.2 Artificial Neural Networks
57
3.3 Applications
59
3.3.1 Microbial Characterization
59
3.3.2 Organic Geochemistry
59
3.3.3 High-Value Products
59
3.3.4 Forensics
59
3.3.5 Polymers
59
3.4 Sample Preparation
60
3.4.1 Curie-Point Foils and Filament Ribbons
60
3.4.1.1 Soluble Solids
60
3.4.1.2 Insoluble Solids
60
3.4.1.3 Bacteria and Yeasts
61
3.4.1.4 Blood or Blood Cultures
61
3.4.1.5 Liquids
61
3.4.2 Curie-Point Ribbons
62
3.4.3 Curie-Point Wires
62
References
63
Chapter 4 Microstructure of Polyolefins 65
Shin Tsuge and Hajime Ohtani
4.1 Introduction
65
4.2 Instrumentation for Pyrolysis Hydrogenation-Gas Chromatography
65
4.3 Analysis of Polyolefins
66
4.3.1 Short-Chain Branching in LDPE
66
4.3.2 Microstructures of Polypropylenes
71
4.3.3 Sequence Distribution in Ethylene-Propylene Copolymers
77
References
80
Chapter 5 Degradation Mechanisms of Condensation Polymers: Polyesters and Polyamides 81
Hajime Ohtani and Shin Tsuge
5.1 Introduction
81
5.2 Polyesters
81
5.3 Polyamides
89
References
Chapter 6 The Application of Analytical Pyrolysis to the Study of Cultural Materials 105
Alexander Shedrinsky and Norbert S. Baer
6.1 Introduction
105
6.2 Instrumental Considerations
107
6.3 Analysis of Materials
109
6.3.1 Waxes
109
6.3.2 Natural Resins
114
6.3.3 Amber
115
6.3.4 Oils and Fats
119
6.3.5 Synthetic Polymers
121
6.3.6 Siloxanes
124
6.3.7 Proteins
125
References
126
Chapter 7 Environmental Applications of Pyrolysis 133
T.O. Munson
7.1 Introduction
134
7.2 Applications Related to Air
134
7.2.1 Examination of Air Particulates/Aerosols
135
7.2.1.1 Smoke Aerosols
135
7.2.1.2 Airborne Particulates
136
7.2.1.3 Organics in Urban Airborne Particles
141
7.2.1.4 Bioaerosols
141
7.2.1.5 Chloroorganic Compounds in Precipitation
141
7.2.2 Examination of Air Pollutants from Thermal Decomposition
142
7.2.2.1 Pyrolysis of Plastic Wrapping Film
142
7.2.2.2 Waste Plastic Processing
143
7.2.2.3 Pyrolysis of Sewage Sludge
146
7.3 Applications Related to Water
147
7.3.1 Wastewater
147
7.3.1.1 Measuring the Organic Carbon in Wastewater
147
7.3.1.2 Analysis of Pulp Mill Effluents Entering the Rhine River
147
7.3.2 Surfacewater: Analysis of Natural Organic Matter
150
7.3.3 Analysis of Groundwater Contamination
154
7.4 Analysis of Soil and Sediment
156
7.4.1 Thermal Distillation-Pyrolysis-GC
156
7.4.2 Flash Pyrolysis-GC and GC/MS
157
7.4.3 TD-Py-FID Applied to Marine Sediments
161
7.4.4 Rock Eval Pyrolysis
163
7.4.5 TMAH-Pyrolysis-GC/MS
164
7.5 Other Environmental Applications
164
7.5.1 Ancient Limestone: Examination by Py-GC and Py-GC/MS
164
7.5.2 Outdoor Bronze Monuments: Examination of Corrosion Patinas by Py-GC/MS
166
7.5.3 Digested and Undigested Pollens: Discrimination by Py-MS
169
7.5.4 Spruce Needles: Examination by Py-FIMS
170
7.5.5 Forest Soils: Examination by Py-MBMS
170
7.5.6 Analysis of Intractable Environmental Contamination
171
References
171
Chapter 8 Examination of Forensic Evidence 175
John M. Challinor
8.1 Introduction
176
8.1.1 The Analysis Challenge
176
8.1.2 Types of Evidence
176
8.1.3 Development of Py-GC
176
8.1.4 Pyrolysis Derivatization: Modifications to the Pyrolysis Process
177
8.2 Paint
177
8.2.1 Automotive Paint
177
8.2.1.1 Repainted Vehicles
178
8.2.1.2 Alkyd-Based Enamels
179
8.2.2 Architectural Paint
180
8.2.3 Industrial Paints
182
8.3 Adhesives
183
8.3.1 Intraclass Differentiation
185
8.4 Rubbers
185
8.5 Plastics
185
8.6 Motor Vehicle Body Fillers
187
8.7 Fibers
188
8.8 Oils and Fats
189
8.9 Cosmetics
192
8.10 Natural Resins: Ancient and Modern Applications
193
8.11 Inks
196
8.12 Miscellaneous
197
8.13 Case Study
197
8.14 Conclusions
197
References
198
Chapter 9 Characterization of Microorganisms by Pyrolysis-GC, Pyrolysis-GC/MS, and Pyrolysis-MS 201
Stephen L. Morgan, Bruce E. Watt, and Randolph C. Galipo
9.1 Introduction
201
9.2 Microbial Chemotaxonomy
203
9.3 Practical Aspects
208
9.3.1 Microbial Sample Handling
208
9.3.2 Analytical Pyrolysis Techniques for Microorganisms
210
9.3.3 Chromatographic Separation and Mass Spectrometric Detection of Pyrolysis Products from Microorganisms
213
9.4 Selected Applications
216
9.4.1 Discrimination of Gram Positive and Gram Negative Bacteria
216
9.4.2 Analysis of Gram Positive Organisms
220
9.4.3 Analysis of Gram Negative Organisms
224
9.4.4 Analysis of Fungi
227
9.5 Conclusions
227
References
229
Chapter 10 Analytical Pyrolysis of Polar Macromolecules 233
Charles Zawodny and Karen Jansson
10.1 Introduction
233
10.2 Synthetic Polymers
234
10.2.1 Poly (methacrylates)
234
10.2.2 Polyesters
237
10.3 Surfactants
240
10.4 Sulfur-Containing Macromolecules
243
10.5 Natural Polymers
244
10.5.1 Cellulose
244
10.5.2 Chitin and Chitosan
245
10.5.3 Proteins
246
10.6 Summary
246
References
248
Chapter 11 Characterization of Condensation Polymers by Pyrolysis-GC in the Presence of Organic Alkali 249
Hajime Ohtani and Shin Tsuge
11.1 Introduction
249
11.2 Measuring System and Procedure
250
11.3 Applications
251
11.3.1 Fully Aromatic Polyester (Compositional Analysis)
251
11.3.2 Aliphatic Polyesters (Compositional Analysis/Biodegradability)
252
11.3.3 Polycarbonate (Composition/End Group)
256
11.3.4 Thermally Treated Polycarbonate/Polyester (Branching and Cross-Linking)
259
11.3.5 UV-Cured Resin (Cross-Linking Network)
266
11.3.6 Poly(Aryl Ether Sulfone)
266
References
269
Chapter 12 Index of Sample Pyrograms 271
Thomas P. Wampler
Index 285

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