Analytical pyrolysis allows scientists to use routine laboratory instrumentation for analyzing complex, opaque, or insoluble samples more effectively than other analytical techniques alone. Analytical Pyrolysis Handbook, Third 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.
The much-anticipated third 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 cultural materials, forensic analysis, and environmental studies.
This book illustrates how the latest advances make pyrolysis a practical, cost-effective, reliable, and flexible alternative for increasingly complex sample analyses. Analytical Pyrolysis Handbook, Third 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.
Author(s): Karen D. Sam and Thomas P. Wampler
Edition: 3
Publisher: CRC Press
Year: 2020
Cover
Half Title
Title Page
Copyright Page
Contents
Preface
Editors
List of Contributors
1. Analytical Pyrolysis: An Overview
I. Introduction
II. Degradation Mechanisms
A. Random Scission
B. Side Group Scission
C. Monomer Reversion
D. Relative Bond Strengths
1. Polyolefins
2. Vinyl Polymers
3. Acrylates and Methacrylates
III. Examples and Applications
A. Forensic Materials
B. Fibers and Textiles
C. Paper, Ink, and Photocopies
D. Art Materials and Museum Pieces
E. Synthetic Polymers
F. Natural Materials and Biologicals
G. Paints and Coatings
H. Trace Level Analyses
References
2. Instrumentation and Analysis
I. Introduction
II. Pyrolysis Instruments
A. General Considerations
III. Analytical Pyrolysis at Rapid Rates
A. Furnace Pyrolyzers
1. Design
2. Sample Introduction
3. Temperature Control
4. Advantages of Furnace Pyrolyzers
5. Disadvantages of Isothermal Furnaces
B. Heated Filament Pyrolyzers
C. Inductively Heated Filaments: The Curie-Point Technique
1. Design
2. Sample Introduction
3. Temperature Control
4. Advantages of Curie-Point Systems
5. Disadvantages of Curie-Point Systems
D. Resistively Heated Filaments
1. Design
2. Sample Introduction
3. Interfacing
4. Temperature Control
5. Advantages of Resistively Heated Filament Pyrolyzers
6. Disadvantages of Resistively Heated Filament Pyrolyzers
IV. Pyrolysis at Slow or Programmed Rates
A. Programmable Furnaces
B. Resistively Heated Filaments at Slow Rates
V. Off-Line Interfacing
VI. Multi-Step Analyses
VII. Auto-Samplers
A. Furnace Autosamplers
B. Curie-Point Auto-Samplers
C. Resistive Heating Autosamplers
VIII. Sample Handling and Reproducibility
A. Sample Size and Shape
B. Homogeneity
References
3. Pyrolysis Mass Spectrometry: Instrumentation, Techniques, and Applications
I. Introduction
A. History
B. Instrument Design
1. Direct Insertion Probes
2. Atmospheric Pressure Interfaces
3. Modified GC/MS for Pyrolysis-MS
4. PyMS Instruments
II. Data Analysis
A. Multivariate Statistics
B. Artificial Neural Networks
III. Applications
A. Microbial Characterization
B. Organic Geochemistry
C. High-Value Products
D. Forensics
E. Polymers
IV. Sample Preparation
A. Curie-Point Foils and Filament Ribbons
1. Soluble Solids
2. Insoluble Solids
3. Bacteria and Yeasts
4. Blood or Blood Cultures
5. Liquids
B. Curie-Point Ribbons
C. Curie-Point Wires
References
4. Microstructure of Polyolefins
I. Introduction
II. Instrumentation for Pyrolysis Hydrogenation-Gas Chromatography
III. Analysis of Polyolefins
A. Short-Chain Branching in LDPE
B. Microstructures of Polypropylenes
C. Sequence Distribution in Ethylene-Propylene Copolymers
References
5. Degradation Mechanisms of Condensation Polymers: Polyesters and Polyamides
I. Introduction
II. Polyesters
III. Polyamide
References
6. The Application of Analytical Pyrolysis to the Study of Cultural Materials
I. Introduction
II. Instrumental Consideration
III. Analysis of Materials
A. Usual Natural Materials: Oils, Wax, Resins, Gums, and Proteins
B. Amber and Bitumen
C. Lacquers
D. Modern Paints
E. Synthetic Organic Pigments
F. Additives
G. Plastics
IV. Conclusion
References
7. Environmental Applications of Pyrolysis
I. Introduction
II. Applications Related to Air
A. Examination of Air Particulates/Aerosols
1. Smoke Aerosols
2. Airborne Particulates
3. Organics in Urban Airborne Particles
4. Bioaerosols
5. Chloroorganic Compounds in Precipitation
B. Examination of Air Pollutants from Thermal Decomposition
1. Pyrolysis of Plastic Wrapping Film
2. Waste Plastic Processing
3. Pyrolysis of Sewage Sludge
III. Applications Related to Water
A. Wastewater
1. Measuring the Organic Carbon in Wastewater
2. Analysis of Pulp Mill Effluents Entering the Rhine River
B. Surfacewater: Analysis of Natural Organic Matter
C. Analysis of Groundwater Contamination
IV. Analysis of Soil and Sediment
A. Thermal Distillation-Pyrolysis-GC
B. Flash Pyrolysis-GC and GC/MS
C. Pyrolysis of Sewage Sludge to Produce Biochar
D. Soil Organic Matter (SOM)
E. TD-Py-FID Applied to Marine Sediments
F. Rock-Eval Pyrolysis
G. TMAH-Pyrolysis-GC/MS
V. Other Environmental Applications
A. Ancient Limestone - Examination by Py-GC and Py-GC/MS
B. Outdoor Bronze Monuments - Examination of Corrosion Patinas by Py-GC/MS
C. Digested and Undigested Pollens - Discrimination by Py-MS
D. Spruce Needles - Examination by Py-FIMS
E. Forest Soils - Examination by Py-MBMS
F. Analysis of Intractable Environmental Contamination
G. Plastic Pollution
References
8. Examination of Forensic Evidence
I. Introduction
A. The Analysis Challenge
B. Types of Evidence
C. Development of Py-GC
D. "Pyrolysis Derivatization" - modifications to the pyrolysis process
II. Paint
A. Automotive Paint
Repainted Vehicles
Alkyd-Based Enamels
B. Architectural Paint
C. Industrial Paints
III. Adhesives
III. A Intraclass Differentiation
IV. Rubbers
V. Plastics
VI. Motor Vehicle Body Fillers
VII. Fibers
VIII. Oils and Fats
IX. Cosmetics
X. Personal Lubricants
XI. Natural Resins - Ancient and Modern Applications
XII. Inks
XIII. Miscellaneous
XIV. Case Study
XV. Conclusions
References
9. Characterization of Microorganisms by Pyrolysis-GC, Pyrolysis-GC/MS, and Pyrolysis-MS
I. Introduction
II. Microbial Chemotaxonomy
III. Practical Aspects
A. Microbial Sample Handling
B. Analytical Pyrolysis Techniques for Microorganisms
C. Chromatographic Separation and Mass Spectrometric Detection of Pyrolysis Products from Microorganisms
IV. Selected Applications
A. Discrimination of Gram-Positive and Gram-Negative Bacteria
B. Analysis of Gram-Positive Organisms
C. Analysis of Gram-Negative Organisms
D. Analysis of Fungi
V. Conclusions
References
10. Analytical Pyrolysis of Polar Macromolecules*
I. Introduction
II. Synthetic Polymers
A. Acrylics
B. Polyesters
C. Water-Soluble Polymers
III. Surfactants
IV. Sulfur-Containing Macromolecules
V. Nitrogen-Containing Polymers
VI. Natural Polymers
A. Proteins
B. Cellulose and Lignin
C. Chitin and Chitosan
VII. Summary
References
11. Characterization of Condensation Polymers by Thermally Assisted Hydrolysis and Methylation-GC
I. Introduction
II. Measurement System and Procedure
III. Applications
A. Fully Aromatic Polyester (Compositional Analysis)
B. Aliphatic Polyesters (Compositional Analysis/Biodegradability)
C. Polycarbonate (Composition/End Group)
D. Thermally Treated Polycarbonate/Polyester (Branching and Cross-Linking)
E. UV-Cured Resin (Cross-Linking Network)
F. Poly(Aryl Ether Sulfone)
References
12. Index of Sample Pyrograms
Index
