Undergraduate Instrumental Analysis 8th Edition by Thomas Bruno, James Robinson, Eileen Skelly Frame, George Frame 1032036915 9781032036915

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ISBN 10: 1032036915

ISBN 13: 9781032036915

Author: Thomas J. Bruno, James W. Robinson, Eileen M. Skelly Frame, George M. Frame

Analytical instrumentation is crucial to research in molecular biology, medicine, geology, food science, materials science, forensics, and many other fields. Undergraduate Instrumental Analysis, 8th Edition, provides the reader with an understanding of all major instrumental analyses, and is unique in that it starts with the fundamental principles, and then develops the level of sophistication that is needed to make each method a workable tool for the student. Each chapter includes a discussion of the fundamental principles underlying each technique, detailed descriptions of the instrumentation, and a large number of applications. Each chapter includes an updated bibliography and problems, and most chapters have suggested experiments appropriate to the technique. This edition has been completely updated, revised, and expanded. The order of presentation has been changed from the 7th edition in that after the introduction to spectroscopy, UV-Vis is discussed. This order is more in keeping with the preference of most instructors. Naturally, once the fundamentals are introduced, instructors are free to change the order of presentation. Mathematics beyond algebra is kept to a minimum, but for the interested student, in this edition we provide an expanded discussion of measurement uncertainty that uses elementary calculus (although a formula approach can be used with no loss of context). Unique among all instrumental analysis texts we explicitly discuss safety, up front in Chapter 2. The presentation intentionally avoids a finger-wagging, thou-shalt-not approach in favor of a how-to discussion of good laboratory and industrial practice. It is focused on hazards (and remedies) that might be encountered in the use of instrumentation. Among the new topics introduced in this edition are: • Photoacoustic spectroscopy. • Cryogenic NMR probes and actively shielded magnets. • The nature of mixtures (in the context of separations). • Troubleshooting and leaks in high vacuum systems such as mass spectrometers. • Instrumentation laboratory safety. • Standard reference materials and standard reference data. In addition, the authors have included many instrument manufacturer’s websites, which contain extensive resources. We have also included many government websites and a discussion of resources available from National Measurement Laboratories in all industrialized countries. Students are introduced to standard methods and protocols developed by regulatory agencies and consensus standards organizations in this context as well.

Undergraduate Instrumental Analysis 8th Table of contents:

Chapter 1 Concepts of Instrumental Analytical Chemistry

1.1 Introduction: What Is Analytical Chemistry?

1.1.1 The Difference between Weight and Mass

1.2 Analytical Approach

1.2.1 Defining the Problem

1.2.2 Designing the Analytical Method

1.2.3 Sampling

1.2.4 Storage of Samples

1.3 A Conceptual Discussion About Uncertainty in Measurements

1.4 BASIC Statistics and Data Handling

1.4.1 Significant Figures

1.4.2 Accuracy and Precision

1.4.3 Types of Errors

1.4.4 Definitions for Statistics

1.4.5 Quantifying Random Error

1.4.6 Detection of Outliers

1.4.7 Expressing Uncertainty

1.5 Sample Preparation

1.5.1 Acid Dissolution and Digestion

1.5.2 Fusions

1.5.3 Dry Ashing and Combustion

1.5.4 Extraction

1.6 Performing the Measurement

1.6.1 Signals and Noise

1.6.2 Plotting Calibration Curves

1.7 Assessing The Data

1.7.1 Limit of Detection

1.7.2 Limit of Quantitation

1.8 Reference Materials and Reference Data

1.8.1 Reference Materials

1.8.2 Reference Data

Problems

Bibliography

Chapter 2 Safety in the Instrumentation Laboratory

2.1 Electrical Hazards and Safety

2.1.1 Electrical Lines, Receptacles, and Cables

2.1.2 PAT Testing Procedures in the U.K.

2.1.3 Electrical Shocks

2.1.4 Batteries

2.1.5 Portable Generators

2.1.6 A Brief Discussion about Ground

2.2 Instrument Cooling

2.3 Compressed Gas Cylinder Safety

2.3.1 Compressed Gas Regulators and Manifolds

2.3.2 Gas Cylinder Markings

2.4 Cryogenic Fluid Safety

2.4.1 Cryogenic Fluids

2.4.2 Cryogenic Liquid Containers

2.5 The Use of Fume Hoods in the Instrumentation Laboratory

2.6 Laser Safety

2.7 Compressed Air Line Safety

2.8 Ladder Safety

2.8.1 Step Ladders

2.8.2 Straight, Combination, and Extension Ladders

2.9 Hearing Protection

2.10 Selection of Laboratory Gloves

2.11 Selection of Respirator Cartridges and Filters

2.12 Safety with Nanomaterials

2.13 Relative Dose Ranges from Ionizing Radiation

2.14 Magnetic Field Safety

2.15 Miscellaneous Hazardous Conditions and Fire Safety

2.15.1 Fire Extinguishers

2.15.2 Hot Work Permits

2.16 Stop Work Orders

References

Chapter 3 Introduction to Spectroscopy

3.1 Interaction Between Electromagnetic Radiation and Matter

3.1.1 What Is Electromagnetic Radiation?

3.1.2 How Does Electromagnetic Radiation Interact with Matter?

3.2 Atoms and Atomic Spectroscopy

3.3 Molecules and Molecular Spectroscopy

3.3.1 Rotational Transitions in Molecules

3.3.2 Vibrational Transitions in Molecules

3.3.3 Electronic Transitions in Molecules

3.4 Absorption Laws

3.4.1 Deviations from Beer’s Law

3.5 Methods of Calibration

3.5.1 Calibration with Standards

3.5.2 Method of Standard Additions

3.5.3 Internal Standard Calibration

3.5.4 Errors Associated with Beer’s Law Relationships

3.6 Optical Systems used in Spectroscopy

3.6.1 Radiation Sources

3.6.2 Wavelength Selection Devices

3.6.3 Optical Slits

3.6.4 Detectors

3.6.5 Single-Beam and Double-Beam Optics

3.6.6 Dispersive Optical Layouts

3.6.7 Fourier Transform Spectrometers

3.7 Spectroscopic Technique and Instrument Nomenclature

Suggested Experiments

Problems

Bibliography

Chapter 4 Visible and Ultraviolet Molecular Spectroscopy

4.1 Introduction

4.1.1 Electronic Excitation in Molecules

4.1.2 Absorption by Molecules

4.1.3 Molar Absorptivity

4.1.4 Shape of UV Absorption Curves

4.1.5 Solvents for UV/VIS Spectroscopy

4.2 Instrumentation

4.2.1 Optical System

4.2.2 Radiation Sources

4.2.3 Monochromators

4.2.4 Detectors

4.2.5 Sample Holders

4.2.6 Microvolume, Nanovolume, and Handheld UV/VIS Spectrometers

4.3 UV Absorption Spectra of Molecules

4.3.1 Solvent Effects on UV Spectra

4.4 UV Spectra and The Structure of Organic Molecules

4.4.1 Conjugated Diene Systems

4.4.2 Conjugated Ketone Systems

4.4.3 Substitution of Benzene Rings

4.5 Analytical Applications

4.5.1 Qualitative Structural Analysis

4.5.2 Quantitative Analysis

4.5.3 Multicomponent Determinations

4.5.4 Other Applications

4.5.5 Measurement of Color

4.6 Accuracy and Precision in UV/VIS Absorption Spectrometry

4.7 Nephelometry and Turbidimetry

4.8 Molecular Emission Spectrometry

4.8.1 Fluorescence and Phosphorescence

4.8.2 Relationship between Fluorescence Intensity and Concentration

4.9 Instrumentation for Luminescence Measurements

4.9.1 Wavelength Selection Devices

4.9.2 Radiation Sources

4.9.3 Detectors

4.9.4 Sample Cells

4.9.5 Spectrometer Systems

4.10 Analytical Applications of Luminescence

4.10.1 Advantages of Fluorescence and Phosphorescence

4.10.2 Disadvantages of Fluorescence and Phosphorescence

Suggested Experiments

Problems

BIbliography

Chapter 5 Infrared, Near-Infrared, Raman, and Photoacoustic Spectroscopy

5.1 Absorption of IR Radiation by Molecules

5.1.1 Dipole Moments in Molecules

5.1.2 Types of Vibrations in Molecules

5.1.3 Vibrational Motion

5.2 IR Instrumentation

5.2.1 Radiation Sources

5.2.2 Monochromators and Interferometers

5.2.3 Detectors

5.2.4 Detector Response Time

5.3 Sampling Techniques

5.3.1 Techniques for Transmission (Absorption) Measurements

5.3.2 Background Correction in Transmission Measurements

5.3.3 Techniques for Reflectance and Emission Measurements

5.4 Ftir Microscopy

5.5 Nondispersive Ir SYSTEMS

5.6 Analytical Applications of IR Spectroscopy

5.6.1 Qualitative Analyses and Structural Determination by Mid-IR Absorption Spectroscopy

5.6.2 Quantitative Analyses by IR Spectrometry

5.7 NIR Spectroscopy

5.7.1 Instrumentation

5.7.2 NIR Vibrational Bands, Spectral Interpretation, and Calibration

5.7.3 Sampling Techniques for NIR Spectroscopy

5.7.4 Applications of NIR Spectroscopy

5.8 Raman Spectroscopy

5.8.1 Principles of Raman Scattering

5.8.2 Raman Instrumentation

5.8.3 Applications of Raman Spectroscopy

5.8.4 Resonance Raman Effect

5.8.5 Surface-Enhanced Raman Spectroscopy

5.8.6 Raman Microscopy

5.9 Chemical Imaging using NIR, IR, and Raman Spectroscopy

5.10 Photoacoustic Spectoscopy

Suggested Experiments

Problems

Bibliography

Chapter 6 Magnetic Resonance Spectroscopy

6.1 Introduction to Nuclear Magnetic Resonance Spectroscopy

6.1.1 Properties of Nuclei

6.1.2 Quantization of 1H Nuclei in a Magnetic Field

6.1.3 Width of Absorption Lines

6.2 FT-NMR Experiment

6.3 Chemical Shifts

6.4 Spin–Spin Coupling

6.5 Instrumentation

6.5.1 Sample Holder

6.5.2 Sample Probe

6.5.3 Magnet

6.5.4 RF Generation and Detection

6.5.5 Signal Integrator and Computer

6.6 Analytical Applications of NMR

6.6.1 Samples and Sample Preparation for NMR

6.6.2 Qualitative Analyses: Molecular Structure Determination

6.6.3 Interpretation of Proton Spectra

6.6.4 13C NMR

6.6.5 2D NMR

6.6.6 Qualitative Analyses: Other Applications

6.6.7 Quantitative Analyses

6.7 Hyphenated NMR Techniques

6.8 NMR Imaging and MRI

6.9 TIME Domain NMR

6.9.1 Solid Fat Content Determination by TD-NMR

6.9.2 Field Homogeneity and Spin Echo

6.9.3 Relaxation Time Distribution

6.9.4 TD-NMR Applications

6.10 Low-Field, Portable, and Miniature NMR Instruments

6.11 Limitations of NMR

6.12 Electron Spin Resonance Spectroscopy

6.12.1 Instrumentation

6.12.2 Miniature ESR Spectroscopy

6.12.3 ESR Spectra and Hyperfine Interactions

6.12.4 Applications

6.12.5 CW-Endor

Suggested Experiments

Problems

Bibliography

Chapter 7 Atomic Absorption Spectrometry

7.1 Absorption of Radiant Energy by Atoms

7.1.1 Spectral Linewidth

7.1.2 Degree of Radiant Energy Absorption

7.2 Instrumentation

7.2.1 Radiation Sources

7.2.2 Atomizers

7.2.3 Spectrometer Optics

7.2.4 Detectors

7.2.5 Modulation

7.2.6 Commercial AAS Systems

7.3 Atomization Process

7.3.1 Flame Atomization

7.3.2 Graphite Furnace Atomization

7.4 Interferences in AAS

7.4.1 Nonspectral Interferences

7.4.2 Spectral Interferences

7.5 Analytical Applications of AAS

7.5.1 Qualitative Analysis

7.5.2 Quantitative Analysis

7.5.3 Analysis of Samples

Suggested Experiments

Problems

7.A Appendix

7.B Appendix

Bibliography

Chapter 8 Atomic Emission Spectroscopy

8.1 Flame Atomic Emission Spectroscopy

8.1.1 Instrumentation for Flame OES

8.1.2 Interferences

8.1.3 Analytical Applications of Flame OES

8.2 Atomic OES

8.2.1 Instrumentation for Emission Spectroscopy

8.2.2 Interferences in Arc and Spark Emission Spectroscopy

8.2.3 Applications of Arc and Spark Emission Spectroscopy

8.3 Plasma Emission Spectroscopy

8.3.1 Instrumentation for Plasma Emission Spectrometry

8.3.2 Interferences and Calibration in Plasma Emission Spectrometry

8.3.3 Applications of ICP, DCP, and MP Atomic Emission Spectroscopy

8.3.4 Chemical Speciation with Hyphenated Instruments

8.4 GD Emission Spectrometry

8.4.1 DC and RF GD Sources

8.4.2 Applications of GD Atomic Emission Spectrometry

8.5 Atomic Fluorescence Spectroscopy

8.5.1 Instrumentation for AFS

8.5.2 Interferences in AFS

8.5.3 Applications of AFS

8.6 Commercial Atomic Emission SYSTEMS

8.6.1 Arc and Spark Systems

8.6.2 ICP, DCP, and MP Systems

8.6.3 GD Systems

8.6.4 AFS Systems

8.7 Laser-Induced Breakdown Spectroscopy

8.7.1 Principle of Operation

8.7.2 Instrumentation

8.7.3 Applications of LIBS

8.7.4 Commercial LIBS Systems

8.8 Atomic Emission Literature and Resources

8.9 Comparison of Atomic Spectroscopic and ICP-MS Techniques

Suggested Experiments

Flame Emission

Arc/Spark or ICP Emission

ICP Emission

PROBLEMS

8.A Appendix

8.B Appendix: Comparison of Atomic Spectroscopic Analytical Techniques

8.B.1 Flame Atomic Absorption

8.B.2 GFAAS

8.B.3 ICP-OES

8.B.4 ICP-MS

8.B.5 LIBS

Bibliography

Chapter 9 X-Ray Spectroscopy1

9.1 Origin of X-Ray Spectra

9.1.1 Energy Levels in Atoms

9.1.2 Moseley’s Law

9.1.3 X-Ray Methods

9.2 X-Ray Fluorescence

9.2.1 X-Ray Source

9.2.2 Instrumentation for Energy-Dispersive X-Ray Spectrometry

9.2.3 Instrumentation for Wavelength-Dispersive X-Ray Spectrometry

9.2.4 Simultaneous WDXRF Spectrometers

9.2.5 Micro-XRF Instrumentation

9.2.6 Total Reflection XRF

9.2.7 Comparison between EDXRF and WDXRF

9.2.8 XRF Applications

9.3 X-RAY Absorption

9.3.1 EXAFS

9.4 X-Ray Diffraction

9.4.1 Single-Crystal X-Ray Diffractometry

9.4.2 Crystal Growing

9.4.3 Crystal Structure Determination

9.4.4 Powder X-Ray Diffractometry

9.4.5 Hybrid XRD/XRF Systems

9.4.6 Applications of XRD

9.5 X-Ray Emission

9.5.1 Electron Probe Microanalysis

9.5.2 Particle-Induced X-Ray Emission

9.6 Commercial X-Ray Instrument Manufacturers

Suggested Experiments/Tutorials

X-Ray Absorption

X-Ray Fluorescence

X-Ray Diffraction

Problems

9.A Appendix: Characteristic x-ray Wavelengths (Å) and Energies (KEV)*

9.B Appendix: Absorption Edge Wavelengths and Energies

Notes

BIBLIOGRAPHY

Chapter 10 Mass Spectrometry I: Principles and Instrumentation

10.1 Principles of MS

10.1.1 Resolving Power and Resolution of a Mass Spectrometer

10.2 Instrumentation

10.2.1 Sample Input Systems

10.2.2 Ionization Sources

10.2.3 Mass Analyzers

10.2.4 Detectors

10.3 Ion Mobility SPECTROMETRY

10.3.1 Handheld DMS JUNO® Chemical Trace Vapor Point Detector

10.3.2 Excellims HPIMS-LC System

10.3.3 Photonis Ion Mobility Spectrometer Engine

10.3.4 SYNAPT G2-S Multistage MS System Incorporating the TriWAVE Ion Mobility Stage

10.4 Leaks in Mass Spectrometer Systems

Problems

Bibliography

Chapter 11 Mass Spectrometry II Spectral Interpretation and Applications

11.1 Interpretation of Mass Spectra: Structural Determination of Simple Molecules

11.1.1 Molecular Ion and Fragmentation Patterns

11.1.2 Nitrogen Rule

11.1.3 Molecular Formulas and Isotopic Abundances

11.1.4 Compounds with Heteroatoms

11.1.5 Halogen Isotopic Clusters

11.1.6 Rings Plus Double Bonds

11.1.7 Common Mass Losses on Fragmentation

11.2 MASS SPECTRAL INTERPRETATION: SOME EXAMPLES

11.2.1 Mass Spectra of Hydrocarbons

11.2.2 Mass Spectra of Other Organic Compound Classes

11.2.3 Compounds Containing Heteroatoms

11.3 APPLICATIONS OF MOLECULAR MS

11.3.1 High-Resolution Mass Spectrometry

11.3.2 Quantitative Analysis of Compounds and Mixtures

11.3.3 Protein-Sequencing Analysis (Proteomics)

11.3.4 Gas Analysis

11.3.5 Environmental Applications

11.3.6 Other Applications of Molecular MS

11.3.7 Limitations of Molecular MS

11.4 ATOMIC MS

11.4.1 ICP-MS

11.4.2 Applications of Atomic MS

11.4.3 Interferences in Atomic MS

11.4.4 Instrumental Approaches to Eliminating Interferences

11.4.5 Limitations of Atomic MS

11.5 Common Spurious Effects in Mass Spectrometry

Problems

11.A Appendix

BIBLIOGRAPHY

Chapter 12 Principles of Chromatography

12.1 Introduction to Chromatography

12.2 The Nature of Mixtures

12.3 What Is the Chromatographic Process?

12.4 Chromatography in More Than one Dimension

12.5 Visualization of The Chromatographic Process At The Molecular Level: Analogy To “People on A Moving Belt Slideway”

12.6 DIGRESSION ON THE CENTRAL ROLE OF SILICON–OXYGEN COMPOUNDS IN CHROMATOGRAPHY

12.7 BASIC EQUATIONS DESCRIBING CHROMATOGRAPHIC SEPARATIONS

12.8 HOW DO COLUMN VARIABLES AFFECT EFFICIENCY (PLATE HEIGHT)?

12.9 PRACTICAL OPTIMIZATION OF CHROMATOGRAPHIC SEPARATIONS

12.10 EXTRA-COLUMN BAND BROADENING EFFECTS

12.11 QUALITATIVE CHROMATOGRAPHY: ANALYTE IDENTIFICATION

12.12 QUANTITATIVE MEASUREMENTS IN CHROMATOGRAPHY

12.12.1 Peak Area or Peak Height: What Is Best for Quantitation?

12.12.2 Calibration with an External Standard

12.12.3 Calibration with an Internal Standard

12.13 EXAMPLES OF CHROMATOGRAPHIC CALCULATIONS

PROBLEMS

BIBLIOGRAPHY

Chapter 13 Gas Chromatography

13.1 HISTORICAL DEVELOPMENT OF GC: THE FIRST CHROMATOGRAPHIC INSTRUMENTATION

13.2 ADVANCES IN GC LEADING TO PRESENT-DAY INSTRUMENTATION

13.3 GC INSTRUMENT COMPONENT DESIGN (INJECTORS)

13.3.1 Syringes

13.3.2 Autosamplers

13.3.3 SPME

13.3.4 Split Injections

13.3.5 Splitless Injections

13.4 GC INSTRUMENT COMPONENT DESIGN (THE COLUMN)

13.4.1 Column Stationary Phase

13.4.2 Selecting a Stationary Phase for an Application

13.4.3 Effects of Mobile Phase Choice and Flow Parameters

13.5 GC INSTRUMENT OPERATION (COLUMN DIMENSIONS AND ELUTION VALUES)

13.6 GC INSTRUMENT OPERATION (COLUMN TEMPERATURE AND ELUTION VALUES)

13.7 GC INSTRUMENT COMPONENT DESIGN (DETECTORS)

13.7.1 Thermal Conductivity Detector

13.7.2 Flame Ionization Detector

13.7.3 Electron Capture Detector

13.7.4 Electrolytic Conductivity Detector

13.7.5 Sulfur–Phosphorus Flame Photometric Detector

13.7.6 Sulfur Chemiluminescence Detector

13.7.7 Nitrogen–Phosphorus Detector

13.7.8 Photoionization Detector

13.7.9 Helium Ionization Detector

13.7.10 Atomic Emission Detector

13.8 HYPHENATED GC TECHNIQUES (GC-MS, GC-IR, GC-GC, OR 2D GC)

13.8.1 GC-MS

13.8.2 GC-IR Spectrometry

13.8.3 Comprehensive 2D Gas Chromatography (GC × GC or GC2)

13.9 RETENTION INDICES (A GENERALIZATION OF RELATIVE Rt INFORMATION)

13.10 SCOPE OF GC ANALYSES

13.10.1 GC Behavior of Organic Compound Classes

13.10.2 Derivatization of Difficult Analytes to Improve GC Elution Behavior

13.10.3 Gas Analysis by GC

13.10.4 Limitations of GC

PROBLEMS

13.A APPENDIX: GC INTERNET WEB RESOURCES

Special GC Calculation Programs

Two Large Publisher Chromatography Websites

BIBLIOGRAPHY

Chapter 14 Chromatography with Liquid (and Fluid) Mobile Phases

14.1 HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

14.1.1 HPLC Column and Stationary Phases

14.1.2 Effects on Separation of Composition of the Mobile Phase

14.1.3 Design and Operation of an HPLC Instrument

14.1.4 HPLC Detector Design and Operation

14.1.5 Derivatization in HPLC

14.1.6 Hyphenated Techniques in HPLC

14.1.7 Applications of HPLC

14.2 CHROMATOGRAPHY OF IONS DISSOLVED IN LIQUIDS

14.2.1 Ion Chromatography

14.3 AFFINITY CHROMATOGRAPHY

14.4 SIZE-EXCLUSION CHROMATOGRAPHY

14.5 SUPERCRITICAL FLUID CHROMATOGRAPHY

14.5.1 Operating Conditions

14.5.2 Effect of Pressure

14.5.3 Stationary Phases

14.5.4 Mobile Phases

14.5.5 Detectors

14.5.6 SFC versus Other Column Methods

14.5.7 Applications

14.5.8 Ultra Performance Convergence Chromatography: A New Synthesis

14.6 ELECTROPHORESIS

14.6.1 Capillary Zone Electrophoresis (CZE)

14.6.2 Sample Injection in CZE

14.6.3 Detection in CZE

14.6.4 Modes of CE

14.6.5 Capillary Electrochromatography

14.7 PLANAR CHROMATOGRAPHY AND PLANAR ELECTROPHORESIS

14.7.1 Thin-Layer Chromatography

14.7.2 Planar Electrophoresis on Slab Gels

PROBLEMS AND EXERCISES

14.A APPENDIX LC/CE/TLC INTERNET WEB RESOURCES

Special LC Calculation Programs

Two Large Publisher Chromatography Websites

BIBLIOGRAPHY

Chapter 15 Electroanalytical Chemistry

15.1 FUNDAMENTALS OF ELECTROCHEMISTRY

15.2 ELECTROCHEMICAL CELLS

15.2.1 Line Notation for Cells and Half-Cells

15.2.2 Standard Reduction Potentials

15.2.3 Sign Conventions

15.2.4 Nernst Equation

15.2.5 Activity Series

15.2.6 Reference Electrodes

15.2.7 Electrical Double Layer

15.3 ELECTROANALYTICAL METHODS

15.3.1 Potentiometry

15.3.2 Coulometry

15.3.3 Conductometric Analysis

15.3.4 Polarography

15.3.5 Voltammetry

15.4 LIQUID CHROMATOGRAPHY DETECTORS

15.4.1 Voltammetric Detection

15.4.2 Conductometric Detection

15.5 SPECTROELECTROCHEMISTRY

15.6 QUARTZ CRYSTAL MICROBALANCE

15.6.1 Piezoelectric Effect

15.6.2 Electrochemical Quartz Crystal Microbalance

15.7 ELECTROCHEMISTRY AT THE NANOSCALE

SUGGESTED EXPERIMENTS

PROBLEMS

15.A APPENDIX: SELECTED STANDARD REDUCTION POTENTIALS AT 25 °C

BIBLIOGRAPHY

Chapter 16 Surface Analysis

16.1 INTRODUCTION

16.2 ELECTRON SPECTROSCOPY TECHNIQUES

16.2.1 X-Ray Photoelectron Spectroscopy

16.2.2 Auger Electron Spectroscopy

16.3 ION SCATTERING SPECTROSCOPY

16.4 SECONDARY ION MASS SPECTROMETRY

16.4.1 Instrumentation for SIMS

16.4.2 Analytical Applications of SIMS

16.5 ELECTRON MICROPROBE (ELECTRON PROBE MICROANALYSIS)

PROBLEMS

BIBLIOGRAPHY

Chapter 17 Thermal Analysis

17.1 THERMOGRAVIMETRY

17.1.1 TGA Instrumentation

17.1.2 Analytical Applications of Thermogravimetry

17.1.3 Derivative Thermogravimetry

17.1.4 Sources of Error in Thermogravimetry

17.2 DIFFERENTIAL THERMAL ANALYSIS

17.2.1 DTA Instrumentation

17.2.2 Analytical Applications of DTA

17.3 DIFFERENTIAL SCANNING CALORIMETRY

17.3.1 DSC Instrumentation

17.3.2 Applications of DSC

17.4 HYPHENATED TECHNIQUES

17.4.1 Hyphenated Thermal Methods

17.4.2 Evolved Gas Analysis

17.5 THERMOMETRIC TITRIMETRY

17.5.1 Applications of Thermometric Titrimetry

17.6 DIRECT INJECTION ENTHALPIMETRY

17.7 MICROCALORIMETRY

17.7.1 Micro-DSC Instrumentation

17.7.2 Applications of Micro-DSC

17.7.3 Isothermal Titration Calorimetry

17.7.4 Microliter Flow Calorimetry

17.8 THERMOMECHANICAL ANALYSIS AND DYNAMIC MECHANICAL ANALYSIS

17.8.1 Instrumentation

17.8.2 Applications of TMA and DMA

17.9 OPTICAL THERMAL ANALYSIS

17.9.1 Heating Microscope

17.9.2 Optical Dilatometers

17.9.3 Optical Thermal Analyzers with Differential Thermal Analysis

17.10 SUMMARY

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