Undergraduate Instrumental Analysis: 7th Edition (Pack - Book and Online) book cover

Undergraduate Instrumental Analysis

7th Edition

By James W. Robinson, Eileen Skelly Frame, George M. Frame II

CRC Press

1,264 pages | 895 B/W Illus.

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Description

Crucial to research in molecular biology, medicine, geology, food science, materials science, and many other fields, analytical instrumentation is used by many scientists and engineers who are not chemists. Undergraduate Instrumental Analysis, Seventh Edition provides users of analytical instrumentation with an understanding of these instruments, covering all major fields of modern instrumentation. Following the tradition of earlier editions, this text is designed for teaching undergraduates and those with no analytical chemistry background how contemporary analytical instrumentation works, as well as its uses and limitations.

Each chapter provides a discussion of the fundamental principles underlying the techniques, descriptions of the instrumentation, and numerous applications. The chapters also contain updated bibliographies and problems, and most have suggested experiments appropriate to the techniques. This completely revised and updated edition covers subjects in more detail, such as a completely revised x-ray chapter, expanded coverage of electroanalytical techniques, and expansion of chromatography and mass spectrometry topics to reflect the predominance of these instruments in laboratories. This includes state-of-the-art sample introduction and mass analyzers, and the latest developments in UPLC and hyphenated techniques. The book also contains new graphics and addresses several new topics:

  • Ion mobility spectrometry
  • Time domain NMR (relaxometry)
  • Electron spin resonance spectroscopy (ESR, EPR)
  • Forensic science and bioanalytical applications
  • Microcalorimetry and optical thermal instruments
  • Laser-induced breakdown spectroscopy (LIBS)

This text uniquely combines instrumental analysis with organic spectral interpretation (IR, NMR, and MS). It provides detailed coverage of sampling, sample handling, sample storage, and sample preparation. In addition, the authors have included many instrument manufacturers’ websites, which contain extensive resources.

Table of Contents

Concepts of Instrumental Analytical Chemistry

Introduction: What is Analytical Chemistry?

Analytical Approach

Basic Statistics and Data Handling

Sample Preparation

Performing the Measurement

Assessing the Data

Problems

Bibliography

Introduction to Spectroscopy

Interaction Between Electromagnetic Radiation and Matter

Atoms and Atomic Spectroscopy

Molecules and Molecular Spectroscopy

Absorption Laws

Methods of Calibration

Optical Systems Used in Spectroscopy

Spectroscopic Technique and Instrument Nomenclature

Suggested experiments

Problems

Bibliography

Magnetic Resonance Spectroscopy

Nuclear Magnetic Resonance Spectroscopy Introduction

The FTNMR Experiment

Chemical Shifts

Spin–Spin Coupling

Instrumentation

Analytical Applications of NMR

Hyphenated NMR Techniques

NMR Imaging and MRI

Time Domain NMR

Low-Field, Portable, and Miniature NMR Instruments

Limitations of NMR

Electron Spin Resonance Spectroscopy

Suggested Experiments

Problems

Spectral Databases

Bibliography

Infrared, Near-Infrared, and Raman Spectroscopy

Absorption of IR Radiation by Molecules

IR Instrumentation

Sampling Techniques

FTIR Microscopy

Nondispersive IR Systems

Analytical Applications of IR Spectroscopy

NIR Spectroscopy

Raman Spectroscopy

Chemical Imaging Using NIR, IR, and Raman Spectroscopy

Suggested Experiments

Problems

Bibliography

Spectral Databases

Visible and Ultraviolet Molecular Spectroscopy

Introduction

Instrumentation

UV Absorption Spectra of Molecules

UV Spectra and the Structure of Organic Molecules

Analytical Applications

Accuracy and Precision in UV/Vis Absorption Spectrometry

Nephelometry and Turbidimetry

Molecular Emission Spectrometry

Instrumentation for Luminescence Measurements

Analytical Applications of Luminescence

Suggested Experiments

Problems

Bibliography

Atomic Absorption Spectrometry

Absorption of Radiant Energy by Atoms

Instrumentation

Atomization Process

Interferences in AAS

Analytical Applications of AAS

Suggested Experiments

Problems

Appendices

Bibliography

Atomic Emission Spectroscopy

Flame Atomic Emission Spectroscopy

Atomic OES

Plasma Emission Spectroscopy

GD Emission Spectrometry

AFS

Commercial Atomic Emission Systems

Laser-Induced Breakdown Spectroscopy

Atomic Emission Literature and Resources

Comparison of Atomic Spectroscopic and ICP-MS Techniques

Suggested experiments

Problems

Appendices

Bibliography

X-Ray Spectroscopy (Contributing authors: Alexander Seyfarth and Eileen Skelly Frame)

Origin of X-Ray Spectra

X-Ray Fluorescence

X-Ray Absorption

X-Ray Diffraction

X-Ray Emission

Commercial X-Ray Instrument Manufacturers

Suggested Experiments

Problems

Appendices

Bibliography

Mass Spectrometry I: Principles and Instrumentation

Principles of MS

Instrumentation

Ion Mobility Spectrometry

Problems

Bibliography

Mass Spectrometry II: Spectral Interpretation and Applications

Interpretation of Mass Spectra: Structural Determination of Simple Molecules

Mass Spectral Interpretation: Some Examples

Applications of Molecular MS

Atomic MS

Problems

Appendix

Bibliography

Principles of Chromatography

Introduction to Chromatography

What is the Chromatographic Process?

Chromatography in More than One Dimension

Visualization of the Chromatographic Process at the Molecular Level: Analogy to "People on a Moving Belt Slideway"

Digression on the Central Role of Silicon–Oxygen Compounds in Chromatography

Basic Equations Describing Chromatographic Separations

How Do Column Variables Affect Efficiency (Plate Height)?

Practical Optimization of Chromatographic Separations

Extra-Column Band Broadening Effects

Qualitative Chromatography: Analyte Identification

Quantitative Measurements in Chromatography

Examples of Chromatographic Calculations

Problems

Bibliography

Gas Chromatography

Historical Development of GC: The First Chromatographic Instrumentation

Advances in GC Leading to Present-Day Instrumentation

GC Instrument Component Design (Injectors)

GC Instrument Component Design (The Column)

GC Instrument Operation (Column Dimensions and Elution Values)

GC Instrument Operation (Column Temperature and Elution Values)

GC Instrument Component Design (Detectors)

Hyphenated GC Techniques (GC-MS, GC-IR, GC-GC, or D-GC)

Retention Indices (A Generalization of Relative Rt Information)

Scope of GC Analyses

Problems

Appendix 12.1

Bibliography

Chromatography with Liquid Mobile Phases

High-Performance Liquid Chromatography

Chromatography of Ions Dissolved in Liquids

Affinity Chromatography

Size-Exclusion Chromatography

Supercritical Fluid Chromatography

Electrophoresis

Planar Chromatography and Planar Electrophoresis

Problems and Exercises

Appendix 13.A

Bibliography

Surface Analysis

Introduction

Electron Spectroscopy Techniques

Ion Scattering Spectroscopy

Secondary Ion Mass Spectrometry

Electron Microprobe (Electron Probe Microanalysis)

Problems

Bibliography

Electroanalytical Chemistry

Fundamentals of Electrochemistry

Electrochemical Cells

Electroanalytical Methods

Liquid Chromatography Detectors

Spectroelectrochemistry

Quartz Crystal Microbalance

Suggested Experiments

Problems

Appendix 15.A

Bibliography

Thermal Analysis

Thermogravimetry

Differential Thermal Analysis

Differential Scanning Calorimetry

Hyphenated Techniques

Thermometric Titrimetry

Direct Injection Enthalpimetry

Microcalorimetry

Thermomechanical Analysis and Dynamic Mechanical Analysis

Optical Thermal Analysis

Summary

Suggested Experiments

Problems

Bibliography

Acronyms Index

Index

About the Authors

James W. Robinson earned his B.Sc. (Hons), PhD, and D.Sc. from the University of Birmingham, England. Heis professor emeritus of chemistry, Louisiana State University, Baton Rouge, Louisiana. A fellow of the Royal Society of Chemistry, he is the author of 250 professional papers, book chapters, and several books including Atomic Absorption Spectroscopy and Atomic Spectroscopy, first and second editions. He was editor in chief of Spectroscopy Letters and the Journal of Environmental Science and Health (both Marcel Dekker, Inc.); executive editor of Handbook of Spectroscopy Vol. 1 – 1974, Vol. 2 – 1974, Vol. 3 – 1981; and Practical Handbook of Spectroscopy— 1991 (all CRC Press). He served on the National University Accreditation Committee from 1970-1971. He was a visiting distinguished professor at University of Colorado – 1972 and University of Sydney, Australia – 1975. He served as the Gordon Conference Chairman in Analytical Chemistry – 1974.

Eileen M. Skelly Frame heads a private consulting company, Full Spectrum Analytical Consultants and is Adjunct Professor, Department of Chemistry and Chemical Biology, Rensselaer Polytechnic Institute, Troy, New York. Dr. Skelly Frame has extensive industrial experience in the use of instrumental analysis to characterize a wide variety of substances, from biological samples and cosmetics to high-temperature superconductors, polymers, metals, and alloys. She is a member of the American Chemical Society and ASTM International. Dr. Skelly Frame earned her BS in chemistry from Drexel University, Philadelphia, Pennsylvania, and her PhD in analytical chemistry from Louisiana State University, Baton Rouge.

George M. Frame II is a retired scientific director, Chemical Biomonitoring Section of the Wadsworth Laboratory, New York State Department of Health, Albany and is a private consultant. He has a wide range of experience in analytical chemistry and has worked at GE Corporate R&D Center, Pfizer Central Research, U.S. Coast Guard R&D Center, Maine Medical Center, and in the United States Air Force Biomedical Sciences Corps. He is a member of the American Chemical Society. Dr. Frame earned his AB in chemistry from Harvard College, Cambridge, Massachusetts, and his PhD in analytical chemistry from Rutgers University, New Brunswick, New Jersey.

Subject Categories

BISAC Subject Codes/Headings:
SCI013010
SCIENCE / Chemistry / Analytic
SCI013040
SCIENCE / Chemistry / Organic
SCI013060
SCIENCE / Chemistry / Industrial & Technical