Undergraduate Instrumental Analysis  book cover
7th Edition

Undergraduate Instrumental Analysis

ISBN 9781420061352
Published July 21, 2014 by CRC Press
1264 Pages 895 B/W Illustrations

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Book 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

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

Magnetic Resonance Spectroscopy
Nuclear Magnetic Resonance Spectroscopy Introduction
The FTNMR Experiment
Chemical Shifts
Spin–Spin Coupling
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
Spectral Databases

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
Spectral Databases

Visible and Ultraviolet Molecular Spectroscopy
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

Atomic Absorption Spectrometry
Absorption of Radiant Energy by Atoms
Atomization Process
Interferences in AAS
Analytical Applications of AAS
Suggested Experiments

Atomic Emission Spectroscopy
Flame Atomic Emission Spectroscopy
Atomic OES
Plasma Emission Spectroscopy
GD Emission Spectrometry
Commercial Atomic Emission Systems
Laser-Induced Breakdown Spectroscopy
Atomic Emission Literature and Resources
Comparison of Atomic Spectroscopic and ICP-MS Techniques
Suggested experiments

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

Mass Spectrometry I: Principles and Instrumentation
Principles of MS
Ion Mobility Spectrometry

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

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

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
Appendix 12.1

Chromatography with Liquid Mobile Phases
High-Performance Liquid Chromatography
Chromatography of Ions Dissolved in Liquids
Affinity Chromatography
Size-Exclusion Chromatography
Supercritical Fluid Chromatography
Planar Chromatography and Planar Electrophoresis
Problems and Exercises
Appendix 13.A

Surface Analysis
Electron Spectroscopy Techniques
Ion Scattering Spectroscopy
Secondary Ion Mass Spectrometry
Electron Microprobe (Electron Probe Microanalysis)

Electroanalytical Chemistry
Fundamentals of Electrochemistry
Electrochemical Cells
Electroanalytical Methods
Liquid Chromatography Detectors
Quartz Crystal Microbalance
Suggested Experiments
Appendix 15.A

Thermal Analysis
Differential Thermal Analysis
Differential Scanning Calorimetry
Hyphenated Techniques
Thermometric Titrimetry
Direct Injection Enthalpimetry
Thermomechanical Analysis and Dynamic Mechanical Analysis
Optical Thermal Analysis
Suggested Experiments

Acronyms Index

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James W. Robinson earned his BS (Hons), PhD, and DSc from the University of Birmingham, England.  Robinson began his career with the British Civil Service as a senior scientific officer before immigrating to the United States in 1955, completing a one-year term as a research associate at LSU. From 1956 to 1964, he worked in research labs at both Esso Corp. and Ethyl Corp., and in 1964 joined the LSU Department of Chemistry as an associate professor. He became professor in 1966 and retired as professor emeritus in 1993.  Robinson’s pioneering research in analytical chemistry and atomic spectroscopy led to the first comprehensive book, Atomic Absorption Spectroscopy, the text Undergraduate Instrumental Analysis (now in its 7th edition).  He published more than 200 peer-reviewed manuscripts and mentored 45 graduate students, many of whom have enjoyed notable careers. He was executive editor of Spectroscopy Letters, the Journal of Environmental Science and Health, the Handbook of Spectroscopy and the Practical Handbook of Spectroscopy.  He was recognized as a Fellow of the Royal Chemical Society, selected for the American Institute of Chemistry’s Honor Scroll, a Guggenheim Fellowship, and received the Gold Medal Award of the New York Section of the Society of Applied Spectroscopy.  He was a visiting distinguished professor at University of Colorado in 1972 and University of Sydney, Australia in 1975. He served as the Gordon Conference Chairman in Analytical Chemistry in 1974.  Professor Emeritus James W. Robinson passed away in November, 2018, at 95 years of age.

Eileen M. Skelly Frame was adjunct professor, Department of Chemistry and Chemical Biology, Rensselaer Polytechnic Institute (RPI), Troy, NY, and head of Full Spectrum Analytical Consultants. Dr.  Skelly Frame was the first woman commissioned from the Drexel University Army ROTC program. She graduated from Drexel summa cum laude in chemistry.  She served as Medical Service Corps officer in the U.S. Army from 1975 to 1986, rising to the rank of Captain. For the first five years of her military career, Eileen was stationed at the 10th Medical Laboratory at the U.S. Army Hospital in Landstuhl Germany. Thereafter, she was selected to attend a three-year Ph.D program in Chemistry at Louisiana State University. She received her doctorate in 1982 and became the first female Chemistry Professor at the U.S. Military Academy at West Point.  Following her military service, she joined the General Electric Corporation (now GE Global Research) and supervised the atomic spectroscopy laboratory.  In addition to her duties at RPI, she was Clinical and Adjunct Professor of Chemistry at Union College in Schenectady, NY.  She was well known for her expertise in 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 was an active member of the American Chemical Society for 45 years, and a member of several ASTM committees.  Dr. Skelly Frame passed away in January of 2020.  

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.