Undergraduate Instrumental Analysis, Seventh Edition
Analytical chemistry today is almost entirely instrumental analytical chemistry and it is performed by many scientists and engineers who are not chemists. Analytical instrumentation is crucial to research in molecular biology, medicine, geology, food science, materials science, and many other fields. While it is true that it is no longer necessary to have almost artistic skills to obtain accurate and precise analytical results using instrumentation, the instruments should not be considered “black boxes” by those using them. The well-known phrase “garbage in, garbage out” holds true for analytical instrumentation as well as computers. We hope this book serves to provide users of analytical instrumentation with an understanding of their instruments.
In keeping with the earlier editions of this text, the book is designed for teaching undergraduates and those with no analytical chemistry background how modern analytical instrumentation works and what the uses and limitations of analytical instrumentation are. Mathematics is kept to a minimum. No background in calculus, physics, or physical chemistry is required. The major fields of modern instrumentation are covered, including applications of each type of instrumental technique. 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. To achieve this, the previous approach of having each chapter be self-contained has been abandoned; repetition has been reduced to a minimum so that more topics could be covered in more detail. The topics of chromatography and mass spectrometry have been greatly expanded, when compared with the sixth edition, to better reflect the predominance of chromatography and mass spectrometry instrumentation in modern laboratories. The equally important topic of NMR, expanded in the last edition to focus on FTNMR, 13C, and 2D NMR spectral interpretation, now includes time domain NMR (relaxometry) and an overview of low-field, benchtop, and miniature instrumentation. The topic of electron spin resonance spectroscopy (ESR, EPR) has been added due to the recent availability of small, lowcost ESR instrumentation and its impact on materials characterization and bioanalysis. Chapter 3 has therefore been renamed to reflect the inclusion of ESR/EPR. Forensic science applications have been added in appropriate chapters.
A unique feature of this text is the combination of instrumental analysis with organic spectral interpretation (IR, NMR, and MS). The NMR, IR, and MS spectra, all new in the sixth edition, courtesy of Bio-Rad Laboratories, Informatics Division (IR, NMR), Aldrich Chemical Company (NMR), Agilent Technologies, Inc., and one of the authors (MS), were obtained on modern instruments to reflect what students will encounter in modern laboratories. Additional NMR spectra have been provided by Bruker Corporation and picoSpin LLC for the seventh edition. The use of spreadsheets for performing calculations has been introduced with examples. Reflecting the ubiquitous nature of the Internet, we have included a large number of instrument manufacturers’ websites, which contain extensive resources for interested students.
Sampling, sample handling, and storage and sample preparation methods are extensively covered, and modern methods such as accelerated solvent extraction, solid-phase microextraction (SPME), QuEChERS, and microwave techniques are included. Instrumentation, the analysis of liquids and solids, and applications of NMR are discussed in detail. A section on hyphenated NMR techniques is included, along with an expanded section on MRI and advanced imaging. The IR instrumentation section is focused on FTIR instrumentation. Absorption, emission, and reflectance spectroscopy are discussed, as is FTIR microscopy. ATR has been expanded. Near-IR instrumentation and applications are presented, and the topic of chemometrics is introduced. Coverage of Raman spectroscopy includes resonance Raman, surface-enhanced Raman, and Raman microscopy.
Chemical imaging is described, including confocal Raman imaging. UV and visible spectroscopy includes innovations such as flow through sample holders and fiber-optic probes, as well as instruments for analysis of submicroliter volumes and nondestructive analysis for nucleic acid and protein determinations. UV absorption spectral interpretation for organic molecules is covered in depth. Applications described include nucleic acid and protein measurements, spectrophotometric titrations, and new applications in forensic chemistry. Nephelometry, turbidimetry, fluorescence, and phosphorescence are described in detail, including instrumentation and applications. The measurement of color using the CIE system is described with examples.
All major modern atomic absorption and emission techniques and instrumentation are covered, including new MP-AES and triple quadrupole ICP-MS instruments. The relatively new technique of laser-induced breakdown spectroscopy (LIBS) has been added to Chapter 7 and is now currently being used on Mars in the Curiosity rover, which landed on the Red Planet in August 2012. Appendices with FAAS and GFAAS conditions have been added, and the appendix with limits of detection for all the atomic spectroscopic techniques has been updated from the sixth edition. The chapter on X-ray has been significantly revised by Dr. Alexander Seyfarth, the new coauthor of the chapter, to reflect the state of the art in XRF, XRD, and related techniques. Many new graphics have been added.
Mass spectrometry has been expanded to two chapters and covers both organic and inorganic MS instrumentation and applications. GC-MS and LC-MS are described along with MSn instruments for organic and inorganic MS, including new triple quad ICP-MS instrumentation. Modern ionization methods such as electrospray and MALDI are also described. New surface scanning and ionization sources, such as desorption electrospray ionization (DESI) and laser ablation electrospray ionization (LAESI), and the DART atmospheric pressure ionization source are introduced. More advanced high-resolution systems, such as the Orbitrap, and long-path time of flight (JEOL SpiralTOF and LECO Citius-LC and Pegasus GC-HRT) are described. The use of MS peak profile correction software to improve mass and spectral accuracy from lower resolution MS instrumentation is described. Uses of HRMS receive increased attention. A new section on ion mobility spectrometry is added, with a discussion of four systems ranging from handheld vapor monitors to stages enabling characterization of different conformational isomers in top-end proteomics analyzers. Organic mass spectral interpretation is covered with many examples and new spectra. Organic and inorganic applications focus on speciation using GC-MS, LC-MS, and hyphenated ICP-MS, with an emphasis on proteomics, biomolecules, and species of environmental interest. Examples of atomic MS applications using new simultaneous and “triple quad” ICP-MS systems and glow discharge surface sampling and hydrogen in metals profiling are added.
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