Principles of Instrumental Analysis

Citation

Skoog, D. A., Holler, F. J., & Crouch, S. R. (2018). Principles of Instrumental Analysis (7th ed.). Cengage Learning.

Chapter Summary

The seventh edition has thirty-four chapters in six sections, followed by four appendixes (evaluation of analytical data; activity coefficients; standard and formal electrode potentials; compounds for preparing standard solutions), answers to selected problems and an index. Each of the six sections closes with an "Instrumental Analysis in Action" case study, and each chapter has an open-ended Challenge Problem. The first chapter introduces the classification of analytical methods, the types of instrumental methods and instruments for analysis.

Chapter 1 and Section I: Introduction; Measurement Basics (Chapters 2–5)

Chapter 1 is the introduction. Section I covers electrical components and circuits (Chapter 2), operational amplifiers in chemical instrumentation (Chapter 3), digital electronics and computers (Chapter 4), and signals and noise (Chapter 5). The case study is "The Electronic Analytical Laboratory".

Section II: Atomic Spectroscopy (Chapters 6–12)

Chapter 6 introduces spectrometric methods in general, and Chapter 7 covers the components of optical instruments (the publisher notes updated material on laser sources, array transducers and Fourier-transform instruments). Chapter 8 introduces optical atomic spectrometry. Chapters 9–12 treat atomic absorption and atomic fluorescence, atomic emission (including plasma spectrometers), atomic mass spectrometry (with time-of-flight and distance-of-flight instruments) and atomic X-ray spectrometry (with bench-top and hand-held energy-dispersive XRF). The case study is "Monitoring Mercury".

Section III: Molecular Spectroscopy (Chapters 13–21)

Chapters 13–14 introduce and apply ultraviolet–visible molecular absorption; Chapter 15 covers molecular luminescence (fiber-optic fluorescence sensors and fluorescence imaging among its new material); Chapters 16–17 introduce and apply infrared spectrometry; Chapter 18 is Raman spectroscopy; Chapter 19 is nuclear magnetic resonance; Chapter 20 is molecular mass spectrometry (atmospheric-pressure ionization, MALDI and electrospray); Chapter 21 is surface characterization by spectroscopy and microscopy (now including ellipsometry). The case study is the analysis of the Vinland Map.

Section IV: Electroanalytical Chemistry (Chapters 22–25)

An introduction to electroanalytical chemistry (Chapter 22), potentiometry (Chapter 23, with biosensors and biomedical applications), coulometry (Chapter 24) and voltammetry (Chapter 25, emphasising solid, thin-film and microelectrodes). The case study is "The Microphysiometer".

Section V: Separation Methods (Chapters 26–30)

An introduction to chromatographic separations (Chapter 26), gas chromatography (Chapter 27), high-performance liquid chromatography (Chapter 28), supercritical-fluid chromatography and extraction (Chapter 29), and capillary electrophoresis, electrochromatography and field-flow fractionation (Chapter 30). The case study is the bisphenol A controversy.

Section VI: Miscellaneous Methods (Chapters 31–34)

Thermal methods (Chapter 31), radiochemical methods (Chapter 32), automated methods of analysis (Chapter 33) and particle size determination (Chapter 34). The case study is the John F. Kennedy assassination, in which neutron activation analysis figured.

Key Concepts

Chapters 1–5

• Signals and noise: the limits that measurement electronics and data handling set on an instrumental method.
• Instrument components: electrical circuits, operational amplifiers and digital electronics.

Chapters 6–21

• Optical instrument components: sources, wavelength selectors, detectors and transducers.
• Atomic and molecular spectrometry: absorption, emission, fluorescence, infrared, Raman and NMR methods.
• Mass spectrometry: atomic and molecular ionization and detection methods.

Chapters 22–34

• Electroanalytical methods: potentiometry, coulometry and voltammetry.
• Chromatographic and electrophoretic separations: gas, liquid and supercritical-fluid chromatography and capillary methods.
• Thermal, radiochemical and automated methods: techniques outside the main families.

Critical Analysis

Strengths

• Systematic organisation by technique family. Six sections group the methods by family (measurement basics, atomic spectroscopy, molecular spectroscopy, electroanalytical chemistry, separations and miscellaneous methods), which suits a course taught by technique.
• Case studies. The six "Instrumental Analysis in Action" case studies draw on forensic, environmental and biomedical examples and show how methods from a section combine on one problem.
• Computational and online support. The publisher states that spreadsheet applications run through the book, that a companion text on Excel in analytical chemistry and a website with more than a hundred interactive tutorials accompany it, and that every chapter has a Challenge Problem.
• Revised content. The publisher lists updates to optical components, plasma and mass spectrometry, luminescence, electrochemistry, chromatography and thermal methods.

Limitations

• Very large. At thirty-four chapters and roughly 1,000 pages, the book exceeds what one course can use; instructors normally select techniques.
• Not a first course. The book opens with electronics and signal processing and then treats instruments and techniques in detail, so it presumes the quantitative analysis of an earlier course.
• Breadth over depth for individual techniques. Each family of methods gets one to a few chapters; readers needing depth in one area, such as electrochemistry, will need a specialist text.

Where It Fits in the Course

Within the analytical chemistry course this is the upper-level survey of instrumental methods. It comes after a first course in quantitative analysis: Harvey's Analytical Chemistry 2.1 is an open text for a first course covering equilibrium, measurement, statistics, spectroscopy, chromatography and electrochemistry; Harris's Exploring Chemical Analysis is a shorter, less mathematical introduction; and Harris and Lucy's Quantitative Chemical Analysis is the fuller textbook. Rouessac and Rouessac's Chemical Analysis: Modern Instrumentation Methods and Techniques is an introductory instrumental text, translated from French, which can serve as a gentler alternative or a first pass before Skoog.

Bard, Faulkner and White's Electrochemical Methods is the graduate text that goes much deeper into the topics of Section IV.

How to Use This Book

The book is for upper-level undergraduates (and early graduate students) who have completed a quantitative analysis course; calculus and general physics are the practical background, and physical chemistry helps.

A practical plan:

• Start with the measurement basics: Chapters 5 (signals and noise) and 6–7 (spectrometric methods and optical components) matter for almost everything that follows; the electronics chapters (2–4) can be read at the depth a course requires.
• Choose by technique family. Sections II–V are largely independent: read atomic spectroscopy (6–12), molecular spectroscopy (13–21), electroanalytical chemistry (22–25) and separations (26–30) in the order a course demands.
• Use the case studies at the end of each section to see how techniques combine.
• Do the problems, using the spreadsheet exercises and the online tutorials where available, and attempt the Challenge Problems for open-ended practice.