Chemical Analysis: Modern Instrumentation Methods and Techniques

Citation

Rouessac, F., & Rouessac, A. (2022). Chemical Analysis: Modern Instrumentation Methods and Techniques (3rd ed.; J. Towey, Trans.). Wiley.

Chapter Summary

The third edition runs to about 620 pages in 22 chapters, translated from the French by John Towey, with a companion website. The publisher describes it as covering the principles and practical aspects of more than 20 separation and spectroscopic methods while "avoiding technical complexity and theoretical depth". The sample first chapter shows the pattern: a short introduction, a list of learning objectives, numbered sections with figures and worked calculations, then end-of-chapter problems followed by their solutions. The book is organised by technique rather than by analytical problem: separations first, then spectroscopic methods, then elemental, electrochemical and supporting topics.

Chapter 1: General Aspects of Chromatography

The foundation for the separation chapters. It describes the chromatogram and the difference between ideal Gaussian and real peaks, then develops plate theory, the Nernst partition coefficient, column efficiency, retention parameters, selectivity and resolution. The effect of mobile-phase speed is treated through the van Deemter, Golay and Knox equations, followed by optimisation and a classification of chromatographic techniques. The chapter ends with quantitative analysis by external standard, internal standard and internal normalisation, including the calculation of relative response factors, and a note on chromatography software.

Chapters 2–7: Gas Chromatography; High-Performance Liquid Chromatography; Ion Chromatography; Thin-Layer Chromatography; Supercritical Fluid Chromatography; Size-Exclusion Chromatography

Six chapters apply Chapter 1 to the main chromatographic techniques, each from its principle to its instrumentation. The index shows chiral stationary phases treated in both the gas and liquid chromatography chapters and detectors such as the nitrogen–phosphorus detector in Chapter 2. The publisher names supercritical fluid chromatography among the topics revised for this edition.

Chapter 8: High-Performance Capillary Electrophoresis

Electrophoretic separation in capillaries, also revised for this edition; the index places capillary electrochromatography and zone electrophoresis here.

Chapters 9–11: Ultraviolet and Visible Absorption Spectroscopy; Infrared and Raman Spectroscopy; Fluorescence and Chemiluminescence Spectroscopy

Molecular spectroscopy. Chapter 9 includes quantitative analysis from absorbance measurements using linear regression. Chapter 10 pairs mid- and near-infrared methods, attenuated total reflection and chemical imaging with Raman scattering. Chapter 11 covers fluorescence and its applications together with chemiluminescence.

Chapters 12–14: X-Ray Fluorescence Spectroscopy; Atomic Absorption Spectroscopy; Atomic Emission Spectroscopy

Elemental analysis by spectroscopy: X-ray fluorescence (including energy-dispersive instruments), atomic absorption with its matrix effects, and atomic emission, where the index places inductively coupled plasma sources and laser-induced breakdown spectroscopy.

Chapter 15: Nuclear Magnetic Resonance Spectroscopy

NMR as an analytical method, reaching coupled spin systems, the COSY sequence and a section touching on magnetic resonance imaging.

Chapter 16: Mass Spectrometry

At about 50 pages, the longest chapter in the book: ionisation methods including electrospray and MALDI, analysers including quadrupole, ion-trap and time-of-flight instruments, tandem mass spectrometry and ICP-MS.

Chapters 17–18: Isotopic Analyses and Labelling Methods; Specific Analysers

Chapter 17 deals with isotope-based methods such as isotope dilution and accelerator mass spectrometry. Chapter 18 gathers dedicated instruments that do not fit the earlier chapters: elemental organic analysis, total nitrogen (including Kjeldahl nitrogen) and total organic carbon analysers, the Karl Fischer method for water and ion mobility spectrometry.

Chapters 19–20: Potentiometric and Ionometric Methods; Voltammetric Methods

Electrochemical analysis. Chapter 19 covers potentiometry and ion-selective measurement, including the glass electrode. Chapter 20 covers polarography in its direct-current and pulsed forms, stripping voltammetry and amperometric sensors, including enzyme-based biosensors.

Chapters 21–22: Sample Preparation; Basic Statistical Parameters

Two short closing chapters that the publisher calls concise overviews: strategies for preparing samples (the index mentions headspace methods and microwave reactors) and the statistics needed to report results, including Student's coefficient and linear regression.

Key Concepts

Chapter 1: General Aspects of Chromatography

• Plate theory and column efficiency: a model that treats the column as a series of equilibrium stages, giving the number of theoretical plates and the plate height.
• Resolution and selectivity: measures of how completely two neighbouring peaks are separated and how differently the column retains them.
• Van Deemter, Golay and Knox equations: relations between mobile-phase speed and band broadening, used to choose operating conditions.
• External standard, internal standard and internal normalisation: three ways of turning peak areas into concentrations.

Chapters 2–8: Separation techniques

• Chiral stationary phases: column packings that separate enantiomers.
• Capillary electrophoresis: separation of charged species by their mobility in an electric field inside a narrow capillary.

Chapters 9–16: Spectroscopic and spectrometric methods

• Attenuated total reflection: an infrared sampling technique that measures a thin surface layer of the sample.
• Inductively coupled plasma: a high-temperature source used for atomic emission and as an ion source for mass spectrometry.
• Tandem mass spectrometry: two stages of mass analysis, the second applied to fragments of ions selected in the first.

Chapters 17–22: Elemental, electrochemical and supporting methods

• Isotope dilution: quantification by adding a known amount of an isotopically labelled form of the analyte.
• Karl Fischer titration: a dedicated method for determining water.
• Stripping voltammetry: preconcentration of an analyte on an electrode followed by its electrochemical release and measurement.
• Student's coefficient: the factor used to give a confidence interval for a mean from a small number of measurements.

Critical Analysis

Strengths

• Breadth in one volume. Twenty-two chapters cover separations, molecular and atomic spectroscopy, NMR, mass spectrometry, isotopic methods, dedicated analysers and electrochemistry. The publisher lists users in the chemical and agri-food industries, medical laboratories and environmental science, and the coverage of practical instruments such as Karl Fischer titrators and total organic carbon analysers reflects that audience.
• Low entry barrier. The publisher states that no background in the subject is assumed and that each chapter explains the basic concepts of a method and its instruments with diagrams and photographs of commercial instruments, rather than with theory.
• Structured for study. The sample chapter opens with explicit objectives and closes with problems whose solutions follow immediately, so a reader can check work without a separate manual. A review of the second edition quoted by the publisher (International Journal of Environmental and Analytical Chemistry) called it an essential introduction to a wide range of techniques.
• Updated instrumentation. The third edition revises supercritical fluid chromatography, capillary electrophoresis, miniaturised sensors, automatic analysers and the role of digitisation and computing.

Limitations

• Little theory by design. The deliberate avoidance of theoretical depth means the physics of spectroscopy, the equilibrium chemistry behind titrations and the electrode kinetics behind voltammetry are treated briefly. Students who need to understand why instruments behave as they do, or to design methods, will need a more theoretical text.
• Classical wet chemistry is largely absent. Apart from Karl Fischer and Kjeldahl methods within Chapter 18, the contents contain no chapters on gravimetry, titrimetry or solution equilibria, which most first analytical chemistry courses include.
• Statistics and quality at the end. Basic statistics and sample preparation are compressed into the last two short chapters rather than introduced at the start, so readers should consult them early.

Where It Fits in the Course

This is an instrument-by-instrument survey, and it pairs naturally with the course's more quantitative books. David Harvey's Analytical Chemistry 2.1, an open text for a first analytical course, and Daniel Harris's Exploring Chemical Analysis teach the equilibrium chemistry, titrations and statistics that Rouessac omits; either can serve as the main text for a first course, with Rouessac as the reference for what each instrument does. Harris and Lucy's Quantitative Chemical Analysis covers the same ground as Exploring Chemical Analysis in more depth.

For an instrumental analysis course, Skoog, Holler and Crouch's Principles of Instrumental Analysis is the standard upper-level text, explaining the physical principles and instrument design that Rouessac deliberately keeps light; reading Rouessac's chapter first gives the overview that makes the corresponding chapter in Skoog easier. Bard, Faulkner and White's Electrochemical Methods is a graduate treatment of what Rouessac covers in Chapters 19–20 and belongs much later.

How to Use This Book

The publisher addresses undergraduates in introductory instrumental analysis courses, students in chemistry, pharmacy, biochemistry and environmental science who need to know which techniques and instruments are available, and industry technicians. General chemistry is enough to start, since no prior knowledge of analytical methods is assumed.

A practical plan:

• Start with Chapters 1, 21 and 22. The general aspects of chromatography underpin six later chapters, and the short chapters on sample preparation and statistics are needed for any quantitative work even though they come last.
• Separations: Chapters 2 and 3 (gas and liquid chromatography) are the core; Chapters 4–8 can be read selectively according to the techniques in a laboratory course.
• Spectroscopy: Chapters 9, 10, 13, 14 and 16 cover the methods most often met in teaching laboratories; Chapters 11, 12 and 15 add fluorescence, X-ray fluorescence and NMR.
• Electrochemistry and dedicated methods: Chapters 18–20 as a course or laboratory requires them; Chapter 17 is optional for most first courses.

Work the end-of-chapter problems before reading the solutions that follow them, and study the objectives list at the start of each chapter as a checklist. Before using an instrument in the laboratory, reading the relevant chapter is a quick way to understand its components and limitations. For the theory behind the methods, follow up with Skoog for instruments and with Harvey or Harris for equilibria and calculations.