Instrumental Analysis will be organized into 5 sections:
Organization and General CoverageOxford
The textbook starts with an introductory chapter titled “The Analyst’s Toolbox” which establishes a perspective of considering instrumental techniques as tools used by the analyst to answer questions. The competent analyst must master the use of multiple tools in order to solve complex chemical problems. This theme is reinforced regularly throughout the textbook. The remainder of this section is devoted to a review of foundational knowledge and includes the underlying quantum mechanics of spectroscopy, optics, basic electronics, and signal processing. Although many undergraduate chemistry programs will have covered these topics in prerequisite course, a review of these topics is helpful prior to delving into the individual instrument types.
This nine-chapter section covers the core topics of instrumental analysis beginning with a discussion of electronic absorption spectroscopy (molecular and atomic) followed by electronic emission spectroscopy (molecular and atomic). This is followed by an expanded discussion of x-ray spectroscopic techniques and we have been deliberate in discussing the role of X-ray spectroscopy as an elemental analysis technique compared against AAS and AES. We follow our discussion of X-ray spectroscopy with two separate chapters on vibrational spectroscopy; infrared and Raman. We introduce the Fourier transform in our discussion of IR spectroscopy with several activities that allow students to perform an FT using excel and with the advent of miniaturized lasers the utility of Raman spectroscopy has greatly improved in the past few decades and as such we have devoted an entire chapter to the discussion of Raman spectroscopy. Next we discuss mass spectrometry using a modular approach that outlines ion generation, mass selection and detection as separate events and we present the most common MS applications as a “plug and play” models, thus allowing the students to “synthesize” a great many different MS instrument types. We conclude this section with a discussion of nuclear magnetic spectroscopy. Although NMR has most likely been discussed in an organic chemistry course, our textbook does not focus on data interpretation but rather on instrument design with an emphasis on how the signal is generated, detected and processed. An advanced NMR chapter on pulse sequences and 2D signal processing is also included in Section E.
Before a chemical analysis can take place, the analyte must be isolated from the matrix. This section discusses the three most common instrumental separation techniques; liquid chromatography, gas chromatography and electrophoresis. Each chapter begins with the fundamental principles governing the technique, followed by the most common applications and ends with the “state of the art” for each technique.
We begin this section with a chapter covering potentiometry and probes followed by a separate chapter on analytical voltammetry. Because the analytical application of potentiometry has benefited greatly from the evolution of miniaturized electronics, we have emphasized the design and application of probes in our discussion of potentiometry. Today, probes find regular use in medicine, environmental monitoring, quality control systems as well as law enforcement, forensics and security systems. Analytical voltammetry provides a quick, inexpensive and reliable means to gain both quantitative and qualitative information about an electroactive system. Voltammetry can provide important evidence regarding the mechanism by which systems undergo chemical and electrochemical reactions. Importantly, voltammetric experiments can be scaled down to the intracellular level. In the analytical voltammetry chapter we discuss the basics of voltammetry and include some common waveforms used in research laboratories, and we demonstrate the utility of and limits imposed by micro- and nano-scale electrodes.
We recognize that most curricula will not have sufficient time to teach all of the chapters in this textbook however, we end Instrumental Analysis with three chapters that represent less common, yet important, topics. At the very least, the more aggressive student can read these chapters on their own time or these chapters may provide useful background for a lab project. The first is a chapter on material and surface analysis in which we discuss important microscopy, thermoanalytical and mechanical stress techniques. The next chapter in this section specifically details the application of pulse sequences as they apply to advanced NMR techniques. Students are taught the significance of T¬1 & T2 relaxation, and the basics of programming 2D experiments such as COSY, TOSCY, NOESY, etc. Next, we end this section with a review of Statistical Data Analysis. We placed this chapter last in recognition of the fact that many schools teach this material in a separate course while others choose to include it in their instrumental analysis course.