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trends in analytical chemistry, vol. 7, no. 7, 1988

books -

HRGC-FTIR: state of the art

HRGC-FTIR: Capillary Gas Chro- matography-Fourier Transform In- frared Spectroscopy, Theory and Ap- plications, by W. Herres, Dr. Arfred Hiithig Verlag 1987, DM 84.00 (viii + 212pages) ISBN3-778.5-1061-4

This book deals with the different as- pects of high-resolution gas chroma- tography-Fourier transform in- frared spectroscopy (HRGC-FTIR) and presents applications of it in sev- eral fields. According to the author, the book is concerned only with background information, and details on FTIR and HRGC are strictly lim- ited to those which directly affect the coupling of the two techniques. The information given is considered suffi- cient to enable the user to tune his system.

The book is composed of fifteen chapters of unequal length: we can group them into four main parts.

The first deals with FTIR and re- lates the different stages of raw data treatment needed to generate the IR spectrum. Two important areas of GC detection are discussed at length: spectral resolution and its relations with the signal-to-noise ratio, and problems arising from the choice of reference spectrum to calculate ab- sorbance. Other aspects of FTIR spectroscopy which often come up for general discussion (apodization, phase correction, its advantages) are merely mentioned. The second part, dedicated to HRGC, is very short. After describing the basic param- eters, the author shows how to opti- mize the choice of carrier gas, inter- nal diameter and film thickness in connection with FTIR detection.

exhaustive survey of the literature are proposed to enhance the perfor- mance of HRGC-FTIR. Then prob- lems of sample preparation and in- troduction are discussed, although there is nothing startingly new here for anyone acquainted with classical chromatography. Chapters 5 and 6 (HRGC sensitivity and column selec- tion for HRGC-FAIR) give infor- mation about the internal diameter of the column, and are not intended to solve problems of separation. Chapter 10, called ‘IR chromato- grams’, is what this book is really all about. Up-to-date software is de- scribed and used to follow a chroma- tographic elution from acquired spectroscopic data. The various pa- rameters are discussed, once again based on a very well documented bibliography. Finally, IR vapor phase spectral search is presented and its ability to identify compounds is reviewed. Experimental details are given in the fourth part of the book, which is devoted to applica- tions of HRGC-FTIR. Various fields of analysis such as petroche- mistry, pesticides, essential oils and polymers are covered. Examples are judiciously chosen to prove that

Process analytical chemistry

Handbook of Separation Process Technology, edited by R. W. Rous- seau, Wiley-Interscience, 1987, f 64.10 (xiv + 1010 pages) + SBN O-471 -89558-x

The chapters dealing with the dif- Anyone with any exposure to the ferent aspects of combining HRGC process industries will known that and FAIR constitute the third part. virtually every process includes to The state-of-the-art in the design of some extent or other some process of the light pipe is first presented in separation, such as chromatography, chapter 3. Solutions chosen from an distillation, crystallisation, and poly-

HRGC-FTIR is complementary to other techniques such as GC-MS or else superior to them, especially in the identification of optical isomers. An appendix containing 73 spectra (acquired by the author) completes the part dedicated to essential oils.

Finally, looking to the future de- velopments of HRGC-FTIR some special methods are presented. They are: the matrix isolation technique, multidimensional GC-FTIR and the double hyphenated technique (GC-FTIR-MS). FI near infrared spectroscopy is presented as a detec- tor for atomic emission (ICP or MIP).

In conclusion, we may say that this book presents an interesting look at the state-of-the-art of the hyphen- ated technique, HRGC-FTIR. In spite of the breadth of the subject, the author has managed to write a book which is concise but densely packed with information. Unfortu- nately this very quality may make it rather difficult for beginners.

JEAN PIERRE HUVENNE and

MARC DEVEAUX

Dr. Jean Pierre Huvenne and Dr. Marc Deveaux are at the Laboratoire de Toxi- cologie, Institut de MCdecine Legale et de MCdecine Sociale, Place Thko Varlet, 59000 Lille, France

mer membrane techniques. Knowl- edge of the functioning of separation processes is thus vitally important in developing and designing control systems.

It is being realised more and more in the 1980s that process analytical chemistry, dealing as it does with an- alytical instrumentation, has to be taken more seriously. It is therefore unfortunate that in only one chapter is there any real mention of control systems - that deals with distillation -

htrends in analyticalchemistry, vol. 7, no. 7,1988 271

and then only in passing. Not all the separation techniques are covered in equal depth. Discussion of filtration, coalescing, gravity separation, and cyclones are briefly dealt with in a general discussion of phase separa- tion in Part 1. Other chapters in Part 1 cover phase equilibria, mass trans- fer, and general processing consider- ations. Part 2 includes chapters on distillation, absorbtion and stripping, extraction, organic chemicals pro- cessing - the most common processes to be found in the oil, petrochemical and chemical industries - followed by chapters on leaching processes. There are also chapters on crystallisa- tion, adsorbtion, ion exchange and large scale chromatography.

ing design and development of sam- ple handling systems for process analysers, which is generally con- fined to individual articles that ap- pear in various journals. Therefore this handbook will be a useful refer- ence for process and chemical engi-

neers, as well as process analytical chemists.

PETERREEVES

Dr. Peter Reeves’ address is Lambertij- nenlaan 127, 4614 EX Bergen op Zoom, The Netherlands.

The Miissbauer effect

Miissbauer Spectroscopy, edited by D. P. E. Dickson and J. F. Berry, Cambridge University Press, 1987, f 30.00/$54.50 (274 pages) ISNB O- 521-26101-5

The last chapters of the book con- centrate on modern membrane tech- niques for ultrafiltration, reverse os- mosis, use of membranes for liquid and gaseous separation, dialysis and electrodialysis, with finally a sum- mary chapter on process selection. These techniques are shown to be of importance in areas such as decon- tamination of radioactive wastes, metals recovery, pollution removal, and also the production of high puri- ty materials.

This book is British: the majority of the authors are British and the appli- cations described are mainly in the field of chemistry where for the past 25 years British scientists have played a major role.

shift is introduced. Topics such as bonding, electron density and config- urations, oxidation states and the na- ture of ligands are discussed, i.e., how the resonance atom senses its environment. Also, the quadrupole interaction gives valuable structural information. Partial quadrupole splittings and correlations between isomer shift and quadrupole interac- tion could have been introduced here. Is is shown that the molecular structure is revealed in the hyperfine parameters, particularly when phase transitions, cooperative spin crossov- ers, mixed valences, molecular dy- namics etc. occur.

There is also a chapter on separa- tion based on reversible chemical complexation - the classical separa- tion methods used in analytical chemistry. It discusses how the often neglected complexation process can be used in chemical processes, by in- cluding the reverse reaction to recov- er the original reactant. Two addi- tional chapters discuss bubble and foam separations for ore flotation and waste treatment.

In chapter 4 (Mossbauer spectro- scopy of magnetic solids) the mag- netic hyperfine parameters are intro- duced. The four common magnetic structures - ferromagnetic, antifer- romagnetic, ferrimagnetic and canted antiferromagnetic - are pre- sented. In addition to their identifi- cation from magnetic split spectra, of special interest are low dimensional magnetism and also magnetism of small particles and highly disordered systems.

To the practicing process analyti- cal chemist, the recurring theme through this book is how there is a continuing interaction between sepa- ration processes and analytical chemistry. For example, membrane technology is of importance not only in advancing separation technology but also in the use of membranes in analysis and measurement technolo- gy. This Handbook of Separation Process Technology brings together in one volume an easily readable dis- cussion of all the various processes. Another useful feature is that it allows access to the literature cover-

The introductory chapter, ‘Prin- ciples of Mossbauer spectroscopy’ is too short to claim that ‘this book will be of value to postgraduate students and research workers with no pre- vious knowledge of the technique’. At least a few simple equations and a schematic drawing of the important Mossbauer resonance line, i.e. the intensity (Debye-Waller factor), the line width (Heisenberg uncertainty principle) and the line shape (Breit- Wigner formula or Lorentzian) should have been included. In fact, the reader who starts at the begin- ning has to wait until p. 74 to see the first Mossbauer resonance line. The reader would be better advised to start with the final chapter in which the basic principles of Mossbauer spectroscopy are indeed well de- scribed.

Chapter 2 (Mossbauer spectro- scopy and the chemical bond) and chapter 3 (Mossbauer spectroscopy as a structural probe) present a wealth of information on the applica- tion of Mossbauer spectroscopy to chemistry. Extensive use is made of the isomer shift; in fact one soon re- alizes why in the early days of Mossbauer spectroscopy the isomer shift was called ‘chemical shift’. Be- cause the isomer shift appears to be an additive function, a partial isomer

Chapter 5 (Time-dependent ef- fects and relaxation in Mossbauer spectroscopy) and chapter 6 (The dy- namics of nuclei studied by Mijssbauer spectroscopy) are some- what similar with a certain amount of overlap, e.g. in the treatment of dif- fusion. However, chapter 5 is more on the theoretical side, while chapter 6 presents interesting data on the dy- namics of atoms. The recoil-free fraction and its anisotropy are con- sidered to lead to the so-called Gold- anskii-Karygin effect. Dynamics of phase transitions, spin reorienta- tions, diffusion in liquids and solids, biological and macromolecular sys- tems are discussed.