Calorimetry: Fundamentals and Practice

trenhin analyticalchemistry, vol. 5, no. 2,19&S

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books Principles of quality assurance: quality assured! Quality Assurance Principles for Analytical Laboratories, by F. M. Garfield, Association of Official Analytical Chemists, US$45.501 1984. US$48.50 (outside U.S.A.) (VI + 211 pages) ISBN O-935584-24-9

This book is probably the first monograph on quality assurance. This has become a very important topic indeed and therefore Dr. Garfield’s book is a timely one. It is a sequel to another publication of the AOAC, namely ‘Optimizing Chemical Laboratory Performance through the Application of Quality Assurance Principles’ [1980, F.M. Garfield et al. (Editors)], which consisted of a series of articles on the subject. The present book contains chapters on administrative considerations, personnel management, management of equipment and supplies, records maintenance, sample analysis, proficiency testing, audit procedures, design and safety of facilities and laboratory accreditation programs. It also contains many appendices with practical examples of forms, procedures, check lists, etc. The introduction states that this publication is not an original treatise on quality assurance, but that it draws on published principles, practices and guidelines. The material of the book is very well organized: Dr. Garfield apparently applies quality assurance principles to writing books. It is a must for laboratories involved in regulatory or enforcement activities and for control laboratories of pharmaceuticals, foods and other commodities. Although the emphasis is on procedures to be applied by rather large laboratories, research analytical chemists can also read the book with profit, since it contains advice for all practising analysts concerned with the quality of their data. Finally, this is one of the very few books with information about management aspects of analytical chemistry and, for

those teachers, who believe that they should prepare analytical chemists for practical work in industry, it contains enough information for several lectures about the subject. Because the emphasis is very much on analysis in those fields in which AOAC is active, analysts in clinical laboratories will probably feel that there is not enough information pertinent to their specific quality assurance problems. It is also probable that non-American specialists will have a similar reaction. When primary reference standards are discussed the only sources stated are NBS, USP and ASTM, while the figure on proficiency testing programs

mentions nine institutions, all of them American. On the other hand, quality assurance for laboratories seems to have gained more acceptance in the U.S.A. than in most other countries. Keeping those short comings in mind, this book can certainly be recommended to a large fraction of the analytical community. D. L. MASSART

D. L. Massart is at the Farmaceutisch Instituut, Vrije Universiteit Brussel, 103 Laarbeeklaan, B-1090, Brussels, Belgium.

Does not meet the set objectives

Calorimetry: Fundamentals and Practice, by W. Hemminger and G. Hohne, Verlag Chemie, 1984. DM 135.OOIUS$ 60.00 (VI + 310 pages) ZSBN3-527-25948-1

I am not sure at whom this book is directed - at the practitioner, at the builder of calorimeters or at those who contemplate using calorimeters. The authors say that it is intended for all these categories and yet it appears to me not to fulfil these objectives. I am not certain whether such an objective could, or indeed, should be satisfied with a book. The contents of the book, then, fall into two parts: calorimetry and calorimeters. In both parts I have some quibbles both with the content and with the extent to which the stated objectives have been met. Part 1, for example, outlines some basic thermodynamic relationships and in doing so identifies E as the thermodynamic potential whereas

IS0 recommendation is the symbol U, for thermodynamic energy or internal energy; the Helmholtz function is identified as F and IS0 recommendation is A. This latter use of a non-standard symbol is doubly confusing in that in the past F was frequently used as the symbol for the Gibbs function, G. At a more frivolous level I feel a book of the ‘weight’ desired by the authors is not well served by the coy use of a bird in various postures to represent the ‘sample’ in figures. At the practical level baseline problems are serious and inhibiting yet here the discussion of baseline ‘correction’ is dismissed as superfluous since the causes must be known before an exact theory for the construction of a baseline can be attempted. Yet it is precisely here over this, and similar points, that many experimentalists will be frustrated. I do, however, applaud the treatment of deconvolution in that the book properly draws attention to estab-

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lishment of the ‘true heat exchange function from the measured curve’. However disappointment arises again at the end of the section on deconvolution because we are told ‘. . . an estimation of error . . . is not (a) simple . . . here it will only be outlined briefly.’ The balance is wrong in some instances, the theoretical approach is elevated over the practical and then in other places the reverse is true. In the second part, which deals with calorimeters, the authors list and describe commercial instruments and make reference to some ‘home-made’ instruments. However, ‘potted’ biographies cannot I think do justice to the breadth of application of each of these instruments. For example in an attempt to achieve wider use of calorimeters LKB have introduced an instrument which they designate as ‘Bioactivity Monitor’ which is abbreviated as BAM. The entry under the BAM (not indexed nor indeed can the descriptions of commercial instruments be found other than by riffling through the book - that for the BAM is on page 224) describes it as ‘an instrument for direct and continuous monitoring of the very small heat effects associated with biological events in living organisms’. Here the authors are guilty of an uncritical approach to advertising material, to the name, to the attempt to ‘sell’ calorimetry to non-physical scientists, to . . . They have ignored the fact that the BAM is a true cal-

trends in analytical chemistry,

orimeter designed for great flexibility of operation allowing many different vessels (ampoule, titration, mixing, batch etc.) to be employed. It is not restricted to living organisms and a practitioner might distil this out of the description if he (1) could read very much between the lines or (2) knew the instrument. A novice would get little guidance from this book itself. There is too, in the second part, an imbalance in favour of scanning type instruments. In summary the book has interest in parts but I feel does not meet the set objectives. Also books have some permanence associated with them and as the authors themselves note in the preface there is a ‘risk that some of the calorimeters described here will be obsolete in a few years’. The page and a half devoted to Possible Future Developments is sketchy and unimaginative. Who will buy the book I do not know - where it will find use is equally unclear, it does not adequately serve either the ‘home-made’ builder nor indeed the novice seeking detailed advice on which instrument to buy. A. E. BEEZER

A. E. Beezer is at the Department of Chemistry, The Bourne Laboratory, Royal Holloway & Bedford Colleges, Egham Hill, Egham, Suney TW20 OEX, U.K.

Useful guide for the practising organic mass spectrometrist Practical Organic Mass Spectrometry, by J. R. Chapman, Wiley, 1985 f 19.50 (vii + 197 pages) ISBN O-471-90696-4

The aim of this book is to provide a practical description of the techniques used in organic mass spectrometry (MS) and, more specifically, of the newer alternative ionization and operating techniques. With this in mind, the author has written a book primarily for the practising

mass spectrometrist who is familiar with the basic principles. Therefore, theoretical aspects are only covered where they are necessary for practical applications. It consists of seven chapters; instrumentation, sample introduction, chemical ionization (CI), negative ion chemical ionization (NICI), the ionization of labile molecules, metastable ions, and quantitative analysis. One of the three attractive features of this book is that it includes theory only where it is relevant to the

vol. 5, no. 2 1986

application being discussed. For instance, electron impact ionization is covered in but a few pages, whereas in the sections of both positive and negative chemical ionization, choice of reagent gases and subsequent reactions are discussed in detail, thus providing a sound basis for not only understanding the phenomena, but also a good introduction on how to tackle a specific problem the reader might be interested in. The second is, as might be expected from a practical guide, the amount of literature cited. At the end of each chapter, usually two lists of references are given, one covering the general literature, and the other with more detailed references, divided in classes of compounds, analyzed with a specific technique. In this way, literature pertaining to practical problems and solutions is readily traced, thus giving a good impression of the state-of-the-art in most fields. References on these practical applications cover the period up to the end of 1982 (metastable ions: end of 1983); for the more general chapters on instrumentation, sample introduction, and quantitative analysis this period has not been stated, but is estimated to be up to the end of 1982. Therefore, in a rapidly expanding field like liquid chromatography-MS, the most recent developments could not be incorporated, the latest reference being a review article published in the course of 1983. This is probably inevitable though one would have hoped for a bit more than the twenty references given. Another section yielding relatively little specific information is that on quantitative analysis, although the subjects treated (specificity, sensitivity, sources of error, selected and metastable monitoring) provide a clear insight into the possibilities and pitfalls of this particular technique. The third attactive aspect is the way in which the techniques of sample preparation, tests on sensitivity, and instrument setting up procedures for various ionization modes are presented. Like measurement of multiplier gain, standard tests on gas chromatography-MS performance, CI and NICI operation, choice of cali-