Books Practical Open Tubular GC
Open Tubular Column Gas Chromatog raphy: Theory and Practice. Milton Lee, Frank Yang, Keith Bartle. χ + 445 pp. John Wiley & Sons, 605 Third Ave., New York, N.Y. 10016. 1984. $48
Reviewed by Richard Laub, Depart ment of Chemistry, San Diego State University, San Diego, Calif. 92182 The preface to this work states that it "is intended to serve as a reference source for those interested in the theo retical and technical background of open tubular column gas chromatog raphy, as well as for analysts con cerned with details of the practice of the technique." The foreword by L. S. Ettre goes on to say that, "The present book by three very gifted young chromatographers fulfills this requirement. Besides presenting a de tailed theoretical background, it deals with the questions related to both col umn preparation and evaluation and the system in which these columns are employed." The second foreword by J. C. Giddings then remarks that, "With this book, those who wish to practice the art have at their disposal a thor ough guide." The tour offered by this text is then begun with an introducto ry chapter (13 pp.), followed by a brief (35 pp.) treatment of the theory of chromatography. Column technology (including a discussion of glass and amorphous silica surfaces) is taken up next in chapter 3 (49 pp.), and instru mentation (chapter 4; 73 pp.) and in strumental considerations (chapter 5; 54 pp.) complete the technical section of the book. Examples of the applica tion of open tubular columns, chapters 6 (82 pp.) and 7 (126 pp.), and a sub ject index comprise the second half of the work. Although the label chromatographer (or electrochemist or spectroscopist) usually signifies one who "does" chromatography (or electrochemistry or spectroscopy), it is not infrequently used in the pejorative sense to imply one who understands little else. Un fortunately, such criticism can be ap plied to this book. A large number of topics crucial to chromatography in general, and peculiar to open tubular column systems in particular, are ig nored completely or are addressed only briefly. Broadly speaking, these
OPEN TUBULAR COLUMN GAS CHROMATOGRAPHY: Theory and Practice
I I Iι
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Milton L. Lee, Frank J. Yang, a n d Keith D. Bartle
can be divided into those that pertain, on the one hand, to the stationary phase and, on the other hand, those that concern the mobile phase. For ex ample, although the column phase ratio is related correctly to the solute capacity factor and partition coeffi cient, no mention is made of activity coefficients (vapor pressures are men tioned only in passing) that govern KR and, hence, that lie at the heart of gas chromatographic separations. More over, the use of thin films of stationary phase portends that there may well be a kind of mesomorphic (not mesogenic) aggregation of the molecules, into which solutes intrude and thereby dis rupt the local ordering. Further, and as evidenced in virtually every chromatogram produced in this book, there is inevitably a considerable con tribution from gas-"liquid" interfacial adsorption that leads to asymmetric peak shapes, irrespective of whether the stationary phase is deposited from solution or synthesized and/or poly merized in situ. Since the phenomenon is rarely anything but Langmuir in na ture, the asymmetry is most often manifested as tailing peaks. In addi tion, recent work has implied that sol ute diffusion in bulk polysiloxanes is no different from that observed when these polymers are heavily crosslinked, i.e., anchored firmly to each
other as well as immobilized in place on the column wall. This in turn indi cates that there is little solute solu tion; rather, solutes sorb onto the sur face of the stationary phase and, per haps in the process, "swell" it to some extent as well. With regard to the mobile phase, flow- and outlet-pressure regulation are discussed in detail in section 4.2, for example, but no mention is made of the fundamental work of R.P.W. Scott and others as to why one might want to increase the column back pressure. In conjunction with this, virial effects have been ignored entirely. These can be significant (as was point ed out more than 20 years ago) and, as such, can be taken advantage of also in enhancing separations. These and related fundamental questions have all arisen since Golay presented the inaugural paper on open tubular col umns in 1957; many of them still await exploration and clarification, and it was disappointing not to find them mentioned in this work. There are a few outright errors in the text. For example, Equation 5.5 for N r e q should contain the factor 36 and not 24; the concept of an effective plate was first introduced by Purnell, not Desty. Figure 2.2, which is a pres entation of the usual van Deemter curve, gives one the specious impres sion that gas as well as liquid phase mass transfer nonequilibrium terms can be determined simultaneously from plots of plate height against the average linear velocity of a single car rier. Many have pointed out that since the van Deemter equation (as well as the Golay version thereof) contains terms both in ΰ and in uo, rather more sophisticated techniques must be used to derive Cs and CM (e.g., use of two carriers). There are a few typographical mis takes in the book (e.g., Reference 285, p. 173), but no-more than usual in a work of this length. Several of the symbols will be unfamiliar to workers in the field, for example, the use of k rather than k'; ÎN for ÎR (although t R is used later in Equations 6.5 and 6.6, p. 282); Ν for N eff ; and so on. Fortu nately, there is a symbols table at the end of chapter 2 to help overcome this difficulty.
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Books Overall, the strength of this book lies in the wealth of practical informa tion presented, as well as the large number of examples of and references to the use of GC capillary columns. Those interested in these (largely ap plied) matters will find the book to be valuable; certainly beyond doubt is that compared to other recent of ferings that purport to deal with the same subject matter, this work excels. Unfortunately, however, those who are interested in a modern treatment of the fundamental aspects of open tubu lar column gas chromatography will be disappointed. Methods of Seawater Analysis. 2nd re vised ed. K. Grasshoff, M. Ehrhardt, K. Kremling, Eds. xxviii + 419 pp. Verlag Chemie International Inc., 303 N.W. 12th Ave., Deerfield Beach, Fla. 33441. 1983. $70
Reviewed by Robert Petty, Marine Science Institute, University of Cali fornia, Santa Barbara, Calif. 93106 The purpose of this book is to update and expand the material cov ered in the first edition, which was published in 1976 and "was quickly accepted by marine scientists as a reli able source of information on analyti cal procedures specifically developed for the use with seawater" (from the preface). Its main emphasis is on pro viding detailed methods for the deter mination of specific substances and properties of seawater. A general dis cussion and specific information on seawater sampling and sample storage and a chapter on automated chemical analysis are also included. Although not intended as compre hensive reviews, each chapter is a rea sonably thorough presentation of a particular topic. The choice of topics, however, has resulted in a wide varia tion in chapter length and complexity. For instance, chapter 6 is a four-page description of the titrimetric determi nation of thiosulfate, whereas chapter 9 is 64 pages long and covers the de termination of nutrients by presenting one section on phosphorus, one on sili ca, and five sections on various forms of nitrogen. Most of the substances covered are specific compounds, ions, or elements. The extensive chapter on organic constituents, however, ad dresses mainly classes of substances, including petroleum residues, organochlorines, phenolics, amino acids, and carbohydrates. Determination of indi vidual components within these groups is generally made possible by chromatographic techniques. Typically included for each analyti cal species or property are an intro-
Books auction, the principle of the determi nation, the specific apparatus and re agents needed, and the detailed proce dure. Other important information, such as preparation of standards, cal culations required to obtain the final value, and expected precision, range, and accuracy, is also usually given. Additional information uniquely use ful to the topic being covered, such as a detailed discussion of the definition of salinity, is frequently included. Oc casionally too much information is presented, as in the chapter on alka linity and total carbonate. Here, four methods are extensively described, only two of which are commonly used by practicing oceanographers. The methods included in this book have generally been thoroughly tested and proven reliable, even under shipboard conditions. Overall editorial control of the book appears to have been relatively weak. For instance, the organization is in consistent: A particular species might stand out as a chapter heading or be buried as a sub-subheading, which makes locating an analysis of interest in the table of contents rather diffi cult. There are a relatively large num ber of proofreading-type errors as
well. Nevertheless, I believe the origi nal aims of the late Klaus Grasshoff, editor and primary author of the first edition, which were to provide a gen eral insight into marine analytical chemistry as well as precise recipes for specific analyses, are substantially achieved by this updated edition. The book should definitely be included in the personal library of anyone who deals with seawater analysis on more than an occasional basis. For those owners of the first edition, the addi tional information presented in the update may not, however, be enough to justify the $70 price.
Books Received Handbook of U.S. Colorants for Foods, Drugs, and Cosmetics. 2nd ed. Daniel Marmion. xii + 466 pp. John Wiley & Sons, 605 Third Ave., New York, N.Y. 10016. 1984. $50 Gas Chromatography/Mass Spectrom etry Applications in Microbiology. G. Odham, L. Larsson, Per-Anders Mardh, Eds. xvi + 444 pp. Plenum Press, 233 Spring St., New York, N.Y. 10013. 1984. $59.50
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Advances in Clinical Chemistry. Vol. 23. L. Latner, Morton Schwartz, Eds. ix + 350 pp. Academic Press, 111 Fifth Ave., New York, N.Y. 10003. 1983. $38.50 Analytical Calorimetry. Vol. 5. Julian Johnson, Philip Gill, Eds. ix + 402 pp. Plenum Press, 233 Spring St., New York, N.Y. 10013. 1984. $59.50 New Approaches in Liquid Chromatog raphy. H. Kalasz, Ed. χ + 291 pp. Else vier Science Publishers, 52 Vanderbilt Ave., New York, N.Y. 10017. 1984. $67.25 Quality Assurance Principles for Ana lytical Laboratories. Frederick Garfield. 224 pp. Association of Official Analyti cal Chemists, 1111 North 19th St., Suite 210, Arlington, Va. 22209. 1984. $45 Wilson & Wilson's Comprehensive An alytical Chemistry. Vol. 12, Pt. D. Jar oslav Sestak. xix + 440 pp. Elsevier Science Publishers, 52 Vanderbilt Ave., New York, N.Y. 10017. 1984. $115.50 Advances in Materials Characteriza tion. David Rossington, Robert Condrate, Robert Snyder, Eds. xi + 680 pp. Plenum Press, 233 Spring St., New York, N.Y. 1983. $89.50
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