ANALYTICAL CHE M ISTRY Manual of Practical Micro and Gen eral Procedures in Clinical Chem istry. Samuel Mettes and W. S. Faulkner, xvi + 3-54 pages, diaries (' Thomas, 301-27 East Lawrence Ave.. Springfield. III. 1962. $11.50. Reviewed by John G. Reinhold, Hospital of the University of Pennsyl vania, Philadelphia, Pa. The development of microchemical techniques for examination of body fluids continues to attract considerable attention. In part, this is a result of the rapidly increasing application of chemical studies in pediatrics. How ever, microanalysis often proves to be advantageous for the study of adults. For chemical studies of small animals such methods are indispensable. The authors of this manual describe procedures used in the microchemistry laboratories of two large medical cen ters, the Children's Hospital of Colum bus and the Cleveland Clinic. Both authors have a background of exten sive experience in the field of clinical microchemistry. A section on prin ciples of microchemistry including blood collection techniques serves as an introduction. This is followed by a section on electrolytes in serum, urine, and whole blood in which direc tions for alternative methods are de scribed in detail. Unfortunately one of the flame photometers discussed is no longer on the market. A chapter is devoted to measurement of blood pH. The operation of the two instruments described is clarified by use of excellent photographs and diagrams. The reviewer would not agree with the authors' choice of chloroformmethanol over aqueous protein-con taining solutions for standardization of bilirubin, a procedure which is difficult to bring off with consistent success. A nomogram for calculation of results by the speetrophotometric method is helpful, as are the illustrative calcula tions for this method. Occasionally, useful methods not generally available in manuals of clinical chemistry are included. Pro cedures for haptoglobin and serum hemoglobin, xylose absorption serve as examples. There are descriptions of diffusion analysis and for paper chromatography of amino acids, re ducing sugars, phenolic acids, and for quantitation of phenylalanine. In general, the procedures are scaleddown versions of standard methods of clinical chemistry modified by the authors in some instances. Principles are stated briefly and the description
NEW of the method is followed by com ments concerning certain sources of error, variants for use in special cir cumstances, standard values, and the like. A bibliography of clinical micro chemistry and information regarding sources of control specimens and of microchemical equipment are helpful. The combination of detailed direc tions for what are in general accept able methods together with the gener ous use of illustrations makes this in deed a most practical guide for lab oratories concerned with clinical micro chemistry. Absorption Spectroscopy,
by R. P.
Bauman. xiv + 611 pages. John Wiley &: Sons, Inc., 440 Park Ave., South, New York 16, Ν. Υ. 1962. $12. Reviewed by Walter H. Foster, Jr., American Cyanamid Co., Bound Brook, JV. J. In writing this introductory book on absorption spectroscopy, the author has based his presentation upon ex perience gained while teaching both theoretical and applied courses on the subject. Of the nine main chapters, four are devoted to theory, two to in strument design and performance, one to sample preparation, and two to qualitative and quantitative analysis. The instrumental chapters are con cerned almost exclusively with the op tical design and performance of spec trometers. The important area of electronics in instrument design has been considerably de-emphasized. A very good chapter on sample prepara tion follows, with a particularly good discussion on the handling of solids. The next three chapters comprise a fairly comprehensive presentation on the theory of spectroscopy. They are well written and include many of the recent developments in this area. Two chapters on qualitative and quantitative analysis are included and these should be especially interesting to the analytical spectrosoopist. The chapter on qualitative analysis is quite brief and general. The chapter on quantitative analysis includes a dis cussion of expanded-scale methods and analysis of multi-component mixtures. The final chapter, on molecular spectroscopy, comprising about Vs of the book, goes into group theory, matrices and quantum mechanical de scription of electronic, vibrational and rotational states in molecules. Problems follow each chapter and an appendix includes an introduction
BOOKS to matrices which proves helpful in digesting the material in the chapter on molecular spectroscopy. In summary, it is quite apparent that the author has tried to include something for everyone. In his pref ace he mentions molecular spectroseopists, analytical speetroscopists, and industrial analysts. In attempting to reach such a wide audience, the book is necessarily brief in some sections. In the reviewer's opinion, this text will be most useful to first-year spectros copy students and to applied spee troscopists who wish to improve their theoretical background in molecular spectroscopy.
Rapid Microchemical Identification Methods in Pharmacy and Toxi cology. Felix Amelink. vi + 121 pages. John Wiley & Sons. Inc.. 440 Park Ave., South, New York 16. Ν. Υ. 1062. $0.00. Reviewed by Walter C. McCrone, McCrone Associates, Inc., Chicago, III. This volume covers microchemical tests based on precipitation reactions with standard reagents for sulfona mides, sulfones, barbiturates, and hydantoins. It is a successor to the same author's earlier work "Schema zur Identification von Alkaloiden," (1934). Short sections on microchem ical methods and utensils, the polariz ing microscope, general reactions, rea gents, extraction methods, and bibli ography precede the summaries of data for the 38 sulfonamides, 6 sulfones, 30 barbiturates, and 3 hydantoins. All compositions are gh'en by trade name although a separate key to the chemi cal names and a summary of pseu donyms are given. The book is con cise and thorough and more than 300 drawings show very well the charac teristic appearance of each composition with each reagent. There are two general microchemi cal methods that may be used to iden tify these compounds: precipitation reactions and Kofler's hot stage pro cedures. Both use the microscope and neither has a clear-cut advantage over the other. Those who are trained in the Kofler procedures will continue to use the hot stage and those trained in precipitation reactions will adopt the new volume with enthusiasm. A be ginner trained in neither may prefer the Kofler methods because they are of more general application or the VOL. 35, NO. 1 , JANUARY 1963
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NEW BOOKS Amelink methods because they are simpler and require less expensive equipment. M e t h o d s o f Forensic Science. V o l . I.
Frank Lundquist, editor, xii + 659 pages. John Wiley & Sons, Inc., 44Ο Park Ave., South, New York 16, Ν. Y. 1962. $19.95. Reviewed by Irving Sunshine, Cuyahoga County Coroner s Office, Cleveland, Ohio.
Forensic scientists in the United States have had a long unsatisfied curiosity about the current practices of their foreign confreres. Because "Methods of Forensic Sciences" fills this gap, they and forensic scientists everywhere will herald its appearance. The eight European experts who each contributed a chapter to this vol ume have comprehensively reviewed and evaluated past achievements and practices on their respective topics. Then they describe, in detail, their
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ANALYTICAL CHEMISTRY
own current laboratory procedure. Much of the cited material is not now easily available to many labora tories. Thus, this volume will also serve as an excellent reference book. Chemically, next to ethyl alcohol, determinations of carbon monoxide, the barbituric acids, and the organic bases are most frequently required from the forensic laboratory. These three agents are excellently presented by Drs. E. G. C. Clarke and George Schmidt and Andreas C. Maehly, re spectively. Their detailed descriptions of laboratory techniques will be ex plored by many and evaluated against present local practices. When only microgram quantities or less of or ganic bases are available, Dr. Clarke's unique technique must be considered. His analytical data for 450 organic bases are an excellent contribution. Dr. Schmidt's detailed presentation on the barbituric acids makes one wonder how much could there be for his forth coming monograph on this subject. His presentation and discussion of the many approaches to barbiturate anal ysis are thorough and provocative. Many laboratories will hasten to ap ply the differential spectrophotometry techniques for carbon monoxide Maehly presents. Remarkably sim ple and straightforward, it should be eye-opening to many. Angelo Fiori's chapter on "Detec tion and Isolation of Blood Stains" as well as F. Schleyer's on "Investiga tion of Biological Stains with Regard to Species of Origin" were not de signed "as a manual for beginners." Trained forensic investigators will be pleased to find the detailed discussions and specific physical, chemical, and immunological techniques described. This is also true of the chapter by Galatius-Jensen on "Serum Haptoglo bin Patterns in Cases of Disputed Paternity." Criminalists will find Nicholl's "Identification of Stains on Non-bio logical Origin" and Ceccaldi's on "Ex amination of Firearms and Ammuni tion" comprehensive descriptions of ho\v their laboratories handle these particular problems. Editor Lundquist is to be com mended for starting this series and rounding up such an imposing array of outstanding contributors. May succeeding volumes continue at the same high level as this first one. Spectroscopy. M. J. Wells, editor, viii + SOS pages. The Institute of Petroleum, 61 New Cavendish St., London, W. 1, England. 1962. $10. The Institute of Petroleum Hydro carbon Research Group Conference on
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Spectroscopy, held at the University of London from March 28 to 31 was at tended by over 300 delegates including 65 from overseas countries. Emi nent authors were invited to review the progress in many fields in order to give a balanced appreciation of spectroscopy as it stands today. This book is a collection of these lectures. The titles and authors arc : Trends in the Chemi cal Applications of Spectroscopy bv H. W. Thompson, (F.R.S., St. John's College, Oxford) ; Atomic Absorption Spectroscopy by A. Walsh (C.S.I.R.O., Melbourne) ; Some Aspects of Atomic Absorption by R. L. Warren (Mid dlesex Hospital) ; X-Bay Fluores cence Analysis by Η. Ν. Wilson and B. J. Otter (LCI., Billingham) ; Nu clear Magnetic Besonance by R. E. Richards, (F.R.S., Lincoln College, Ox ford) ; A Study of Nuclear Magnetic Resonance Performance Parameters by R. B. Williams (Humble Oil and Re fining Co., Texas) ; The Method and Technique of Electron Resonance and Its Application to Metal Complexes by D. J. E. Ingram (University College of North Staffs) ; Electron Spin Reso nance of Free Radicals by D. H. Whiff en (National Physical Labora tory) ; Free Radical Spectroscopy bv Β. Ν. Dixon (Sheffield University)'; The Spectrophotometry of Free Radi cals in Flames by T. M. Sugden (Cam bridge University) ; Optical Absorption Spectra of Oriented Free Radicals bv G. W. Chantry (National Physical Laboratory) ; Far Infra-Red Spectros copy by G. R. Wilkinson, S. A. Inglis, and C. Smart (King's College, London) ; Rotation in Solution by W. J. Jones and N. Sheppard (Cambridge University) : The Origins of Group Frequency Shifts. Pt. I I . The In fluence of Inductive Effects and of NonBonded Interactions on Infra-Bed Group Frequencies, by L. J. Bellamy (E.R.D.E., Waltham Abbey) ; Fac tors Affecting the Characteristics of Infra-Red and Raman Vibrational Bands by H. W. Thompson, (F.R.S., St. John's College, Oxford) ; Develop ments in Applied Spectroscopy by V. Z. Williams (Perkins-Elmer Corp.) ; Some Uses of Electronic Computing Ma chines in Spectroscopy by A. D. Booth (Birkbeck College) ; Solvent Effects on Infra-Bed Spectra of Inorganic Com plexes by D. M. Adams (I.C.I., The Frythe) ; Vacuum Ultra-Violet Spectra and Photoionization of Molecules and Radicals by W. C. Price, F.R.S., R. Bralsford, and D. M. Boessler (King's College, London) ; The Electronic Spec tra of Small Polyatomic Molecules with Especial Reference to the Absorption Spectrum of Nitrogen Dioxide by R. K. Ritchie, A. D. Walsh, P. A. Warsop
ACCESSORIES INCREASE THE CAPABILITIES OF PERKIN-ELMER'S MODELS 421, 221 AND 21 INFRARED SPECTROPHOTOMETERS Sample preparation and handling are probably the most critical operations in infrared spectroscopy. That's why second best won't do when you choose sampling accessories. You'll realize the best per formance from your Perkin-EImer Mode! 421,221, o r 2 1 Spectrophotometer with Perkin-Elmer's quality cells and attachments, no matter what investiga tions you're undertaking. FOR GAS S A M P L I N G : Perkin-EImer cells include a wide variety of window and body materials, in path lengths from 2 centimeters to 40 meters, Pressure and Ijeated cells are also available. FOR LIQUID S A M P L I N G : Cells are provided in demountable or sealed versions, in various dis crete path lengths, for regular or micro sampling. Special cells with micrometer adjustments for vary ing path length are afso available, as well as heated cells for special studies. FOR
SOLID S A M P L I N G :
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technique is facilitated by special-purpose acces sories: dies, holders, vibrators—for preparing and analyzing samples in standard 13mm and micro KBr discs. Perkin-EImer also has special accessories that equip the Models 4 2 1 , 221 and 21 to handle other un usual sampling problems. A n d - m o s t large-instru ment accessories are adaptable to P-E's low-cost line of IR spectrophotometers. For complete de tails, write to Instrument Division, Perkin-EImer Cor poration, 7 5 1 Main Avenue, Norwalk, Connecticut.
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PERKIN-ELMER Circle No. 185 on Readers' Service Card Circle No. 182 on Readers' Service Card
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NEW BOOKS (Queen's College, University of St. Andrews) ; The High Resolution Spec tra of Some Benzenoid Molecules by T. M. Dunn (University College, London) : Excitation-Modulation Spec troscopy; A Technique for Obtaining Vibrational Spectra of Excited Elec tronic States by R. M. Ilexter (Mellon Institute, Pittsburgh). A d v a n c e s in Electrochemistry and Electrochemical E n g i n e e r i n g . Vol. 2. Electrochemical Engineering.
C. W. Tobias, ix + 300 pages. John Wiley Λ Sons, Inc., 440 Park Ave. South, New York 16, Ν. Υ. 1962. $12. This new, continuing series bridges the gap between electrochemistry as part of physical chemistry and electro chemical engineering. Volume 1, "Electrochemistry," edited by P. Delahay was published in 1961, while Volume 3 will be published in March 1963.
The chapter headings and their authors for Volume 2 are: The Scope of Electrochemical Engineering, C. Wagner; Conduction in Heterogeneous Systems, R. E. Meredith and C. W. Tobias; Applications of Mass Trans fer Theory: The Formation of Pow dered Metal Deposits, N. Ibl ; Appli cations of Mass Transfer Theory: Electrodeposition on Small-Scale Pro files, 0. Kardos and D. G. Foulke; and Design and Scale-Up Considerations for Electrochemical Fuel Cells, M. Eisenberg. I n v e s t i g a t i o n s of I n f r a - R e d
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This work, long out of print, has been reprinted in a limited edition. It is divided into two parts. Part I is titled "Infra-Red Absorption Spectra" while Part II is "Infra-Red Emission Spectra." The book is interesting as a study of the beginnings of infrared spectroscopy, both in the development of apparatus and methods and the application of these techniques to the study of gases, liquids, and solids. S y m p o s i u m o n Extension of S e n sitivity for Determining Various Constituents in M e t a l s - S T P 3 0 5 .
Optics (Prisms, Lenses,
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William W. Coblentz. vi + 331 pages, Part I, and ÎS3 pages, Part II. Paperbound. The Coblentz Society, Inc., clo The Perkin-Elmer Corp., Main Ave., Norwalk, Conn. 1962. $3.50.
68 + vi pages. Paper Cover. American Society for Testing and Materials. 1916 Race St., Philadelphia 3, Pa. 1962. S3.00 To AST M members: 82.40. The book covers the following: methods for determining small amounts of elements; limits of detection for these elements; obstacles that must be overcome to obtain increased sensitivity and how to overcome them. The topics covered and the authors are: Some Recently Developed Electroanalytical Techniques for Determination of Traces of Metals by Louis Meites, Polytechnic Institute of Brooklyn; Radioactivation Analysis— Specific for Trace Element Determination by G. W. Leddicotte, Oak Ridge National Laboratory; Ultratrace Emission Spectroscopy by George H. Morrison, Cornell University, and R. L. Rupp, General Telephone and Electronics Laboratories; Use of the Electron Probe to Measure Low Average but High Local Concentration by L. S. Birks and R. E. Seebold, U. S. Naval Research Laboratory; and Extension of Sensitivity in Analysis of Impurities in Solids by Mass Spectrometry by C. M. Stevens, Argonne National Laboratory.
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BUNGE 25 UM ULTRA-MICRO BALANCE CAPACITY: SENSITIVITY: 2 mg optical scale 0.1 Ag 9 mg automatic weight loader Estimations to ± 0.01 ng 2.5 g built-in tare weights 2.511 g Total O U T S | D E LOADING: By automatic pan extraction through front panel
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NEW BOOKS The Interpretation of NMR Spectra. K. B. Wiberg and B. J. Nist. vii + 593 pages. W. A. Benjamin, Inc., 346-5 Broadway, New York 25, Ν. Υ. 1962. $25. This book presents theoretically cal culated N M R spectra in a format t h a t can be used for comparison with ob served spectra making it possible to estimate coupling constants and chem ical shifts. T h e spectra were calcu lated with t h e aid of the IBM-709 computer, the plots have been pre pared by the computer and printed out b y associated equipment. The chemical shift between A and Β has been maintained at 6 s e e r ' , correspond ing 0.1 p.p.m. at 60 mc. T h e plots were m a d e b y replacing t h e spectra lines with Gaussian curves having a width of 0.3 sec.- 1 at half height, fol lowed b y summing t h e curves where they overlap. T h e data supplied with the spectra a r e : the spin coupling constants; a sorted list of frequencies and intensi ties; and the intensity of t h e highest peak in the plot.
Ionization Constants of Acids a n d Bases. Adrien Albert, E. P. Ser jeant, xii -f- 179 pages. John Wiley Park Ave.. South. New York 16, Ν. Υ. 1962. $3.75. This practical m a n u a l is written for those who, without previous experi ence, wish to determine an ionization constant. In addition, more advanced instruction is provided for those who wish to extend their range of tech niques. T h e first examples require only a few, very simple calculations; more complicated calculations are in troduced as gradually as possible with full explanatory detail. Help in the interpretation of ioniza tion constants is given ; it is shown how they are related to solubility and how they are used for deciphering an unknown. T h e last chapter deals with the determination of the stability con stants of metal complexes.
Physics a n d C h e m i s t r y of Electronic Technology. H. L. Van Velzer. xii + 372 pages. McGraw-Hill Book Co.. Inc., 330 West J,2nd St., New York 36, N. Y. 1962. $10. This book was originally prepared as a text for laboratory technicians to increase their understanding of vac u u m - t u b e fabrication. I t is written for the nonspecialist whose formal technical education is limited or non existent. Among the specific subjects
NEW BOOKS •
covered are: structure of matter; energy and current; the solid state; theory of metals and alloys; machin ing operations; the oxide coated cath ode; gas filled tubes; the electromag netic spectrum; vacuum equipment and techniques; and leak detection and mass spectroscopy. As might be expected with the number of subjects covered and the basic aims of the book, the discussions of any particular sub ject are necessarily rather limited.
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An Introduction to the Chemistry of Complex Compounds. A. A. Grinberg, xxi + 363 pages. AddisonWesley Publishing Co., Inc., Reading. Mass. 1962. $15.
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This book is a translation of the 2nd edition (1951) of A. A. Grinberg's "Vvedenie ν Khimiyu Kompleksnykh Soedinenii." As construed by the author "complex compound" is a term used to define molecular com pounds which, through a coupling of their components, can form positively or negatively charged complex ions capable of existing both in crystalline form and in solution. In some cases the charge on such a complex ion can be zero—this definition also includes oxygen acids of the type H 2 S0 4 and their corresponding salts. This book was translated to provide a background of this subject as the Russian chemist sees it in order to facilitate understanding individual Russian research papers. Also, it is pointed out that there is no English counterpart to this book, and that it can serve as a textbook in this area of chemistry. The editors have added comments at appropriate places where the date of publication has resulted in a void or inbalance in presentation. A sup plementary bibliography has also been provided for readers who want more extensive or more recent information on various topics.
Gas Chromatography, 3rd Interna tional Symposium Held Under the Auspices of the Analysis Instru mentation Division of the Instru ment Society of America, June 13—16, 1 9 6 1 . Nathaniel Brenner, J. E. Calien, M. D. Weiss, editors. xxiv + 719 pages. Academic Press, Inc., Ill Fifth Ave., New York 3, Ν. Υ. 1962. $22.
This book contains thirty-seven pa pers by an international group of ex perts, and appendices which include the edited transcripts of the informal
discussions on these papers as well as the edited transcripts of discussions on Preparative Chromatography and Food and Flavor Analysis. An ex tensive bibliography is included which consists of new entries not duplicated in the bibliographies (totaling 1975 en tries) in the first two volumes.
Proceedings of the International Microscopy Symposium, Chicago, 1960. W. C. McCrone, editor. vii + 22^ pages. McCrone Research Institute, 451 East 31st St., Chicago 16, III. Paperbound. $7.50. The Microscopy Symposium held in Chicago, June 13 to 15, 1960, was the eighth in a series of symposia which started in 1948. This meeting was at tended by nearly 300 microscopists from this country and abroad; more than 70 technical papers were pre sented. These meetings are sponsored by the McCrone Research Institute, a nonprofit corporation devoted to re search and teaching in microscopy and related fields.
The Application of Organic Bases in Analytical Chemistry. E. A.
Ostroumov. xxv + 159 pages. Pergamon Press. The Macmillan Co., 60 Fifth Ave., New York 11, Ν. Υ. 1962. $7.75. This volume, translated from Rus sian by D. A. Paterson, is a collection of systematic studies by the author on the application of a particular class of organic compounds—organic bases—in the analytical chemistry of inorganic substances. The methods described have been tested by many years of practical experience in the Analytical Chemistry Laboratory of the AUUnion Scientific Research Institute for Mineral Raw Materials and are used by the Analytical Chemistry Group in the Marine Deposit Laboratory of the U.S.S.R. Academy of Sciences In stitute of Oceanology, and in a num ber of other Russian laboratories. Chapter headings are: The Precipi tation of Metals Using Pyridine; The Precipitation of Metals by Pyridine in the Presence of Its Salts; The Pre cipitation of Metals with Hydrogen Sulphide in the Presence of Pyridine; The Precipitation of Metals Using α-Picoline; The Precipitation of Met als with Hydrogen Sulphide in the Presence of Hexamethylenetetramine, and Methods for the Separation of Metals Using Pyridine, α-Picoline, and Hexamethylenetetramine.
