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Chromatographic systems: Maintenance and troubleshooting
BOOK
REVIEWS
341
shifts, the other with 13C coupling constants to 13C and other magnetic nuclei. Each segment contains three elements of analyses: experimental techniques used in acquiring the data, a substantial compilation of data and theoretical explanations and correlations of the experimental data. The chemical shift compilation includes chapters on hydrocarbons, substituted hydrocarbons, organometallics and carbonium ions, heterocyclic compounds and on functional groups (i.e., carbonyls and nitriles). As throughout the rest of the book references well into 197 1 seem to be in evidence. Because of the well-resolved spectra obtained for simpler molecules, “C magnetic resonance has proved to be and will continue to be a fertile ground for theoretical model building and the author presents a wide survey of the successes and failures of the theoretical approaches employed to account for chemical shift and coupling-constant correlations. and 11C-‘SF data priThe coupling-constant tabulation includes I:iC-‘H, l”C-‘“C, marily but also lists ‘“C coupling data to other magnetic nuclei such as zr’P, lSN and others. Finally, a brief survey of the applications of ‘“C nuclear magnetic spectroscopy to the solution of a variety of problems is presented. Outstanding among these are ‘“C studies on conformational equilibria and ring inversion barriers in mobile cyclohexane like systems and conformational analysis of carbohydrates; l”C analysis of nucleic acid constituents; of amino acids and polypeptides and the very important use of 13C as tracer in biosynthetic mechanistic studies. Clearly, with the advent of widespread availability of pulsed NMR instruments, the myriad of applications of rsC nuclear magnetic resonance are yet to be explored. The book is to be recommended as an essential addition to any library since it is a convenient starting point for a literature search for anyone comtemplating a ‘K experiment. More than that, anyone having access to an instrument with a ‘“C probe may want to consult this almost encyclopedic work on the variety of applications researchers have found for ‘VI NMR spectroscopy. FRANK JORDAN, Rutgers, the State Universiiy, Newark, New Jersey 07102
Chromatographic Systems: Maintenance and Troubleshooting. By J. Q. WALKER, M. T. JACKSON, JR., AND 3. B. MAYNARD. Academic Press, New York and London, 197 1. ix + 289 pp. $8.95. It is hard to imagine any laboratory engaged in the analysis of organic substances which does not use some chromatographic methods. Gas- and liquid-chromatographic instruments represent a reasonable investment of money. When said instruments are in need of repair however they are of no use. Worse yet, in smaller laboratories the loss of such equipment can lead to overcrowding of back up units and often the underutilization of personnel. The present book provides a means for even the smallest laboratory using gas or liquid chromatographic instruments to provide all important routine maintenance procedures as well as methods for troubleshooting the instrument when problems do develop. The book consists of two parts, liquid chromatography and gas chromatography. In dealing with the first method there are sections on an introduction to I.C. describing basic procedures and very limited theory. There is a section on the solvent transport system which provides numerous hints for actually running a separation as well as tables and text which describes symptoms of malfunctions erroneously associated with pump
342
BOOK
REVIEWS
failure. The next section describes sample introduction systems including recommendations on choosing septa for various solvents. This is followed by a section on section and choice of a column, ovens and heaters, and detection systems. A final section is a guide for trouble shooting an I.C. systems which shows recorder output indicating problems, the cause of such problems and what corrective action to take to eliminate the condition. The discussion of gas chromatography is equally useful. After an introduction, there are sections on pneumatic and sample introduction systems, pyrolytic inlet systems, column ovens, and temperature controllers, detectors, electronics, auxiliary systems (GC-IR, GC-MS combinations, and molecular separators), and finally comprehensive system troubleshooting. This is a fine, useful work which will easily pay for itself in improved instrument performance and by reducing the number of service calls. It is highly recommended to the users of such instrumentation. It is also good reading for anyone new to the techniques. PAUL HEMMES, Rutgers,
Ultracentrifugation
the State University,
of Macromolecules.
Newark,
By J. W. WILLIAMS.
New Jersey 07102
Academic Press,
Inc., New York, 1972. xviii + 118 pp. $9.50 It may seem out of place to see the prefix macro in the title of a book reviewed in a journal concerned with micro procedures. However, macromolecules are large only in a relative sense, and ultrucentrifugution is a valuable technique for the separation of substances small in either size or quantity. Dr. Williams, well qualified in this field, has written an authoritative monograph. The first two chapters are concerned with polydisperse solute systems and cover sedimentation equilibrium in polydisperse nonideal solutions and size distribution analysis by ultracentrifugal methods. The first chapter also contains a brief but lucid exposition of the history and theory of the ultracentrifuge. Chapters three and four discuss self-association reactions in protein systems-the third presenting work on P-lactoglobulin B. lysozyme, and chymotrypsinogen B, and the fourth covering the sedimentation analysis of a multiple y G-globulin. Each chapter gives the theory of the process involved. An appendix, approximately a third of the entire book, contains a brief introduction to the theory of the ultracentrifugal analysis and describes the demonstration of molecular homogeneity in terms of sedimentation velocity and sedimentation equilibrium. Mathematical equations and their derivation are used freely throughout the text. Each chapter is followed by an ample bibliography, and there is also a good subject index. A complete list of symbols precedes the first chapter. Anyone concerned with the application of ultracentrifugal analysis to problems in physical biochemistry and organic high polymers will find this book useful and valuable. DAVID B. SABINE, 484 Hawthorne
Avenue,
Yonkers, New York 10705
Oxidation in Organic Chemistry. Vol. 5-B. Edited by W. S. TRAHANOVSKY. Academic Press, New York, 1973. XI + 248 pp. $15.00.
This is the second part of the two-volume monograph on oxidation which is part of the ongoing series of monographs under the general editorship of Blomquist and Wasserman. The first part of the monograph was edited by Wiberg and published in 1965. Three of the four chapters deal with specific oxidants, namely: copper (II), thallium
REVIEWS
341
shifts, the other with 13C coupling constants to 13C and other magnetic nuclei. Each segment contains three elements of analyses: experimental techniques used in acquiring the data, a substantial compilation of data and theoretical explanations and correlations of the experimental data. The chemical shift compilation includes chapters on hydrocarbons, substituted hydrocarbons, organometallics and carbonium ions, heterocyclic compounds and on functional groups (i.e., carbonyls and nitriles). As throughout the rest of the book references well into 197 1 seem to be in evidence. Because of the well-resolved spectra obtained for simpler molecules, “C magnetic resonance has proved to be and will continue to be a fertile ground for theoretical model building and the author presents a wide survey of the successes and failures of the theoretical approaches employed to account for chemical shift and coupling-constant correlations. and 11C-‘SF data priThe coupling-constant tabulation includes I:iC-‘H, l”C-‘“C, marily but also lists ‘“C coupling data to other magnetic nuclei such as zr’P, lSN and others. Finally, a brief survey of the applications of ‘“C nuclear magnetic spectroscopy to the solution of a variety of problems is presented. Outstanding among these are ‘“C studies on conformational equilibria and ring inversion barriers in mobile cyclohexane like systems and conformational analysis of carbohydrates; l”C analysis of nucleic acid constituents; of amino acids and polypeptides and the very important use of 13C as tracer in biosynthetic mechanistic studies. Clearly, with the advent of widespread availability of pulsed NMR instruments, the myriad of applications of rsC nuclear magnetic resonance are yet to be explored. The book is to be recommended as an essential addition to any library since it is a convenient starting point for a literature search for anyone comtemplating a ‘K experiment. More than that, anyone having access to an instrument with a ‘“C probe may want to consult this almost encyclopedic work on the variety of applications researchers have found for ‘VI NMR spectroscopy. FRANK JORDAN, Rutgers, the State Universiiy, Newark, New Jersey 07102
Chromatographic Systems: Maintenance and Troubleshooting. By J. Q. WALKER, M. T. JACKSON, JR., AND 3. B. MAYNARD. Academic Press, New York and London, 197 1. ix + 289 pp. $8.95. It is hard to imagine any laboratory engaged in the analysis of organic substances which does not use some chromatographic methods. Gas- and liquid-chromatographic instruments represent a reasonable investment of money. When said instruments are in need of repair however they are of no use. Worse yet, in smaller laboratories the loss of such equipment can lead to overcrowding of back up units and often the underutilization of personnel. The present book provides a means for even the smallest laboratory using gas or liquid chromatographic instruments to provide all important routine maintenance procedures as well as methods for troubleshooting the instrument when problems do develop. The book consists of two parts, liquid chromatography and gas chromatography. In dealing with the first method there are sections on an introduction to I.C. describing basic procedures and very limited theory. There is a section on the solvent transport system which provides numerous hints for actually running a separation as well as tables and text which describes symptoms of malfunctions erroneously associated with pump
342
BOOK
REVIEWS
failure. The next section describes sample introduction systems including recommendations on choosing septa for various solvents. This is followed by a section on section and choice of a column, ovens and heaters, and detection systems. A final section is a guide for trouble shooting an I.C. systems which shows recorder output indicating problems, the cause of such problems and what corrective action to take to eliminate the condition. The discussion of gas chromatography is equally useful. After an introduction, there are sections on pneumatic and sample introduction systems, pyrolytic inlet systems, column ovens, and temperature controllers, detectors, electronics, auxiliary systems (GC-IR, GC-MS combinations, and molecular separators), and finally comprehensive system troubleshooting. This is a fine, useful work which will easily pay for itself in improved instrument performance and by reducing the number of service calls. It is highly recommended to the users of such instrumentation. It is also good reading for anyone new to the techniques. PAUL HEMMES, Rutgers,
Ultracentrifugation
the State University,
of Macromolecules.
Newark,
By J. W. WILLIAMS.
New Jersey 07102
Academic Press,
Inc., New York, 1972. xviii + 118 pp. $9.50 It may seem out of place to see the prefix macro in the title of a book reviewed in a journal concerned with micro procedures. However, macromolecules are large only in a relative sense, and ultrucentrifugution is a valuable technique for the separation of substances small in either size or quantity. Dr. Williams, well qualified in this field, has written an authoritative monograph. The first two chapters are concerned with polydisperse solute systems and cover sedimentation equilibrium in polydisperse nonideal solutions and size distribution analysis by ultracentrifugal methods. The first chapter also contains a brief but lucid exposition of the history and theory of the ultracentrifuge. Chapters three and four discuss self-association reactions in protein systems-the third presenting work on P-lactoglobulin B. lysozyme, and chymotrypsinogen B, and the fourth covering the sedimentation analysis of a multiple y G-globulin. Each chapter gives the theory of the process involved. An appendix, approximately a third of the entire book, contains a brief introduction to the theory of the ultracentrifugal analysis and describes the demonstration of molecular homogeneity in terms of sedimentation velocity and sedimentation equilibrium. Mathematical equations and their derivation are used freely throughout the text. Each chapter is followed by an ample bibliography, and there is also a good subject index. A complete list of symbols precedes the first chapter. Anyone concerned with the application of ultracentrifugal analysis to problems in physical biochemistry and organic high polymers will find this book useful and valuable. DAVID B. SABINE, 484 Hawthorne
Avenue,
Yonkers, New York 10705
Oxidation in Organic Chemistry. Vol. 5-B. Edited by W. S. TRAHANOVSKY. Academic Press, New York, 1973. XI + 248 pp. $15.00.
This is the second part of the two-volume monograph on oxidation which is part of the ongoing series of monographs under the general editorship of Blomquist and Wasserman. The first part of the monograph was edited by Wiberg and published in 1965. Three of the four chapters deal with specific oxidants, namely: copper (II), thallium