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Introduction to microwave sample preparation
MICROCHEMICAL
JOURNAL
41, 121-123 (1990)
BOOK REVIEWS
Introduction to Microwave Sample Preparation. Edited by H. M. KINGSTON AND LOIS B. JASSIE. American Chemical Society, Washington, D.C., 1988. xxii + 263 pp., $49.95 (U.S. and Canada), $59.95 (Export). As one who spent innumerable hours in his younger years moving samples around hot plates and in and out of muffle furnaces, not to mention encounters with Kjeldahl flasks and Carius tubes, this book comes as the guide to a new and wondrous age. Although microwaves have been used in sample preparation and analysis during the last few years, this is the first book, to my knowledge, to give a thorough and up to date presentation of the theory and application of this new technology. In the preface the editors state, “This reference book is designed to enable individuals to equip and operate a microwave sample preparation laboratory in a safe, productive, and cost effective manner.” This they have done very well. In Chapter 1 the editors give a chronological review of the literature of microwave-assisted sample preparation. Innovations including fiber optic thermometry are surveyed. Chapter 2, “Microwave Heating: Theoretical Concepts and Equipment Design,” is intended to give those working in Analytical Chemistry not only a theoretical understanding of microwave heating and its relation to sample preparation but also a description of how microwave hardware functions in sample preparation. Open-vessel digestion, closed-vessel digestion, microwave muffle furnaces, and microwave ashing blocks are discussed. Chapters 3,4, and 5 address applications involving geological, metallurgical, and biological samples. Biological samples are discussed again both in Chapter 7, where microwave digestion is described as a method of preparing samples for selenium determination by electrothermal atomic absorption spectrometry, and again in Chapter 8, where Kjeldahl nitrogen determination using a microwave system is described. Chapter 6, “Monitoring and Predicting Parameters in Microwave Dissolution,” is summarized by the authors as follows: Procedures are described for the real time measurement of temperature and pressure during closed-vessel microwave sample decomposition. Pressure and temperature profiles of biological Standard Reference Materials and solitary as well as mixed acids are given to illustrate unique advantages that are available with the closed-vessel technique. A set of equations that permits prediction of target temperatures and times is derived from the fundamental heat capacity relationship for absorptive materials. From a series of fundamental measurements, original equations are introduced that permit the power consumption of common mineral acids to be calculated. This method is proposed as a model to approximate the thermal behavior of reagents intended for microwave use. The fundamental degradation patterns of biological matrices arc presented for model compounds. This chapter is “must reading” for anyone wanting to undertake microwave dissolution in a systematic fashion. Chapters 7, 8, 9, and 10 cover microwave digestion of biological samples, Kjeldahl nitrogen determination using a microwave system, remote operation and chemical dissolution in highly radioactive environments, and both manual and robotically controlled microwave dissolution of minerals, respectively. Chapter 11 is devoted to safety guidelines for microwave systems in the analytical laboratory. This chapter and the literature cited are “must reading” before these procedures are undertaken. The
121 0026-265X90
$1.50
Copyrisbt 0 1990 by Academic F’ress, Inc. Au rights of reproduction in any form reserved.
122
BOOK REVIEWS
relatively new technique of microwave sample preparation plus the use of microwave equipment introduce unique factors that many analysts have not yet encountered. Although there is a certain amount of redundancy in this book as chapters were written as independent units by a variety of experts, it is to be highly recommended to all analysts involved in bringing samples into solution. JAMES J. MARKHAM Department of Chemistry Villanova University Villanova, Pennsylvania HO85 Practical Statistics for the Physical Sciences. By L. L. HAVILCEK AND R. D. CRAIN. American Chemical Society, Washington, D.C., 1988. xvi + 489 pp., $59.95. This is a well-written introductory book on statistics with a large number of illustrative worked-out examples applied to chemical situations. Problems are provided for the reader to work at the end of nearly every chapter and answers are provided to these problems in a separate section near the end of the book. The most significant needed statistical equations are printed directly on the inside of the front and back covers and their facing pages. Much of the subject content is the same as that in any elementary book on statistics such as the deftition of terms, calculation of measures of central tendency, and uses of the t test. Verm diagrams are also included to help clarify statistical concepts. Unfortunately, many examples are based on hypothetical data, which raises questions in the reader’s mind as to how well the treatment that is read will apply to actual practice. There is very minimal treatment of control charts, about one-half page only. This is unfortunate because of their wide applications in industrial process work and analytical laboratories. The section on the use of factorial design of experiments which is the statistical treatment and interpretation of the interaction of factors is very good. The “Latin Square” concept is very well explained. References are provided at the end of each chapter, although readers needing to study statistics from this book probably would not gain much comfort and assistance from the cited literature. Minimal information is provided on commercially available statistical programs for computer use. No comparison of the listed programs is offered nor are any suggestions as to the desirability of one set of programs over another; mainly a listing is given. This is mentioned because of the large availability of personal computers capable of running statistical software so that information on the use of personal computers for statistical calculations could be incorporated into the book and thus would make problem solving as well as future applications much easier. Furthermore, in the biographical information about the authors in this “American Chemical Society Professional Reference Book,” the reader is informed that one of the co-authors currently is the co-owner of a computer store. The incorporation of computer use would enhance the practical value of the book immensely. This disregard of computer use and the lack of a definitive control chart treatment are probably the greatest weaknesses of this otherwise well-prepared book. In addition to the usual section on statistical tables (which are printed in blue to make it easy to find them), the book contains a glossary of statistical terms, as well as a good index. It would make an excellent text for an undergraduate course or an excellent reference for anyone desiring information on the basic theory and applications of basic statistics. PETER F. Lore Chemistry Department University of Missouri Kansas City, Missouri 64110
Electroanalytlcal Techniques in Clllcal Chemistry and Laboratory Medlclne. By J. WANG. VCH Publishers, Inc., New York, 1988. x + 177 pp., $45.00. The five chapters in this book are, respectively: Chapter 1 “Voltammetry and Other Controlled-Potential Techniques” Chapter 2 “Ion Selective Electrodes in Clinical Medicine”
JOURNAL
41, 121-123 (1990)
BOOK REVIEWS
Introduction to Microwave Sample Preparation. Edited by H. M. KINGSTON AND LOIS B. JASSIE. American Chemical Society, Washington, D.C., 1988. xxii + 263 pp., $49.95 (U.S. and Canada), $59.95 (Export). As one who spent innumerable hours in his younger years moving samples around hot plates and in and out of muffle furnaces, not to mention encounters with Kjeldahl flasks and Carius tubes, this book comes as the guide to a new and wondrous age. Although microwaves have been used in sample preparation and analysis during the last few years, this is the first book, to my knowledge, to give a thorough and up to date presentation of the theory and application of this new technology. In the preface the editors state, “This reference book is designed to enable individuals to equip and operate a microwave sample preparation laboratory in a safe, productive, and cost effective manner.” This they have done very well. In Chapter 1 the editors give a chronological review of the literature of microwave-assisted sample preparation. Innovations including fiber optic thermometry are surveyed. Chapter 2, “Microwave Heating: Theoretical Concepts and Equipment Design,” is intended to give those working in Analytical Chemistry not only a theoretical understanding of microwave heating and its relation to sample preparation but also a description of how microwave hardware functions in sample preparation. Open-vessel digestion, closed-vessel digestion, microwave muffle furnaces, and microwave ashing blocks are discussed. Chapters 3,4, and 5 address applications involving geological, metallurgical, and biological samples. Biological samples are discussed again both in Chapter 7, where microwave digestion is described as a method of preparing samples for selenium determination by electrothermal atomic absorption spectrometry, and again in Chapter 8, where Kjeldahl nitrogen determination using a microwave system is described. Chapter 6, “Monitoring and Predicting Parameters in Microwave Dissolution,” is summarized by the authors as follows: Procedures are described for the real time measurement of temperature and pressure during closed-vessel microwave sample decomposition. Pressure and temperature profiles of biological Standard Reference Materials and solitary as well as mixed acids are given to illustrate unique advantages that are available with the closed-vessel technique. A set of equations that permits prediction of target temperatures and times is derived from the fundamental heat capacity relationship for absorptive materials. From a series of fundamental measurements, original equations are introduced that permit the power consumption of common mineral acids to be calculated. This method is proposed as a model to approximate the thermal behavior of reagents intended for microwave use. The fundamental degradation patterns of biological matrices arc presented for model compounds. This chapter is “must reading” for anyone wanting to undertake microwave dissolution in a systematic fashion. Chapters 7, 8, 9, and 10 cover microwave digestion of biological samples, Kjeldahl nitrogen determination using a microwave system, remote operation and chemical dissolution in highly radioactive environments, and both manual and robotically controlled microwave dissolution of minerals, respectively. Chapter 11 is devoted to safety guidelines for microwave systems in the analytical laboratory. This chapter and the literature cited are “must reading” before these procedures are undertaken. The
121 0026-265X90
$1.50
Copyrisbt 0 1990 by Academic F’ress, Inc. Au rights of reproduction in any form reserved.
122
BOOK REVIEWS
relatively new technique of microwave sample preparation plus the use of microwave equipment introduce unique factors that many analysts have not yet encountered. Although there is a certain amount of redundancy in this book as chapters were written as independent units by a variety of experts, it is to be highly recommended to all analysts involved in bringing samples into solution. JAMES J. MARKHAM Department of Chemistry Villanova University Villanova, Pennsylvania HO85 Practical Statistics for the Physical Sciences. By L. L. HAVILCEK AND R. D. CRAIN. American Chemical Society, Washington, D.C., 1988. xvi + 489 pp., $59.95. This is a well-written introductory book on statistics with a large number of illustrative worked-out examples applied to chemical situations. Problems are provided for the reader to work at the end of nearly every chapter and answers are provided to these problems in a separate section near the end of the book. The most significant needed statistical equations are printed directly on the inside of the front and back covers and their facing pages. Much of the subject content is the same as that in any elementary book on statistics such as the deftition of terms, calculation of measures of central tendency, and uses of the t test. Verm diagrams are also included to help clarify statistical concepts. Unfortunately, many examples are based on hypothetical data, which raises questions in the reader’s mind as to how well the treatment that is read will apply to actual practice. There is very minimal treatment of control charts, about one-half page only. This is unfortunate because of their wide applications in industrial process work and analytical laboratories. The section on the use of factorial design of experiments which is the statistical treatment and interpretation of the interaction of factors is very good. The “Latin Square” concept is very well explained. References are provided at the end of each chapter, although readers needing to study statistics from this book probably would not gain much comfort and assistance from the cited literature. Minimal information is provided on commercially available statistical programs for computer use. No comparison of the listed programs is offered nor are any suggestions as to the desirability of one set of programs over another; mainly a listing is given. This is mentioned because of the large availability of personal computers capable of running statistical software so that information on the use of personal computers for statistical calculations could be incorporated into the book and thus would make problem solving as well as future applications much easier. Furthermore, in the biographical information about the authors in this “American Chemical Society Professional Reference Book,” the reader is informed that one of the co-authors currently is the co-owner of a computer store. The incorporation of computer use would enhance the practical value of the book immensely. This disregard of computer use and the lack of a definitive control chart treatment are probably the greatest weaknesses of this otherwise well-prepared book. In addition to the usual section on statistical tables (which are printed in blue to make it easy to find them), the book contains a glossary of statistical terms, as well as a good index. It would make an excellent text for an undergraduate course or an excellent reference for anyone desiring information on the basic theory and applications of basic statistics. PETER F. Lore Chemistry Department University of Missouri Kansas City, Missouri 64110
Electroanalytlcal Techniques in Clllcal Chemistry and Laboratory Medlclne. By J. WANG. VCH Publishers, Inc., New York, 1988. x + 177 pp., $45.00. The five chapters in this book are, respectively: Chapter 1 “Voltammetry and Other Controlled-Potential Techniques” Chapter 2 “Ion Selective Electrodes in Clinical Medicine”