Books in Analytical separations

Selective Sample Handling and Detection in High-Performance Liquid Chromatography

1st Edition
Volume B
October 30, 1989
K. Zech + 1 more
English
eBook
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This is the second of a two-volume project which treats the handling, separation and detection of complex samples as an integrated, interconnected process. On the basis of this philosophy the editors have selected those contributions which demonstrate that optimal sample preparation leads to a simplification of detection or reduced demands on the separation process. Throughout the book emphasis is on chemical principles with minimum discussion of the equipment required - an approach which reflects the editors' view that the limiting factor in the analysis of complex samples is an incomplete knowledge of the underlying chemistry rather than the hardware available. This lack of knowledge becomes more evident as the demands for lower detection limits grow, as solving complex matrix problems requires a greater understanding of the chemical interaction between the substance to be analysed and the stationary phase. Thus, apart from one chapter dealing with chemically modified silicas, the main theme of the book is developed in three chapters on sample preparation and three on detection.The opening chapter outlines concentration and chromatography on chemically modified silicas with complexing properties, and gives examples of the use of these phases with organic and inorganic compounds. Chapter II, the first of the three contributions dealing with sample preparation, addresses such questions as whether the prepared sample is representative of the material to be analysed; how to avoid contamination; which separation procedure should be used to avoid tedious sample preparation. Chapter III describes the processing of whole blood for drug analysis. The determination of cyclosporine and its metabolites (an especially difficult case) demonstrates how comprehensive the optimisation of sample preparation must be to successfully perform the analysis. Several other examples are also given. Chapter IV deals with radio-column liquid chromatography and introduces the other theme of the book, i.e. selective detection methods. The widespread use of radioisotopes requires a high degree of purification during the manufacture of the compounds, as well as highly accurate detection methods in biological and biochemical studies.Chapter V continues the theme of selective detection with an overview of post-column reaction detection. The use of immobilised enzymes in post-column reactors or `pumpless' reactor systems for on-line reagent generation after the chromatographic separation step is discussed in detail. Various examples of the separation of biological compounds show how the production of electrochemical reagents and photochemical reaction detection have increased the selectivity of the detection, leading to more economical analytical systems. Selective detection employing luminescence detection techniques is outlined in Chapter VI. The use of immobilised fluorophores or the coupling to photochemical reactions leads to highly selective detection systems which can greatly simplify the sample handling. The final chapter reviews the use of continuous separation techniques in flow injection analysis thus revealing the need for a strong interdisciplinary dependence between sample handling and separation in this area.Written by experienced practitioners, this book will be extremely useful to investigators in many areas of application. Each chapter includes sufficient references to the literature to serve as a valuable starting point for more detailed investigation. The strong emphasis on sample handling makes the book unique in many ways and it will be welcomed by environmental scientists as well as those active in the clinical, pharmaceutical and bioanalytical fields.

Natural Products Isolation

1st Edition
Volume 43
December 1, 1988
G.H. Wagman + 1 more
English
eBook
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This new book encompasses, in great detail, the most recent progress made in the isolation and separation of natural products. It covers antibiotics, marine and plant-derived substances, enzyme inhibitors and interferons. The most recent separation methodology is described. Although there is a bias toward antibiotics, it was done because this is still the largest natural products area of research.The fourteen chapters are written by experts in their respective fields. The first two chapters are largely devoted to new methodology applied to purification of a variety of compounds. They include an extensive review and new applications of counter-current chromatography and the newly emerging HPLC-photodiode array technology. Chapter 3 provides a review of affinity chromatography applied to the separation of antibiotics for the first time. Next are chapters on antimicrobials with an update on all the most recent &bgr;-lactam (after 1976) discoveries. A comprehensive review of a very important class of antiparasitic agents - the avermectins - follows. An update of isolation and purification of a variety of marine-derived compounds is next. The succeeding chapter is a comprehensive review of the most recent developments in isolation and purification of interferons. This is followed by a discussion of enzyme inhibitors and their isolation and purification and ties in with a chapter on plant-derived natural products, some of which are also in this same category. The final chapter is a futuristic essay indicating the isolation of minute amounts of natural products and the fascinating biological properties which they possess.The book has extensive isolation schemes, tables, figures and chemical structures. In many instances a short summary of the producing organism, brief chemical description and structure and biological activity of the compounds is presented. Detailed information of extraction, separation and purification techniques follow. Each chapter has an extensive bibliography and, where applicable, an appendix showing sources of materials and equipment. A detailed index to the subject matter is included at the end of the book.The book thus offers the reader: up-to-date reviews (including 1988) of specific topics in the natural products field not to be found elsewhere; information on new chromatographic methods and techniques described in sufficient detail to be utilized by investigators in this area of research; and extensive references to enable the serious researcher to pursue particular information. It will appeal to pharmaceutical and natural products researchers and is a valuable acquisition for university chemistry and biochemistry departments.

Separation of Individual Compound Classes

1st Edition
Volume B
November 1, 1988
O. Mikes
English
eBook
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Quantitative Gas Chromatography for Laboratory Analyses and On-Line Process Control

1st Edition
Volume 42
June 1, 1988
G. Guiochon + 1 more
English
eBook
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Here is an invaluable new book on quantitative gas chromatography which explains how the method can - or should - be used for accurate and precise analysis. Gas chromatography is firmly established as one of the few major methods for the quantitative analysis of complex mixtures. It is fast, accurate and inexpensive, with a broad range of applications. It has however become very complex and involved: over 200 stationary phases, more than 10 detector principles and several very different column types are available from among the catalogs of over 100 manufacturers and major retailers. The progressive changes in the nature of gas chromatography have created new needs for information which are not satisfied by the literature presently available.This book provides a complete discussion of all the problems involved in the achievement of quantitative analysis by gas chromatography, whether in the research laboratory, in the routine analysis laboratory or in process control. For this reason the presentation of theoretical concepts has been limited to the essential, while extensive explanations have been devoted to the various steps involved in the derivation of precise and accurate data. This starts with the selection of the instrumentation and column, continues with the choice of optimum experimental conditions, then calibration and ends with the use of correct procedures for data acquisition and calculations. Finally, there is almost always a way to reduce errors and an entire chapter deals with this single issue. Numerous relevant examples are presented.The first part of the book presents the theoretical background, simple enough to be understood by all analytical chemists, but still complete and up-to-date. It discusses the problems of flow dynamics, retention and band broadening. The changes in band profile associated with column overloading are explained without much recourse to mathematics. The second part describes the gas chromatograph and discusses the properties of each of its parts: gas flow and pressure controller sampling system, oven, column switching valves, detectors. The different implementations, their advantages and drawbacks are discussed and compared. In addition, three chapters present packed column technology, open tubular column technology and some sophisticated new phase systems, respectively. The new phase systems described use adsorbents, modified by coating or grafting organic phase, and carrier gases containing vapors which are sorbed by the stationary phase and modify it, such as steam. The third part discusses the applications in qualitative and quantitative analysis. Calibration, peak integration, sources of errors arising from the various parts of the instrument as well as from the measurement process itself are carefully described in four detailed chapters. Methods to carry out accurate and precise analysis are presented. A last chapter is devoted to process control analysis and gives a number of detailed examples of applications. A lexicon explaining the most important chromatographic terms and a detailed index complete the book.This is a book which no chemical analyst should be without. It should be on the library shelf of all universities, instrument companies and any laboratory and plant where gas chromatography is used.

Aqueous Size-Exclusion Chromatography

1st Edition
Volume 40
May 1, 1988
P.L. Dubin
English
eBook
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The rapid development of new packings for aqueous size-exclusion chromatography has revolutionized this field. High resolution non-adsorptive columns now make possible the efficient separation of proteins and the rapid and precise determination of the molecular weight distribution of synthetic polymers. This technology is also being applied to the separation of small ions, the characterization of associating systems, and the measurement of branching. At the same time, fundamental studies are elucidating the mechanisms of the various chromatographicproce... developments in principles and applications are assembled for the first time in this book. Fundamental issues are dealt with: the roles of pore structure and macromolecular dimensions, hydrophobic and electrostatic effects, and the determination and control of column efficiency. High-performance packings based on derivatized silica are reviewed in detail. Special techniques are thoroughly described, including SEC/LALLS, inverse exclusion chromatography, and frontal zone chromatography. Attention is focussed on special applications of size-exclusion methods, such as the characterization of micelles, separations of inorganic ions, and Hummel-Dreyer and related methods for equilibrium systems. Protein chromatography is dealt with in both dedicated sections and throughout the book as a whole.This is a particularly comprehensive and authoritative work - all the contributions review broad topics of general significance and the authors are of high repute. The material will be of special value for the characterization of synthetic water-soluble polymers, especially polyelectrolytes. Biochemists will find fundamental and practical guidance on protein separations. Researchers confronted with solutes that exhibit complex chromatographic behavior, such as humic acids, aggregating proteins, and micelles should find the contents of this volume illuminating.

Preparative Liquid Chromatography

1st Edition
Volume 38
July 1, 1987
B.A. Bidlingmeyer
English
eBook
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This volume provides a straightforward approach to isolation and purification problems with a thorough presentation of preparative LC strategy including the interrelationship between the input and output of the instrumentation, while keeping to an application focus.The book stresses the practical aspects of preparative scale separations from TLC isolations through various laboratory scale column separations to very large scale production. It also gives a thorough description of the performance parameters (e.g. throughput, separation quality, etc.) as a function of operational parameters (e.g. particle size, column size, solvent usage, etc.). Experts in the field have contributed a well balanced presentation of separation development strategies from preparative TLC to commercial preparative process with practical examples in a wide variety of application areas such as drugs, proteins, nucleotides, industrial extracts, organic chemicals, enantiomers, polymers, etc.

Polymer Characterization by Liquid Chromatography

1st Edition
Volume 34
February 1, 1987
G. Glöckner
English
eBook
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The main subject of this book is the characterization of plastics. To a high degree the properties of these polymers depend on the distribution of the molar mass and of other structural features, and small deviations frequently have a great effect. Therefore the characterization of polymers cannot be restricted to the determination of mean values but must yield information on these distributions. Using classical methods, the analytical fractionation of polymer homologues and structurally isomeric polymers is extremely time-consuming. Therefore, efficient chromatographic techniques are being increasingly employed in modern polymer characterization.In the first place, high-performance liquid chromatography is applied, in the form of size exclusion chromatography. It is also possible, however, to use other separation modes. More space is devoted to these other possibilities in this volume than is merited by their current range of applications, as the author believes that many separation problems will be solved by separation techniques of the non-exclusion type. Nevertheless, much emphasis is placed on size exclusion chromatography. Not only because of its current wide range of applications, but also because its relative importance, as a complement to other chromatographic techniques may even increase in the forthcoming years.This book is the first to cover all phenomena related to the above considerations. Starting with an introduction to basic liquid chromatography and to polymer science, it deals with the adsorption behaviour of polymers, with gradient techniques, with the kinetic band broadening in liquid chromatography, with instrumental features and packing materials. The book consists of four balanced sections and related information from about 1800 references is compiled in the tables. Some 250 figures and 30 tables will help give the reader a clear insight of the topics discussed. The book is aimed at helping the analyst or polymer chemist who is looking for information about chromatographic methods for the characterization of polymers.

Chemical Derivatization in Gas Chromatography

1st Edition
Volume 19
July 1, 1986
J. Drozd
English
eBook
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Selective Gas Chromatographic Detectors

1st Edition
Volume 36
July 1, 1986
M. Dressler
English
eBook
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This book gives a comprehensive, up-to-date review of all selective detectors used in combination with gas chromatography. For each detector, the historical background, design and principle are described, and the working parameters affecting the detector performance are analyzed critically and in detail. The analytical possibilities of the detectors and the main characteristics such as sensitivity, noise and minimum detectability are discussed. All the selective detectors that are currently used are discussed in detail. Combinations of GC with other techniques such as plasma emission spectroscopy, atomic absorption spectrometry, ion-selective electrodes, piezoelectric sorption detector, mass spectrometry and infrared spectroscopy are discussed briefly.Chromatograp... and users of gas chromatographs, especially in the field of environmental protection, agriculture, clinical chemistry, and toxicology will find the book useful to their work. Institutes and organisations dealing with analytical chemistry will also find it of interest.

Liquid Chromatography Detectors

2nd Edition
Volume 33
February 1, 1986
R.P.W. Scott
English
eBook
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The renaissance of liquid chromatography took place in the late 1960's and early 1970's. The first edition of this book published in 1977 described the detectors that were available at that time and which provided a performance matching that of the contemporary equipment with which they were associated. It is interesting to note that the most popular detectors then (the UV detector, the refractometer detector, the fluorescence detector and the electrical conductivity detector) are still the most commonly used detectors nearly a decade later. Detector design, however, has changed very significantly over the intervening years. Modern high efficiency columns provide very narrow peaks and very fast separations, and thus the physical design of the detectors had to change to meet these new challenges. In 1977, there was little real understanding of the important role played by the detector in the overall function of the chromatographic system and although some of the factors were pointed out in the first edition of this book, in retrospect they appeared to be little understood.This second edition gives an entirely new presentation of the subject of liquid chromatography detectors. It contains sections dealing with the fundamental aspects of the interaction between columns and detectors and the interaction between ancillary equipment and the detector. It brings the reader up-to-date with new designs and novel detecting systems that have been developed since 1977 and extends significantly the subject of the association of the liquid chromatography detector with spectroscopic techniques. In particular the book now explores the association of liquid chromatography with nuclear magnetic resonance, infrared and atomic absorption spectrometry. This book not only gives a comprehensive treatment of the subject of liquid chromatographic detectors and provides a rational procedure for defining their performance and so permit valid comparisons, but also discusses detector performance in relation to the whole of the chromatographic system.

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