Sample Preparation in Chromatography - 1st Edition - ISBN: 9780444503947, 9780080540702

Sample Preparation in Chromatography, Volume 65

1st Edition

Authors: S.C. Moldoveanu V. David
eBook ISBN: 9780080540702
Hardcover ISBN: 9780444503947
Imprint: Elsevier Science
Published Date: 8th May 2002
Page Count: 942
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Table of Contents

Part 1. Introduction and General Considerations. Preparatory information. Overview of a chemical analysis. Types of operations used in sample preparation. Some theoretical aspects of phase transfers. Introductory approach to theory of distribution equilibrium. Some aspects of mass transfer processes. Characterization of chromatographic separations. General characteristics of separations. Elementary discussion on thermodynamic and kinetic factors in chemical reactions. Brief survey on molecular interactions. Empirical and estimated parameters for sample preparation problems. Introductory discussion on precision, accuracy, sensitivity, and limit of detection in chemical analysis. Validation of an analytical method.

Sampling and Its Connection with Sample Preparation. Relation of sampling to sample preparation. Representative samples. Techniques for sample collection. Handling, preservation, and storage of samples.

Overview on Sample Preparation for Chromatography. The role of sample preparation. The use of preliminary information for the choice of a sample preparation procedure. Sample homogenization and dissolution. Sample cleanup, fractionation, and concentration. Chemical modifications of the sample. Other types of sample modifications. Differences in sample preparation for different chromatographic techniques. Quantitation techniques in chromatography and their relation to sample preparation. Method development in sample preparation.

Chromatography as the Core Step in an Analytical Process.

The choice of the core analytical technique. Gas chromatography as a core step in the analytical process. Conventional high performance liquid chromatography as a core analytical technique. Other chromatography types used as a core analytical technique.

Data Processing in Chromatographic Methods. Information gain from chromatographic data. Qualitative and quantitative data from the chromatographic process.

Automation in Sample Preparation. Automation in the instrumentation used in sample preparation. Computer assisted method development.

Part 2. Sample Preparation Techniques Using Physical Processes.

Mechanical processing in sample preparation. Grinding, sieving, and blending. Filtration, microfiltration, and ultrafiltration. Centrifugation.

Phase Transfer Separations Applied in Sample Preparation. Distillation, vaporization, and drying. Dissolution, crystallization, and precipitation.

Headspace Sampling Techniques in Gas Chromatography. Static headspace techniques. Dynamic headspace. Other headspace techniques.

Solvent Extraction.

Liquid-liquid extraction. Conventional liquid-solid extraction. Accelerated solvent extraction. Microwave-assisted solvent extraction. Simultaneous distillation and extraction. Supercritical solvent extraction.

Sorbent Extraction. Solid phase extraction procedures. Solid phase microextraction. Matrix solid phase dispersion. Other solid phase sample preparation techniques.

Chromatographic Procedures as Preliminary Separation.

Gas chromatography as a sample preparation technique and bidimensional GC. Liquid chromatography as a sample preparation technique. Size exclusion used in sample preparation.

Membrane Separations.

Gas diffusion through membranes and stripping. Reverse osmosis and dialysis.

Electroseparation Techniques in Sample Preparation.

Electrophoretic techniques. Other electroseparation techniques.

Other Separation Techniques in Sample Preparation. Ion exchange in sample preparation. Other techniques in sample preparation.

Part 3. Sample Preparation Techniques Involving Chemical Modifications .

Chemical Modifications for Dissolution and Fractionation. Chemical modifications for sample dissolution. Changes in pH and chemical modifications for fractionation purposes.

Purpose of Derivatization in Chromatographic Analysis. General aspects regarding derivatization. Preparation of the sample for derivatization and common derivatization labware. Derivatization for improving gas chromatographic process. Derivatization for improving detection in GC. Derivatization for Improving mass spectral identification. Derivatization for improving detection in HPLC and TLC. Derivatization for chiral separations.

Chemical Reactions used in Derivatization.

Reactions with formation of Alkyl or Aryl derivatives. Silylation reactions. Acylation reactions. Reactions of addition to Carbon-Heteroatom multiple bonds used for derivatization. Derivatization reactions with formation of cyclic compounds. Other derivatization reactions. Derivatization reactions involving solid phase reagents. Derivatization on a solid support.

Derivatization Reactions for Analytes with Various Functional Groups.

Derivatization of compounds with Alcohols, Epoxide, or Ether Groups. Derivatization reactions for Phenols. Derivatization reactions for Thiols and Sulfides. Derivatization of compounds with Amino and other Nitrogen-containing groups. Derivatization of Aldehydes and Ketones. Derivatization of Carboxylic acids. Derivatization of Amides, Esters, and other derivatives of Carboxylic acids, and of Carbonic acid. Derivatization of other organic groups and organometallic and inorganic compounds. Derivatization of carbohydrates. Derivatization of Amino acids and related compounds. Derivatization of other multifunctional compounds.

Chemical Degradation of Polymers and Pyrolysis.

Chemical degradation of polymeric carbohydrates. Chemical degradation of proteins for analytical purposes. Chemical degradation of other macromolecular compounds. Overview of analytical pyrolysis. Pyrolysis as a chemical modification technique. Instrumentation used in analytical pyrolysis. Application of analytical pyrolysis.


Sample preparation is an essential step in many analyses. This book approaches the topic of sample preparation in chromatography in a methodical way, viewing it as a logical connection between sample collection and analytical chromatography. Providing a guide for choosing the appropriate sample preparation for a given analysis, this book describes various ways to process the sample, explaining the principle, discussing the advantages and disadvantages, describing the applicability to different types of samples, and showing the fitness to specific chromatographic determinations.

The first part of the book contains an overview of sample preparation showing its relation to sample collection and to the core chromatographic analysis. The second part covers procedures that do not use chemical modifications of the analyte and includes methods for sample dissolution, concentration and cleanup designed mainly for modifying the initial matrix of the sample. This part starts with conventional separations such as filtration and distillation and finishes with more advanced techniques such as solid phase extraction and electroseparations. The third part gives a description of the chemical modifications that can be performed on a sample either for fractionation purposes or to improve a specific property of the analyte. This part includes derivatizations, polymer chemical degradations, and pyrolysis.


For a wide range of readers, including specialists in analytical chemistry and beginners in this field.


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© Elsevier Science 2002
Elsevier Science
eBook ISBN:
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@from:U.A. Th. Brinkman @qu:Much useful information is provided for a wide range of readers. @source:THE ANALYST

About the Authors

S.C. Moldoveanu Author

Affiliations and Expertise

Brown & Williamson Tobacco Corporation, 2600 Weaver Rd, Macon, GA 31217, USA

V. David Author

Affiliations and Expertise

Department of Analytical Chemistry, University of Bucharest, Sos. Panduri 90, Sect.5, Bucharest, Romania