by Professor D. E. Games, Mass Spectrometry Research Unit, University College of Swansea Sample preparation can be viewed as occupying a Cinderella role in analytical science. However, the quality of sample preparation plays a key role in high In the past decade, there has been quality analysis and deserves higher stature. considerable interest in the use of supercritical fluid extraction (SFE) as an alternative to conventional procedures for the preparation of samples for ana lysis. The driving force for this development is the need for automated, sim pler, faster, non-destructive and selective methods for extraction, preferably using non-toxic extraction media which are easily disposed of. Utilization of supercritical fluids for extraction fulfils these requirements because of their unique physical chemical properties and usually low toxicity. Selectivity can be achieved by suitable selection of pressure (density), temperature and modi fier conditions which enable solvating power to be varied. The high diffusivity of supercritical fluids provides rapid sample penetration and extraction. Use of fluids with low critical temperatures enables extraction to be conducted under mild thermal conditions ensuring that thermally labile compounds do not decompose. The technique can be used off-line, and the extracts analysed by appropriate techniques, or it can be used on-line, by coupling with a variety of chromatographic techniques. These can then, if necessary, be coupled fur ther with spectroscopic techniques, such as Fourier transform infrared, ultra violet or mass spectrometry, to provide specific identification or structural information.

During the past decade supercritical fluid extration (SFE) has attracted considerable attention as a sample preparation procedure in analytical chemistry. The successful implementation of this technique can lead to improved sample throughput, more efficient recovery of analytes, cleaner extracts, economic replacement of halogenated solvents and a high level of automation, compared to conventional sample preparation procedures. This book provides an overview of basic principles of SFE as well as in-depth reviews of both on- and off-line SFE methods. The on-line coupling of SFE with both chromatographic and spectroscopics techniques has been the subject of a great deal of research effort and is dealt with in detail. Newer developments, such as off-line SFE of solid and liquid matrices, are starting to attract a great deal of interest, and the coverage of these areas will prove of particular value to the analytical chemist. The international team of authors has illustrated these topics with many `state-of-the-art' applications, and each chapter provides a comprehensive list of references. For the convenience of the reader, an appendix which contains pressure conversion scales and supercritical fluid carbon dioxide density tables appears at the end of the book. The volume's extensive coverage of both on-line and off-line extraction will be particularly useful to analytical chemists, in a wide range of environments, seeking to develop high quality, simple and robust SFE methods.

The continued search for rapid, efficient and cost-effective means of analytical measurement has introduced supercritical fluids into the field of analytical chemistry. Two areas are common: supercritical fluid chroma tography and supercritical fluid extraction. Both seek to exploit the unique properties of a gas at temperatures and pressures above the critical point. The most common supercritical fluid is carbon dioxide, employed because of its low critical temperature (31 °C), inertness, purity, non-toxicity and cheapness. Alternative supercritical fluids are also used and often in conjunction with modifiers. The combined gas-like mass transfer and liquid-like solvating characteristics have been used for improved chroma tographic separation and faster sample preparation. Supercritical fluid chromatography (SFC) is complementary to gas chro matography ( GC) and high performance liquid chromatography (HPLC), providing higher efficiency than HPLC, together with the ability to analyse thermally labile and high molecular weight analytes. Both packed and open tubular columns can be employed, providing the capability to analyse a wide range of sample types. In addition, flame ionization detection can be used, thus providing 'universal' detection.

Comprehensive Sampling and Sample Preparation is a complete treatment of the theory and methodology of sampling in all physical phases and the theory of sample preparation for all major extraction techniques. It is the perfect starting point for researchers and students to design and implement their experiments and support those experiments with quality-reviewed background information. In its four volumes, fundamentals of sampling and sample preparation are reinforced through broad and detailed sections dealing with Biological and Medical, Environmental and Forensic, and Food and Beverage applications. The contributions are organized to reflect the way in which analytical chemists approach a problem. It is intended for a broad audience of analytical chemists, both educators and practitioners of the art and can assist in the preparation of courses as well in the selection of sampling and sample preparation techniques to address the challenges at hand. Above all, it is designed to be helpful in learning more about these topics, as well as to encourage an interest in sampling and sample preparation by outlining the present practice of the technology and by indicating research opportunities. Sampling and Sample preparation is a large and well-defined field in Analytical Chemistry, relevant for many application areas such as medicine, environmental science, biochemistry, pharmacology, geology, and food science. This work covers all these aspects and will be extremely useful to researchers and students, who can use it as a starting point to design and implement their experiments and for quality-reviewed background information There are limited resources that Educators can use to effectively teach the fundamental aspects of modern sample preparation technology. Comprehensive Sampling and Sample Preparation addresses this need, but focuses on the common principles of new developments in extraction technologies rather than the differences between techniques thus facilitating a more thorough understanding Provides a complete overview of the field. Not only will help to save time, it will also help to make correct assessments and avoid costly mistakes in sampling in the process Sample and sample preparation are integral parts of the analytical process but are often less considered and sometimes even completely disregarded in the available literature. To fill this gap, leading scientists have contributed 130 chapters, organized in 4 volumes, covering all modern aspects of sampling and liquid, solid phase and membrane extractions, as well as the challenges associated with different types of matrices in relevant application areas

Here, authors specializing in different branches of chromatography--including gas chromatography, supercritical fluid chromatography, and high-pressure liquid chromatography--describe their fields while drawing out connections with other branches.

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.

Recent advances in analytical chemistry have turned it into a virtually unrecognizable science compared to a few decades ago, when it lagged behind other sciences and techniques. However, advances in analytical science have been far from universal: while innovations in instrumentation and data acquisition and processing systems have reached unprecedented levels thanks to parallel breakthroughs in computer science and chemo metrics, progress in preliminary operations has been much slower despite their importance to analytical results. Thus, such clear trends in analytical process development as automation and miniaturization have not reached preliminary operations to the same extent, even though this area is pro bably in the greatest need. Improvement in preliminary operations is thus an urgent goal of analytical chemistry on the verge of the twenty first century. Increased R&D endeavours and manufacture of commercially available automatic equipment for implementation of the wide variety of operations that separate the uncollected, unmeasured, untreated sample from the signal measuring step are thus crucial on account of the wide variability of such operations, which precludes development of all-purpose equipment, and the complexity of some, particularly relating to solid samples. Supercritical fluid extraction opens up interesting prospects in this context and is no doubt an effective approach to automatioI1 and mini aturization in the preliminary steps of the analytical process. The dramatic developments achieved in its short life are atypical in many respects.

Packed Column SFC is the third title to be published in this series and has been produced as a result of the dramatic re-emergence, in the last three years, of packed column instrumentation. This has led to a redefinition of the technique and an urgent need for a practical guide that deals with its subtleties. This book fulfils that need and deals exclusively with packed column SFC. It places the emphasis on understanding the underlying chemistry in order to perform rapid, systematic optimizations and provides many practical tips to help the new user avoid problems unique to SFC. It also proposes a detailed scheme for method development and provides lists of prioritized guidelines. The book clears up some of the confusion that surrounds the analytical use of supercritical fluids and assists the user in understanding the power and utility of this technique. Detailed chapters cover the most promising new application areas for packed column SFC, which are often overlooked in the mainstream chromatography literature. Like the other books in this popular series, Packed Column SFC will prove an invaluable guide and is essential reading for graduates, postgraduates and researchers with interests in pharmaceuticals, agricultural chemistry, small polar drug molecules, chiral analysis, environmental chemistry, and chromatography/instrumentation.

The Application of Green Solvents in Separation Processes features a logical progression of a wide range of topics and methods, beginning with an overview of green solvents, covering everything from water and organic solvents, to ionic liquids, switchable solvents, eutectic mixtures, supercritical fluids, gas-expanded solvents, and more. In addition, the book outlines green extraction techniques, such as green membrane extraction, ultrasound-assisted extraction, and surfactant-mediated extraction techniques. Green sampling and sample preparation techniques are then explored, followed by green analytical separations, including green gas and liquid capillary chromatography, counter current chromatography, supercritical fluid chromatography, capillary electrophoresis, and other electrical separations. Applications of green chemistry techniques that are relevant for a broad range of scientific and technological areas are covered, including the benefits and challenges associated with their application. - Provides insights into recent advances in greener extraction and separation processes - Gives an understanding of alternatives to harmful solvents commonly used in extraction and separation processes, as well as advanced techniques for such processes - Written by a multidisciplinary group of internationally recognized scientists

The importance of accurate sample preparation techniques cannot be overstated--meticulous sample preparation is essential. Often overlooked, it is the midway point where the analytes from the sample matrix are transformed so they are suitable for analysis. Even the best analytical techniques cannot rectify problems generated by sloppy sample pretreatment. Devoted entirely to teaching and reinforcing these necessary pretreatment steps, Sample Preparation Techniques in Analytical Chemistry addresses diverse aspects of this important measurement step. These include: * State-of-the-art extraction techniques for organic and inorganic analytes * Sample preparation in biological measurements * Sample pretreatment in microscopy * Surface enhancement as a sample preparation tool in Raman and IR spectroscopy * Sample concentration and clean-up methods * Quality control steps Designed to serve as a text in an undergraduate or graduate level curriculum, Sample Preparation Techniques in Analytical Chemistry also provides an invaluable reference tool for analytical chemists in the chemical, biological, pharmaceutical, environmental, and materials sciences.