PRE-SYMPOSIUM SUNDAY SHORT COURSES

Newcomers and those interested in review are invited to participate in pre-symposium short courses preceding the symposium. See Meeting Registration Form to pre-register.

Sunday, August 1, 2004

Fundamentals of Critical Fluids and Their Application; Supercritical Fluid Chromatography – Theory and Application
8:00 AM – 5:00 PM
Instructors: Dr. Jerry King, Los Alamos National Laboratory, Prof. Larry Taylor, Virginia Tech, and Dr. Thomas Chester, Procter & Gamble
Morning session: Designed to provide a knowledge of critical fluid technology and its applications in non-analytical uses, i.e. engineering aspects, and applications in the fields of processing, treatment of materials, and scale-up with respect to plant design and products that can be developed. The initial two hours will be devoted to a discussion of historical context and development of the technology platform, literature and intranet resources, thermodynamic and mass transfer considerations, phase equilibria, solubility of compounds in critical fluid media, useful correlations, etc. The lectures will relate as to how these principles are used in both engineering and analytical application. The final two hours will focus on engineering aspects: how to use super- and sub-critical fluids in conducting extractions, fractionation, reactions and the essential design features. The final section will be devoted to applications in materials science, cleaning with SC-CO₂, food and natural products (nutraceuticals), the use of compressed water for extractions, reactions, and materials modification, as well as particle formation in critical fluid media. Finally, the use of the critical fluid technology platform will be placed in the context of “green” technologies, sustainable development, and combinatorial investigations.

Afternoon session: Chromatographic theory and applications associated with the use of supercritical fluid chromatography and related fluid phases will be presented. This will include an introductory discussion on the use of compressed fluids in chromatography, major developments in the field, and its current status in the context of analytical use. A discussion of the basic relevant chromatographic theory, requisite phase equilibria, and optimization of parameters to achieve the desired separation will be presented. Practical and operational aspects, such as: packed and open tubular columns, choice of fluid phase, design of fluid phase programming with respect to temperature- pressure-time - co solvent use will be covered. Integration of SFC with appropriate detectors or coupled on-line with tandem analytical techniques, such as MS, IR, SFE, will be noted. The relation of high temperature LC, enhanced fluidity, and use of sub-critical fluids (i.e., sub-critical water) in relation to SFC will be cited. Application of the above techniques will heavily emphasize their use in the areas of pharmaceutical, polymer, petroleum, food, and related uses. The use of SFC related to affecting the separation of chiral compounds, oligomers, and thermally-sensitive analytes will receive special attention. Finally, a short discussion on the use of SFC for physicochemical property determination and in preparative use will conclude the course.

Fundamentals of Critical Fluids and Their Application; Analytical Pressurized Fluid Extraction (Pressurized Liquids, SFE and Sub-critical Water Extraction
8:00 AM – 5:00 PM
Instructors: Dr. Jerry King, Los Alamos National Laboratory, Prof. Doug Raynie, South Dakota State University, and Prof. Larry Taylor, Virginia Tech
Morning session: Designed to provide a knowledge of critical fluid technology and its applications in non-analytical uses, i.e. engineering aspects, and applications in the fields of processing, treatment of materials, and scale-up with respect to plant design and products that can be developed. The initial two hours will be devoted to a discussion of historical context and development of the technology platform, literature and intranet resources, thermodynamic and mass transfer considerations, phase equilibria, solubility of compounds in critical fluid media, useful correlations, etc. The lectures will relate as to how these principles are used in both engineering and analytical application. The final two hours will focus on engineering aspects: how to use super- and sub-critical fluids in conducting extractions, fractionation, reactions and the essential design features. The final section will be devoted to applications in materials science, cleaning with SC-CO₂, food and natural products (nutraceuticals), the use of compressed water for extractions, reactions, and materials modification, as well as particle formation in critical fluid media. Finally, the use of the critical fluid technology platform will be placed in the context of “green” technologies, sustainable development, and combinatorial investigations.

Afternoon session: This analytical-orientated course will feature a thorough discussion on the basics and applications of using pressurized fluids for extraction purposes. Including will be the techniques of pressurized liquid extractions (ASE, PSE, sub-critical water), supercritical fluid extraction (SFE); in both the off- and on-line operational modes. Practical aspects such as the addition of extraction enhancers, modifiers (co-solvents), choice of fluid and optimization of extraction conditions will be emphasized. The role of the matrix effect will be noted with respect to the above mentioned experimental parameters and how they affect analyte adsorption, matrix swelling, and ultimately recovery of the analyte. The importance of the analyte trapping technique in terms of the final analytical results will be discussed in detail. A survey of appropriate instrumentation and when pressurized fluid extraction versus SFE should be employed is included in the course. Applications of the above techniques in such areas as polymer science, pharmaceutical industry, to food and agricultural analysis, environmental assays, and derivatization of target analytes will be documented. The course will conclude with an assessment of how these methods and techniques can be use in the context of the field of sample preparation and reducing the use of solvents in a laboratory, and ultimately the environment.