Sample preparation and application

The condition necessary for a successful GPC separation is the total solubility of the sample in the mobile phase at the temperature of experiment. If this condition is fulfilled, the sample can also be dissolved and applied into the column in the liquid different from the mobile phase, provided both solvents are fully miscible. Prior to application the sample solution must often be cleaned by filtration or centrifugation. 

During filtration, the layer of very small, insoluble particles can also act as an ultrafilter trapping the largest macromolecules. In this case, either using filters with larger pores and larger surface areas, or centrifugation of samples, is recommended. 

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Kingston, H. M. Haswell, S. J., eds. Microwave-Enhanced Chemistry Fundamentals, Sample Preparation, and Applications. American Ghemical Society Washington, DG, 1997. 

H.M. Kingston and S.J. Haswell (eds) Microwave-enhanced Chemistry. Fundamentals, Sample Preparation and Applications, American Chemical Society, Washington, DC (1997). 

Quantification of known analytes in PK and distribution studies makes different demands on the analytical procedure than detection of unknown compounds in biotransformation experiments or identification of unknown and postulated molecules in toxicological screening. For example, requirements for quantitative analysis of fixed analytes with optimum sensitivity and selectivity differ from those for qualitative detection of intact molecular weight or diagnostic MS/MS fragments. Selectivity of sample preparation and applicability of diverse scan modes represent relevant critical issues. The following sections address this context. 

Kingston HM, Haswell SJ (eds) (1997) Microwave-enhanced chemistry, fundamentals, sample preparation and applications. American Chemical Society, Washington... 

Mermet, J.M. Focused-microwave-assisted reactions atmospheric-pressure acid digestion, on-line pretreatment and acid digestion, volatile species production, and extraction. In Kingston, H.M., Haswell, S.J. (eds.) Microwave-Enhanced Chemistry. Fundamentals, Sample Preparation, and Applications. ACS, Washington, DC (1997)... 

For more detailed di.scussions of microwave sample preparation and commercial instrumentation, see H. M. Kingston and S. J. Haswell, Microwaye-Eninmced Chemistry Fundamentals, Sample Preparation and Applications. Washington, DC American Chemical Society, 1997 B. E. Erickson. Ano/. Chem., 1998, 70. 467A-471A R. C. Richter, D. Link, and H. M. King.ston, Ann/. Chem., 2001, 73. 31A-37A. 

Knapp. G, Panholzee F, Schalk A and Kettisch P (1997) Pressure-controlled microwave-assisted wet digestion. In Kingston HM and Haswell SJ, eds. (1997) Microwave-Enhanced Chemistry, Eunda-mentals, Sample Preparation, and Applications, pp. 423-451. American Chemical Society, Washington, DC. 

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