An evaluation and comparison of micro-techniques for concentration of volatile components from dilute solutions

Summary

Several micro-techniques for the removal of solvent from dilute solutions of volatile compounds have been compared. Large solute losses were experienced when the conventional blow-down technique was applied. Better yields could be obtained with static evaporation procedures, as long as an effective reflux was maintained. However, careful optimization of the vessel design and operating conditions is necessary. The most efficient volume reduction technique was shown to be chromatographic evaporation. Quantitative recoveries were obtained for the compounds tested and the process was significantly faster than static concentration. Moreover, operating conditions (gas flow, temperature) are less critical. With modifications, the principle can be used for the concentration of large sample volumes down to a few microliters.