Improved solvent trapping of volatiles in supercritical fluid extraction by pressurizing the collection vial

The high flour rates that result after decompression make the trapping of a nalytes one of the more difficult aspects of a supercritical extraction. By elevation of the pressure on the collection vial, the now may be reduced a nd trapping efficiency improved, considerably. The effects of different col lection vial pressures were evaluated. The best results were obtained at 25 atm, With the collection vial at 25 atm, the trapping efficiencies of diff erent solvents were then investigated. Also considered were the effects of solvent volume, extraction now rate, collection solvent geometry, and restr ictor temperature, For a 30 min exraction-with the restrictor line at 200 d egrees C-quantitative recoveries were obtained with analytes as volatile as chlorobenzene (similar to 90%) in 1 mL of solvent. Mild precooling of the collection vessel allowed quantitative recoveries to be obtained down to be nzene (94.2%).