Comparison of supercritical fluid extraction and Soxhlet extraction for the determination of polychlorinated biphenyls in environmental matrix standard reference materials

1998 ◽  
Vol 816 (2) ◽  
pp. 213-220 ◽  
Author(s):  
Michele M Schantz ◽  
Søren Bøwadt ◽  
Bruce A Benner ◽  
Stephen A Wise ◽  
Steven B Hawthorne
1996 ◽  
Vol 79 (1) ◽  
pp. 142-156 ◽  
Author(s):  
Viorica Lopez-A Vila ◽  
Richard Young ◽  
Nataly Teplitsky

Abstract Microwave-assisted extraction (MAE), Soxhlet, soni cation, and supercritical fluid extraction (SFE) were compared in their ability to extract 95 compounds listed in U.S. Environmental Protection Agency Method 8250. Freshly spiked soil samples and 2 standard reference materials were extracted with hexane-acetone (1 + 1) by MAE and Soxhlet extraction, with methylene chloride-acetone (1 + 1) by sonication extraction, and with supercritical carbondioxide modified with 10% methanol by SFE. Results indicate that MAE is a promising extraction technique. Of 94 compounds for which we are reporting data, 51 compounds gave MAE recoveries of >80%; 33,50-79%; 8,20-49%; and 2, <19%. Soxhlet extraction gave very similar results: 50 recoveries were >80%; 32,50-79%; 8,20-49%; and 4, <19%. Sonica tion recoveries were slightly higher: 63 values were >80%; 25,50-79%; 4,20-49%; and 2, <19%. SFE recoveries were the lowest: 37 values were >80%; 37, 50-79%; 12,20-49%, and 8, <19%. MAE gave the best precision: relative standard deviations (RSDs) were <10% for 90 of 94 compounds. Soxhlet extraction gave the worst precision: only 52 of 94 samples gave RSDs ≤10%. Although MAE looks promising, 15 polar basic compounds extracted at 115°C with hexane acetone for 10 min (1000 W power) gave poor recoveries. Because no technique gave acceptable recoveries for these polar compounds, we investigated their extraction with MAE using acetonitrile at 50° and 115°C. Ten of the 15 compounds were quantitatively recovered (>70%) with acetonitrile at 115°C.


1995 ◽  
Vol 78 (4) ◽  
pp. 1124-1125 ◽  
Author(s):  
Walter Holak

Abstract A method, using supercritical fluid extraction, for determining methylmercury in seafood has been developed to eliminate use of toxic organic solvents. Seafood samples were treated with 1N NaOH and then acidified with HCI to release CH3HgCI. After mixing the sample with cellulose powder (40 mesh) containing stearic acid modifier at 5 mg/g, the extraction was performed with supercritical CO2 under the following conditions: pressure, 200 atm; temperature, 50°C; time, 20 min; and trap, 0.01N Na2S2O3 in a conical tube immersed in a flask of warm water to prevent freezing. The extract was then analyzed by a suitable method, such as cold-vapor atomic absorption spectrophotometry. The accuracy of the procedure was verified by analyzing biological standard reference materials. Several commercial seafood samples and spikes have been analyzed.


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