Investigation of the supercritical fluid extraction and detection of metals in contaminated soils
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Experiments involving the on-line extraction and detection of ferrocene spiked sea sand were very promising, in that unity of extraction and detection was achieved with this nonpolar compound. Percent recovery was greatly reduced when the on-line extraction of Iron III Trifluoroacetylacetonate (FeTFA) was attempted. Off-line extraction studies were performed to establish the optimum conditions necessary to effect the SFE of the following Iron III complexes: Iron III Acetylacetonate (FeAcac) and Iron III Trifluoroacetylacetonate. The greatest recovery (55.85 0/0) was achieved with Supercritical Fluid-C02 under the following conditions: 60Â°C, 150 atm, 20 minute static extraction followed by 20 minute dynamic extraction. The extraction vessel contained 0.250 mg iron complex, 20 Î¼L HPLC grade methanol, and 20 Î¼L deionized water. Trapping of the analyte was achieved by decompressing the SF-C02 and analyte in 10 mL of HPLC grade methanol held at OÂ°C.
- Doctoral Dissertations