Fm. Guo et al., Na(4)EDTA-assisted sub-/supercritical fluid extraction procedure for quantitative recovery of polar analytes in soil, ANALYT CHEM, 71(7), 1999, pp. 1309-1315
Supercritical carbon dioxide (SC-CO2) is effective in extracting nonpolar a
nd slightly polar chemicals from soils. However, pure SC-CO2 is unsatisfact
ory for recovering polar chemicals in soils. A simple supercritical fluid e
xtraction (SFE) procedure was developed to quantitatively recover polar and
nonpolar chemicals from soils. The polar chemicals tested were aromatic ac
ids and phenols. The nonpolar and slightly polar chemicals used as model co
mpounds were common pesticides and environmental pollutants such as polycyc
lic aromatic hydrocarbons. The procedure required pretreatment of the sampl
es with 15% water (g/g), 5% (ethylenedinitrilo)tetraacetic acid tetrasodium
salt (Na(4)EDTA) (g/g), and 50% methanol (mL/g) prior to extractions using
SC-CO2 at 60 degrees C and 34.5 MPa. Recoveries ranged from 90 to 106% for
the aromatic acids using the Na(4)EDTA-assisted SFE compared with only 7-6
3% recoveries of the corresponding chemicals when no Na(4)EDTA was used. Th
e method quantitatively extracted 2,4-D and its close analogues aged in the
soil for 2-30 days. The Na(4)EDTA-assisted SFE was also adequate for extra
cting phenolic analytes including picric acid and pentachlorophenol with re
coveries from 85 to 104%. Na(4)EDTA is a good enhancer for extraction of th
e 29 analytes representing a wide range of polarity from the soil using SC-
COB. The method is valuable for the analysis of parent pollutants and trans
formed products, particularly oxygen-borne metabolites in the environment.