Hb. Lee et al., SUPERCRITICAL CARBON-DIOXIDE EXTRACTION OF POLYCYCLIC AROMATIC-HYDROCARBONS FROM SEDIMENTS, Journal of chromatography, 653(1), 1993, pp. 83-91
A supercritical fluid extraction (SFE) method using carbon dioxide was
developed for the determination of the 16 US Environmental Protection
Agency polycyclic aromatic hydrocarbon (PAH) priority pollutants in n
aturally contaminated sediments. While carbon dioxide is less efficien
t for the heavier PAHs than other fluids such as nitrous oxide and Fre
on-22, its deficiency was remedied by the use of a mixture of water, m
ethanol, and dichloromethane as modifiers, a higher extraction tempera
ture of 120 degrees C, as well as repetitive extractions. Extraction t
ime can be further reduced to ca. 70 min per sample if a high-pressure
pump is used for the delivery of the modifiers during dynamic extract
ion. Except for naphthalene, the SFE results for the 16 PAHs obtained
from several certified reference materials and sediments samples were
comparable to certified or Soxhlet values in terms of both precision a
nd accuracy. The SFE recoveries of naphthalene as well as methylnaphth
alenes which were coextracted alongside other PAHs and methyl-PAHs, ra
nged from 150 to 125% of their respective Soxhlet values due to higher
evaporative losses in the Soxhlet procedure.