Mt. Tena et al., SCREENING OF POLYCYCLIC AROMATIC-HYDROCARBONS IN SOIL BY ONLINE FIBER-OPTIC-INTERFACED SUPERCRITICAL-FLUID EXTRACTION SPECTROFLUOROMETRY, Analytical chemistry, 68(14), 1996, pp. 2386-2391
An interface for spectrofluorometric measurements in the supercritical
(SC) CO2 emerging from the extraction cell of a supercritical fluid e
xtractor prior to depressurization was developed. The windowless now c
ell designed for this purpose is furnished with an inlet and outlet fo
r the SC-CO2 stream; it can withstand pressures up to at least 350 bar
and is connected to the light source and detector by means of two fib
er-optic cables. The combined system allows the real-time on-line fluo
rometric monitoring of the supercritical fluid extraction (SFE) proces
s and provides qualitative and semiquantitative information from super
critical extracts of real and spiked samples. The determination of fiv
e polycyclic aromatic hydrocarbons (PAHs) in spiked soil by SFE with o
n-line fluorescence detection provided relative standard deviations le
ss than 5%, as well as benzo[k]fluoranthene recoveries from several sp
iked soils between 93 and 107%, with an RSD less than 10%. Also, cryse
ne-benzo[a]anthracene binary mixtures in spiked soil were resolved wit
h recoveries of 89-103% and an RSD of about 10%. The use of the propos
ed equipment for screening real soil samples for PAHs using on-line SF
E spectrofluorometry is demonstrated.