C. Rivasseau et M. Caude, COMPARISON OF ONLINE SPE-HPLC AND SPME-GC FOR THE ANALYSIS OF MICROCONTAMINANTS IN WATER, Chromatographia, 41(7-8), 1995, pp. 462-470
Citations number
26
Categorie Soggetti
Chemistry Analytical","Biochemical Research Methods
Solid-phase preconcentration coupled on-line with liquid chromatograph
y, and solid-phase microextraction coupled with gas chromatography hav
e been applied to the determination of trace-level concentrations of b
enzene and sulfur compounds (tetrahydrothiophene (THT), t-butyl mercap
tan (TBM), and n-butyl mercaptan (nBM)) in aqueous media. The first te
chnique uses a microcolumn packed with a styrene-divinylbenzene copoly
mer. Retention values for THT, TBM, and benzene on this sorbent, expre
ssed as the capacity factors, are 1100, 1600, and 4000, respectively.
It is, therefore, possible to preconcentrate them efficiently and this
method enables minimum concentrations of 0.05, 0.7, and 0.8 mu g L(-1
), respectively, to be reached. In microextraction, a fine silica fibe
r coated with a thin layer of polydimethylsiloxane is used. The partit
ion coefficients of the analytes between the polymeric coating and wat
er have been determined to be 40, 115, and 110 for THT, TBM, and benze
ne, respectively. When sampling is performed from the liquid phase, pa
rtition equilibrium is reached within 5 to 20 minutes, or more quickly
when the solution is agitated. Using a flame ionization detector, det
ection limits for THT, TBM, and benzene were 3, 5, and 0.2 mu g L(-1),
respectively. Extraction of volatile or semi-volatile analytes can al
so be performed from the headspace with very similar detection limits.
In addition, the extraction time is shorter since equilibrium is reac
hed within 1 to 1.5 minute, which can again be reduced by agitation of
the sample. The advantages and drawbacks of both techniques are gathe
red and discussed in this paper, which also underlines their complemen
tarity.