H. Degeus et al., DETERMINATION OF TRIALKYL AND TRIARYL PHOSPHATES IN SEDIMENT USING MICROWAVE EXTRACTION AND PACKED-CAPILLARY SUPERCRITICAL-FLUID CHROMATOGRAPHY, International journal of environmental analytical chemistry, 56(2), 1994, pp. 119-132
Trialkyl and triaryl phosphates (TAPs) are widely used as flame retard
ants in plasticizers and hydraulic fluids. A microwave extraction meth
od used to isolate these compounds from harbour sediment was developed
and compared with traditional Soxhlet and shake-flask techniques. Mic
rowave extraction proved to be 15 times faster than the traditional me
thods and resulted in higher recoveries for non-polar TAPs. Another ad
vantage of the method is a significant saving in organic extraction so
lvents and energy. For the analysis of microwave extracts, packed-capi
llary supercritical fluid chromatography (PC-SFC) coupled with thermio
nic detection was used. It is shown that by using density programming
faster analyses and lower limits of detection, can be obtained than wi
th isoconfertic SFC. Detection limits of TAPs in sediment extracts wer
e 0.10-0.20 mg/kg. The method showed good reproducibility and linearit
y over three orders of magnitude.