DETERMINATION OF TRIALKYL AND TRIARYL PHOSPHATES IN SEDIMENT USING MICROWAVE EXTRACTION AND PACKED-CAPILLARY SUPERCRITICAL-FLUID CHROMATOGRAPHY

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.