Determination of DDT and its metabolites in cattle dip soil available in aqueous phase after remediation.

Soil taken from a former cattle tick dip site in NSW Australia, was remediated with a chemical leaching technology. The pre- and post-remediated soil (20g) was dispersed in water (100mL) and subjected to passive diffusion using polymeric membranes. The remediation reduced tDDT from 1174.3 microg/g to 102.9 microg/g (ash weight basis), which was further reduced to 43.2 microg/g with composting. The membranes accumulated 41.3 microg tDDT/g from the dip soil, 49.2 microg tDDT/g from the chemically leached soil and 3.1 microg tDDT/g from the leached composted soil. The chemical leaching removed over 90% of the tDDT, but released soil bound DDT, which was converted to DDE, while 2.99 microg/g was accumulated by the membranes from dip soil, 37.52 microg/g was accumulated from remediated soil. Composting, however, almost eliminated the availability for passive diffusion by the membranes from 50-60 microg/g in remediated soil to 3 -3.5 microg/g in composted soil. Variability studies of the membranes using eight replicates demonstrated that the accumulation by the membranes was reproducible with an average relative error of 20.3% for p,p'-DDT in soil type two, whilst the lowest average relative error for p,p'-DDE was 4.3%, suggesting that triplicate analyses will achieve acceptable accuracy.

Cleanup of biological extracts by a Pasteur pipette column and a comparison of in vivo-accumulated chlorinated pesticide residues with other clean up systems.

Biological samples are extracted with n-hexane/acetone (60:40) and 1 mL of the concentrated extract is eluted through a pasteur pipette column prepacked with alumina (0.3 g) and silicic acid (0.25 g) with 10 mL n-hexane (containing 4% acetone). The fat and other co-extractives are retained by the column and clear eluate is directly injected on a GLC column for determination on electron capture detector. A comparison of the Pasteur pipette cleanup with the modified method of Cole et al. (1967) on 41 samples of fish, One Step Method, (Ahmad and Marolt (1986] on 86 samples of fish and Maunder et al. (1964) on 10 type of wildlife (100 samples) was made. The Pasteur pipette method gives results which are significantly higher (p greater than 0.5) than the other methods except the One step method. The Pasteur pipette method has a detection limit of 0.01 microgram/g for DDT and its metabolites.

One-step extraction and cleanup procedure for determination of p,p'-DDT, p,p'-DDD, and p,p'-DDE in fish.

A simplified method that combines extraction, partitioning, and cleanup in a single step for measuring p,p'-DDT and its metabolites in fish is described. Minced fish samples are emulsified with disodium hydrogen orthophosphate and trisodium citrate, ground with sodium sulfate, and eluted from a chromatographic column prepacked with alumina and silicic acid. The fats and fatty acids are solubilized and easily extracted from the tissues and retained by the column, while p,p'-DDT and its metabolites are quantitatively eluted with 40 mL n-hexane. The eluate is directly applied to a gas chromatographic column. Average recoveries of p,p'-DDT and its metabolites added to fish in vitro are 81%. The average coefficient of variation for recoveries of p,p'-DDT and its metabolites is less than 6.5% and the detection limit is 0.001 micrograms/g for p,p'-DDE, thus making this method very suitable for residue analysis.