Determination of dissolved kepone by direct addition of XAD-2 resin to water

Abstract

buta [c,d]pentalen-2-one), a chlorinated hydrocarbon pesticide, was manufactured at Hopewell, Va., from 1966-1975. Waste discharges contaminated the adjacent James River from Richmond to the Chesapeake Bay, producing adverse environmental and economic impacts (1-3).Extraction techniques have been developed for the determination of Kepone in water, using benzene (1, 4), tolueneethyl acetate (2), or ethyl ether-hexane (5) as solvents, with detection limits ranging from 20-40 ng/L (1, 2, 4, 5). However, because of insensitivity of these existing methods, concentration differences of a few parts-per-trillion (ng/L) dissolved Kepone may go undetected. Therefore, an analytical procedure was needed to quantify Kepone in water at concentrations of <20 ng/L.In addition to solvent extraction, techniques for removing organics from water have involved the use of columns packed with porous XAD polymer resins (6-10). Columns of

Kepone in the James River

“…The experimental design involved collecting contaminated animals from the James and placing them in Kepone-free water of various temperatures in the laboratory. Subsequent sampling and analyses showed that with summer temperatures, oysters need about two weeks to purge themselves; with winter temperatures, seven weeks (Huggett et al, 1980). The experimental conclusions were validated by analyzing oysters from the James which had been transplanted into other rivers for varying periods of time.…”

“…By applying the factor of 0.004 to the most sensitive species tested in the James, we predicted maximum acceptable concentrations for dissolved Kepone of 0.14 Mg/L in the freshwater zone and 0.026 µg/L in the lower estuary. No measurements of dissolved Kepone have been made in the lower estuary, but levels of 3-10 ng/L were observed in the middle estuary (Harris et al, 1980). Kepone levels as high as 45 ng/L were reported in the upper freshwater zone (Saleh et al, 1978 and EPA, 1978a).…”

“…Kepone concentrations in zooplankton sometimes reach levels of 16 µg/g (dry weight), while phytoplankton range from nondetectable to 2.1 µg/g. Huggett et al (1980) have shown that Kepone is associated mainly with the organic portion of bottom sediments and that the inorganic mineral grains are relatively clean. Therefore, a change in the ratio of inorganic to organic particles has the potential to change Kepone concentrations; this occurs with suspended sediments whenever the tides change because the mineral grains are more dense than the organic particles and therefore settle more rapidly.…”

Analysis of chlordecone by LC/MS–MS in surface and wastewaters

“…Numerous studies, dedicated to the CLD determination in various matrixes has been conducted since 1960. Electron capture gas chromatography (GC-ECD) has become a technique of choice for the determination of CLD in water [4] and [5], soil and sediments [5], [6] and [7] food [8] and biological tissues [9] and [10]. More recently gas chromatography equipped with mass spectrometry has also been employed for CLD determination (GC-MS).…”

Solid-phase microextraction and gas chromatography-mass spectrometry for quantitative determination of chlordecone in water, plant and soil samples

“…Few attempts have been made to simplify the chlordecone extraction and analysis protocol. XAD-2 resin was tested on river water but required 20-L samples, filtration and finally, extraction by solvent [23]. Near-Infrared Spectroscopy (NIRS) has been tentatively used for solid soil samples [24], allowing fast and cheap determination of chlordecone contamination in soil.…”