Evaluating bottle liquid-liquid extraction technique for monitoring residual levels of organochlorine pesticides in wastewater treatment-associated matrices

The gold standard for recovering residual organochlorine pesticides from wastewater and aqueous environmental matrices is the continuous liquid-liquid extraction (CLLE) technique that requires methylene chloride (CH₂Cl₂) as solvent at its refluxing temperature. In light of a recent USEPA proposed prohibitions and workplace protections for CH₂Cl₂ (due to its toxicity) and the fact that CLLE requires expensive and hard-to-acquire glassware, an alternative to CLLE as currently practiced is needed. The bottle liquid-liquid extraction (BLLE) technique, demonstrated for extracting semi-volatile organic contaminants from surface water, is potentially a low cost and high throughput alternative for such recovery. BLLE is cheaper and has a smaller laboratory footprint. The technique, performed at ambient temperature in a tightly capped bottle, requires less amount of solvent and contains solvent vapor within the bottle. The latter means less CH₂Cl₂ is encountered in the workplace. In this study, BLLE was performed directly in 1-L amber sampling bottles and shown to recover 21 organochlorine pesticides as efficiently as CLLE from influents and effluents of two wastewater treatment plants Because no statistical differences were found between CLLE (mean = 77.4, SD = 9.28) and BLLE (mean = 79.1, SD = 14.3); t(22) = 0.548, p(same mean) = 0.58, even though CLLE recovered more pesticides than BLLE by 5.18 ± 8.15%, these techniques are amenable to interchangeable usage. The systematic bias so far detected fits the expression BLLE = 1.4[CLLE] – 35 (r = 0.88). Both CLLE and BLLE recoveries were consistently higher for 4,4′-DDD and lower for aldrin, heptachlor and endrin aldehyde. Diethyl ether addition, as some suggested, did not improve BLLE.

Synopsis: There is need to find a cheap, reliable and high throughput technique for purifying SVOCs from aqueous environmental media efficiently. BLLE, a little known technique, fulfils this need.