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  • Determination of Organotin Compounds in Water,Sediments, and Sewage Sludge UsingPerdeuterated Internal Standards, AcceleratedSolvent Extraction, and Large-Volume-InjectionGC/MS
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  • Two new methods for the simultaneous identification andquantification of organotin compounds (OTs) includingmonobutyltin, dibutyltin, tributyltin, monophenyltin,diphenyltin, triphenyltin, and tricyclohexyltin (TCyT) innatural waters and sediments, respectively, are presented.For water samples, aqueous ethylation followed byliquid−liquid extraction (LLE) or solid-phase extraction and large-volume-injection GC/MS (50−200 μL) were used. Forsediment samples, accelerated solvent extraction at 100°C with a methanolic mixture of sodium acetate andaceticacid was developed. By using for the first timeperdeuterated OTs as internal standards, excellent precision(relative standard deviations <5%) and low method detection limits ranging from 0.3 to 1.5 ng/L for 50 mL ofaqueous samples and from 0.4 to 2 ng/g for 2.5 g of driedsediments were achieved. Using LLE, recoveries determined in spiked harbor water (+5 ng/L) and sedimentpore water (+25 ng/L) were in the range of 93−103 (RSD0.5−4.6%) and 97−108% (RSD 0.8−4.2%),respectively.For spiked sediment samples (+10 ng/g) recoveriesof98−105% (RSD 1−7%) were achieved for all OTs, exceptfor TCyT (51%, RSD 4%). The developed analyticalprocedures were validated with reference material andapplied to various environmental samples, such as fresh-and seawater, field runoff, wastewater, sediments, andsewage sludge.
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