Determinations of N-nitrosodimethylamine at part-per-trillion concentrations in contaminated groundwaters and drinking waters featuring carbon-based membrane extraction disks

被引:40
作者
Tomkins, BA
Griest, WH
机构
关键词
D O I
10.1021/ac9601573
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A new solid-phase extraction procedure extracts N-nitrosodimethylamine (NDMA) at part-per-trillion (ng/L) concentrations from aqueous samples using a C-18 (reversed-phase) membrane extraction disk layered over a recently introduced carbon-based extraction disk, The reversed-phase disk removes nonpolar water-insoluble neutrals and is set aside; the carbon-based disk is extracted with a small volume of dichloromethane. NDMA is quantified in the organic extract using a gas chromatograph equipped with both a short-path thermal desorber and a chemiluminescent nitrogen detector, The detection limit for the procedure, calculated using two statistically unbiased protocols, is 3 ng of NDMA/L; the analyte recovery is similar to 57%. A related procedure substitutes a standard automatic sampler for the short-path thermal desorber and is suitable for determining NDMA in heavily contaminated (> 300 ng of NDMA/L) aqueous samples, The detection limit for the procedure, calculated in the same manner as above, is 300 ng of NDMA/L, with an analyte recovery of similar to 64%. The detection limits and measured recovery values are comparable to those observed in earlier work, in which a conventional continuous overnight extraction with dichloromethane was used to remove NDMA from the aqueous samples. The newer procedures described herein offer a 50-fold savings in extraction time and a 100-fold reduction in dichloromethane consumed per sample while maintaining the wide range (3-4 orders of magnitude concentrations of NDMA) observed for the original procedures used in tandem, Authentic contaminated groundwaters are extracted using both the conventional and disk-based extraction procedures and analyzed; the observed NDMA concentrations are virtually identical over a target range spanning 100-10000 ng of NDMA/L.
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页码:2533 / 2540
页数:8
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