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饮用水和受污染地下水中万亿分之一水平的N-亚硝基二甲胺的测定。

Determination of N-nitrosodimethylamine at part-per-trillion levels in drinking waters and contaminated groundwaters.

作者信息

Tomkins B A, Griest W H, Higgins C E

机构信息

Organic Chemistry Section, Chemical and Analytical Sciences Division, Oak Ridge National Laboratory, Tennessee 37831-6120, USA.

出版信息

Anal Chem. 1995 Dec 1;67(23):4387-95. doi: 10.1021/ac00119a030.

Abstract

The carcinogen N-nitrosodimethylamine (NDMA) may be quantitated routinely at ultratrace (ng/L) levels in drinking water or contaminated groundwater. The aqueous sample is passed through a preconditioned Empore C18 filter disk to remove neutral nonpolar species and then extracted continuously overnight with highest purity dichloromethane. The latter is then concentrated to 1 mL, and a large aliquot (up to 200 microL) is loaded onto a dual-stage carbon sorbent trap, after which the solvent is removed with ultrapure helium. The concentrated residues are then injected onto a gas chromatographic column using a short-path thermal desorber. NDMA is selectively detected using a chemiluminescent nitrogen detector (CLND) operated in its nitrosamine-selective mode. The reporting limit for this procedure, evaluated using two independent statistically unbiased protocols, is 2 ng of NDMA/L. A related procedure, employing an automatic sampler instead of the short-path thermal desorber, provides convenient analysis of heavily contaminated samples and exhibits a reporting limit (same protocols cited previously) of 110 ng of NDMA/L. When the two methods are used together in a "two-tiered" protocol, NDMA concentrations spanning 4 orders of magnitude (ng/L to microgram/L levels) may be measured routinely. The low-level procedure employing only the short-path thermal desorber was applied successfully to three sources of drinking water, where NDMA concentrations ranged between 2 and 10 ng of NDMA/L. The two-tiered protocol was applied to a series of contaminated groundwaters whose NMDA concentrations ranged between approximately 10-7000 ng of NDMA/L. The results agreed with those obtained from an independent collaborating laboratory, which used a different analytical procedure.

摘要

致癌物质N-亚硝基二甲胺(NDMA)可在饮用水或受污染的地下水中以超痕量(纳克/升)水平进行常规定量。水样通过预处理过的Empore C18滤盘以去除中性非极性物质,然后用最高纯度的二氯甲烷连续萃取过夜。然后将后者浓缩至1毫升,并将大量等分试样(最多200微升)加载到双级碳吸附阱上,之后用超纯氦气去除溶剂。然后使用短路径热解吸器将浓缩的残留物注入气相色谱柱。使用以亚硝胺选择性模式运行的化学发光氮检测器(CLND)选择性检测NDMA。使用两种独立的无统计学偏差方案评估该程序的报告限为2纳克NDMA/升。一种相关程序,采用自动进样器代替短路径热解吸器,可对严重污染的样品进行方便的分析,其报告限(与之前引用的相同方案)为110纳克NDMA/升。当两种方法在“两级”方案中一起使用时,可常规测量跨度为4个数量级(纳克/升至微克/升水平)的NDMA浓度。仅采用短路径热解吸器的低水平程序成功应用于三个饮用水源,其中NDMA浓度在2至10纳克NDMA/升之间。两级方案应用于一系列受污染的地下水,其NMDA浓度在约10 - 7000纳克NDMA/升之间。结果与使用不同分析程序的独立合作实验室获得的结果一致。

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