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首页> 外文期刊>Analytical Sciences >Gas Chromatography/Mass Spectrometric Determination of Traces of Hydrophilic and Volatile Organic Compounds in Water after Preconcentration with Activated Carbon
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Gas Chromatography/Mass Spectrometric Determination of Traces of Hydrophilic and Volatile Organic Compounds in Water after Preconcentration with Activated Carbon

机译:活性炭富集-气相色谱/质谱法测定水中痕量亲水性和挥发性有机物。

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摘要

The authors have developed an analytical method for extracting trace amounts of 15 hydrophilic compounds in water using gas chromatography/mass spectrometry coupled with an activated carbon preconcentration procedure. As internal standards, perdeuterated p-dioxane and N, N-dimethylformamide were added to 11 of a water sample; the water was passed through a granular activated carbon column. Organic substances adsorbed on the activated carbon were eluted with acetone and dichloromethane; the extract was then concentrated to 10ml with a Kuderna-Danish concentrator. Quantitative analyses using GC/MS with a selected ion monitor (GC/MS-SIM) were performed to measure the recovery efficiencies of the 15 compounds spiked into water samples at concentrations of 0.2 and 2.0μg/l. The recovery efficiencies through the internal standard method of the compounds, except alcohols and acetonitrile, gave more than 90% and their relative standard deviations were less than 7% at a concentration of 0.2μg/l. In this study, it was confirmed that the activated carbon preconcentration procedure is useful for extracting trace amounts of polar compounds which have a log P value (dichloromethane-water partition coefficient) greater than -0.5, except for compounds containing a hydroxy group or having a very small molecular weight. The method was applied to the analysis of river water and seawater for polar compounds. p-Dioxane, 1-propanol, N-nitrosodimethylamine, N-nitrosodiethylamine, N, N-dimethylformamide and N, N-dimethylacetamide were detected below the μg/l level.
机译:作者已经开发出一种分析方法,可以使用气相色谱/质谱联用活性炭预浓缩程序,从水中提取痕量的15种亲水性化合物。作为内标,将氘化的对二恶烷和N,N-二甲基甲酰胺添加到11个水样品中;使水通过粒状活性炭柱。吸附在活性炭上的有机物质用丙酮和二氯甲烷洗脱;然后用Kuderna-Danish浓缩器将提取液浓缩至10ml。使用GC / MS和选定的离子监测器(GC / MS-SIM)进行了定量分析,以测量加标到水样品中浓度为0.2和2.0μg/ l的15种化合物的回收效率。通过内标方法回收的化合物,除醇和乙腈外,在0.2μg/ l的浓度下回收率均超过90%,相对标准偏差小于7%。在这项研究中,已证实,活性炭预浓缩程序可用于萃取痕量极性对数化合物,其对数P值(二氯甲烷-水分配系数)大于-0.5,但含有羟基或具有分子量很小。该方法用于河流水和海水中极性化合物的分析。对二恶烷,1-丙醇,N-亚硝基二甲胺,N-亚硝基二乙胺,N,N-二甲基甲酰胺和N,N-二甲基乙酰胺的含量低于μg/ l。

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