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铋(III)4-甲基哌啶二硫代氨基甲酸盐共沉淀法用于水样中痕量金属离子的分离与预富集——火焰原子吸收光谱法测定

Bi(III)4-methylpiperidinedithiocarbamate coprecipitation procedure for separation--pre-concentration of trace metal ions in water samples by flame atomic absorption spectrometric determination.

作者信息

Efendioğlu Ayşegül, Yağan Mehtap, Bati Bekir

机构信息

Ondokuz Mayis University, Faculty of Art and Science, Department of Chemistry, 55139 Samsun, Turkey.

出版信息

J Hazard Mater. 2007 Oct 1;149(1):160-5. doi: 10.1016/j.jhazmat.2007.03.065. Epub 2007 Mar 27.

Abstract

A pre-concentration method was developed for determination of trace amounts of cadmium, copper and lead in water samples by FAAS after coprecipitation by using potassium 4-methylpiperidinedithiocarbamate (K4-MPDC) as a chelating agent and Bi(III) as a carrier element. This procedure is based on filtration of the solution containing precipitate on a cellulose nitrate membrane filter following Cd(II), Cu(II) and Pb(II) coprecipitation with Bi(III)4-MPDC and then the precipitates together with membrane filter were dissolved in concentrated nitric acid. The metal contents of the final solution were determined by FAAS. Several parameters including pH of sample solution, amount of carrier element and reagent, standing time, sample volume for precipitation and the effects of diverse ions were examined. The accuracy of the method was tested with standard reference material (MBH, C31XB20 and CRM BCR-32) and Cd, Cu and Pb added samples. Determination of Cd, Cu and Pb was carried out in sea water, river water and tap water samples. The recoveries were >95%. The relative standard deviations of determination were less than 10%.

摘要

开发了一种预富集方法,以4-甲基哌啶二硫代氨基甲酸钾(K4-MPDC)作为螯合剂,铋(III)作为载体元素,通过共沉淀法对水样中的痕量镉、铜和铅进行火焰原子吸收光谱法(FAAS)测定。该方法基于在硝酸纤维素膜过滤器上过滤含有沉淀物的溶液,此前镉(II)、铜(II)和铅(II)与铋(III)-4-MPDC发生共沉淀,然后将沉淀物连同膜过滤器一起溶解在浓硝酸中。通过FAAS测定最终溶液中的金属含量。考察了几个参数,包括样品溶液的pH值、载体元素和试剂的用量、静置时间、沉淀的样品体积以及各种离子的影响。用标准参考物质(MBH、C31XB20和CRM BCR-32)以及添加了镉、铜和铅的样品测试了该方法的准确性。对海水、河水和自来水样品中的镉、铜和铅进行了测定。回收率>95%。测定的相对标准偏差小于10%。

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