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通过固相萃取和石墨炉原子吸收光谱法对矿泉水中铬的形态分析以及盐田分析。

Speciation of chromium in mineral waters and salinas by solid-phase extraction and graphite furnace atomic absorption spectrometry.

作者信息

Chwastowska Jadwiga, Skwara Witold, Sterlińska Elzbieta, Pszonicki Leon

机构信息

Department of Analytical Chemistry, Institute of Nuclear Chemistry and Technology, ul. Dorodna 16, 03195 Warsaw, Poland.

出版信息

Talanta. 2005 Jun 15;66(5):1345-9. doi: 10.1016/j.talanta.2005.01.055. Epub 2005 Feb 26.

Abstract

A simple GF-AAS method for speciation analysis of chromium in mineral waters and salinas was developed. Cr(VI) species were separated from Cr(III) by solid-phase extraction with APDC (ammonium pyrrolidinedithiocarbamate). The APDC complexes were formed in the sample solution under proper conditions, adsorbed on Diaion HP-2MG resin and the resin was separated from the sample. After elution with concentrated nitric acid Cr(VI) was determined by GF-AAS. Total chromium was determined by GF-AAS directly in the sample and Cr(III) concentration was calculated as the difference between those results. The detection limit of the method defined as 3s of background variation was 0.03mugl(-1) for Cr(VI) and 0.3mugl(-1) for total chromium. RSD for Cr(VI) determination at the concentration of 0.14mugl(-1) was 9%, and for total chromium at the concentration of 5.6mugl(-1) was 5%. The recovery of Cr(VI) was in the range of 94-100%, dependently on type of the sample. The investigation of recovery of the spiked Cr(VI) showed that at concentration levels near 1mugl(-1) and lower recovery may be reduced significantly even by pure reagents that seem to be free from any reductants.

摘要

开发了一种用于矿泉水中铬形态分析的简单石墨炉原子吸收光谱法(GF-AAS)。通过用吡咯烷二硫代氨基甲酸铵(APDC)进行固相萃取,将六价铬(Cr(VI))与三价铬(Cr(III))分离。在适当条件下,在样品溶液中形成APDC配合物,吸附在Diaion HP-2MG树脂上,然后将树脂与样品分离。用浓硝酸洗脱后,通过GF-AAS测定Cr(VI)。直接用GF-AAS测定样品中的总铬,并计算Cr(III)浓度,即两者结果之差。该方法以背景变化的3倍标准偏差定义的检测限,对于Cr(VI)为0.03μg l⁻¹,对于总铬为0.3μg l⁻¹。在0.14μg l⁻¹浓度下测定Cr(VI)的相对标准偏差(RSD)为9%,在5.6μg l⁻¹浓度下测定总铬的RSD为5%。Cr(VI)的回收率在94%至100%之间,具体取决于样品类型。对加标Cr(VI)回收率的研究表明,在浓度接近1μg l⁻¹及更低时,即使是看似不含任何还原剂的纯试剂,回收率也可能显著降低。

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