Themelis Demetrius G, Kika Fotini S, Economou Anastasios
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece.
Talanta. 2006 May 15;69(3):615-20. doi: 10.1016/j.talanta.2005.10.031. Epub 2005 Nov 23.
A new rapid and sensitive FI assay is reported for the simultaneous direct spectrophotometric determination of trace Cr(VI) and Cr(III) in real samples. The method is based upon the reaction of Cr(VI) with chromotropic acid (CA) in highly acidic medium to form a water-soluble complex (lambda(max)=370nm). Cr(III) reacts with CA only after its on-line oxidation to Cr(VI) by alkaline KIO(4). The determination of each chromium species in the sample was achieved by absorbance differences. The calibration curves were linear over the range 3-4000mugl(-1) and 30-1200mugl(-1) for Cr(VI) and Cr(III), respectively, while the precision close to the quantitation limit was satisfactory in both cases (s(r)=3.0% for Cr(VI) and 4.0% for Cr(III) (n=10) at 10 and 50mugl(-1) level, respectively). The method developed proved to be adequately selective and sensitive (c(L)=1 and 10mugl(-1) for Cr(VI) and Cr(III), respectively). The application of the method to the analysis of water samples (tap and mineral water) gave accurate results based on recovery studies (93-106%). Analytical results of real sample analysis were in good agreement with certified values.
报道了一种新的快速灵敏的流动注射分析方法,用于同时直接分光光度法测定实际样品中的痕量Cr(VI)和Cr(III)。该方法基于Cr(VI)在高酸性介质中与变色酸(CA)反应形成水溶性络合物(λ(max)=370nm)。Cr(III)只有在通过碱性KIO(4)在线氧化为Cr(VI)后才与CA反应。通过吸光度差异实现样品中各铬物种的测定。Cr(VI)和Cr(III)的校准曲线分别在3 - 4000μg l(-1)和30 - 1200μg l(-1)范围内呈线性,而在两种情况下接近定量限的精密度均令人满意(在10μg l(-1)和50μg l(-1)水平下,Cr(VI)的s(r)=3.0%,Cr(III)的s(r)=4.0% (n = 10))。所开发的方法具有足够的选择性和灵敏度(Cr(VI)和Cr(III)的检测限分别为1μg l(-1)和10μg l(-1))。基于回收率研究(93 - 106%),该方法应用于水样(自来水和矿泉水)分析得到了准确的结果。实际样品分析的结果与认证值吻合良好。