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首页> 外文期刊>Analytical Sciences >Speciation Analysis of Ultratrace Chromium in Water by On-line Reaction/Concentration/Separation Method Using a Cation-Exchange Column
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Speciation Analysis of Ultratrace Chromium in Water by On-line Reaction/Concentration/Separation Method Using a Cation-Exchange Column

机译：阳离子交换柱在线反应/浓缩/分离法分析水中的痕量铬

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A cation-exchange column (TSK IC-Cation, 4.6 mm i.d., 10 mm) was used as a reaction/concentration/separation medium in an HPLC system. Cr(VI) and 1,5-diphenylcarbazide (DPC) were on-line mixed and reacted in a flow tube. When the reagents flowed into the column, both DPC and the complex were concentrated on the column, and the higher DPC concentration accelerated the remaining Cr(VI) to quickly complete the reaction with the DPC on the column. After the complexation and preconcentration, the complex and the extra DPC were eluted by a mixed solution containing lanthanum chloride and 1-propanol. The absorbance of the Cr(III)-DPCO complex at 540 nm was continuously monitored. In addition, the dissolved Cr(III) could be oxidized to Cr(VI) by 185-nm irradiation using a low pressure ultraviolet (UV) lamp for 8 min, and then analyzed by the present method as total chromium, thus the quantitative speciation analysis of Cr(III) and Cr(VI) was realized. In the range of 1 ng dm−3 – 100 μg dm−3 Cr(VI) concentration, the calibration curve was linear. The analytical time was 8 min for Cr(VI) and 24 min for total Cr. The detection limit (3σ) of the method was 0.6 ng dm−3 for Cr(VI) and 0.8 ng dm−3 for total chromium when using a 3.9-cm3 water sample. The present method could be successfully applied to the speciation analysis of dissolved chromium in natural water, and the leaching test of Cr(III) and Cr(VI) from stainless steel.
机译：阳离子交换柱（TSK IC-Cation，4.6mm i.d.，10mm）用作HPLC系统中的反应/浓缩/分离介质。 Cr（VI）和1,5-二苯基咔嗪（DPC）在线混合并在流管中反应。当试剂流入色谱柱时，DPC和络合物都在色谱柱上浓缩，较高的DPC浓度会加速剩余的Cr（VI），从而快速完成与色谱柱上DPC的反应。络合和预浓缩后，将络合物和多余的DPC用含有氯化镧和1-丙醇的混合溶液洗脱。连续监测Cr（III）-DPCO络合物在540 nm处的吸光度。此外，使用低压紫外灯（UV）185 nm照射8 min，可将溶解的Cr（III）氧化为Cr（VI），然后通过本方法分析为总铬，因此可进行定量形态分析。对Cr（III）和Cr（VI）进行了分析。在1 ng dm-3 – 100μgdm-3 Cr（VI）浓度范围内，校准曲线是线性的。 Cr（VI）的分析时间为8分钟，总Cr的分析时间为24分钟。当使用3.9-cm3水样时，该方法的检出限（3σ）对Cr（VI）的检测极限为0.6 ng dm-3，对总铬的检测极限为0.8 ng dm-3。该方法可成功应用于天然水中溶解铬的形态分析，以及不锈钢中Cr（III）和Cr（VI）的浸出试验。

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