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Simultaneous determination of Cr(III) and Cr(VI) in tannery wastewater using low pressure ion chromatography combined with flow injection spectrophotometry

机译:低压离子色谱-流动注射分光光度法同时测定制革废水中的Cr(III)和Cr(VI)

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Trivalent and hexavalent chromium have been successfully separated and determined using low pressure ion chromatography combined with flow injection spectrophotometric analysis (LPIC-FIA). A column packed with crosslinking starch microspheres was used for on-line separation of Cr(III) from Cr(VI) in a flow-injection system because of its absorptive effect on Cr(III). To determine the concentration of Cr(III) and Cr(VI) in samples, we used 3.0 mmol/L nitric acid to elute adsorbed Cr(III) from the column and then used ceric sulfate-sulfuric acid as oxidant to convert all Cr(III) into Cr(VI). Then, Cr(VI) directly came from the samples and Cr(VI) came from Cr(III) successively formed a amaranthine complex with diphenycarbazide and the complex shows a maximum absorption at 530 nm. Analytical parameters including the concentration of eluent and oxidant solution, oxidizing temperature, length of oxidizing reaction coil, reaction coil and injection coil, interfering effects, etc., were optimized. The limit of detection was 1.25 μg/L for Cr(VI) and 3.76 μg/L for Cr(III). The linear relationship between absorption with the concentration of Cr(VI) and Cr(III) was 0.001-1.000 mg/L and 0.030-1.000 mg/L with correlation coefficients of 0.9995 and 0.9994, respectively. The relative standard deviation of Cr(VI) and Cr(III) was 1.21% and 1.66%, respectively (n = 10). Major cations and anions did not show any interference. We validated this method through certified reference materials and through measuring the recovery in tannery wastewater.
机译:三价铬和六价铬已成功分离并使用低压离子色谱法与流动注射分光光度法分析(LPIC-FIA)结合测定。填充有交联淀粉微球的色谱柱由于其对Cr(III)的吸收作用,用于在流动注射系统中从Cr(VI)在线分离Cr(III)。为了测定样品中Cr(III)和Cr(VI)的浓度,我们使用3.0 mmol / L的硝酸从色谱柱上洗脱吸附的Cr(III),然后使用硫酸铈-硫酸作为氧化剂将所有Cr( III)转化为Cr(VI)。然后,Cr(VI)直接来自样品,而Cr(VI)来自Cr(III)并与苯二碳酰肼连续形成a菜红素配合物,该配合物在530 nm处显示最大吸收。优化了洗脱液和氧化剂溶液的浓度,氧化温度,氧化反应盘管,反应盘管和注入盘管的长度,干扰效应等分析参数。 Cr(VI)的检出限为1.25μg/ L,Cr(III)的检出限为3.76μg/ L。吸收与Cr(VI)和Cr(III)的浓度之间的线性关系分别为0.001-1.000 mg / L和0.030-1.000 mg / L,相关系数分别为0.9995和0.9994。 Cr(VI)和Cr(III)的相对标准偏差分别为1.21%和1.66%(n = 10)。主要的阳离子和阴离子没有显示出任何干扰。我们通过认证的参考材料并通过测量制革废水的回收率验证了该方法。

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