超痕量六价铬分析仪检测制革场地中六价铬  

Determination of Hexavalent Chromium in Leather Field by Ultra Trace Hexavalent Chromium Analyzer

作　　者：李晓敏 吴小龙 符式锦 张临 黄玉洁 LI Xiaomin;WU Xiaolong;FU Shijin;ZHANG Lin;HUANG Yujie(Hainan Province Environmental Monitoring Centre,Haikou,Hainan 570100,China)

机构地区：[1]海南省生态环境监测中心,海口570100

出　　处：《中国无机分析化学》2023年第11期1176-1182,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：海南省自然科学基金资助项目(423QN316)。

摘　　要：为解决制革等污染场地中Cr(Ⅲ)-有机络合物会干扰六价铬(Ⅵ)测定的问题,通过优化仪器色谱条件、在现有行业标准基础上改进前处理方式,使用超痕量六价铬分析仪检测六价铬,并通过在土壤中投加低、中、高浓度的三价铬、六价铬以及Cr(Ⅲ)-有机络合物考察三价铬、色度和Cr(Ⅲ)-有机络合物对六价铬测定的影响。结果表明,仪器的最佳色谱条件为流动相浓度0.1 mol/L、流动相pH=9、浓硫酸体积分数为1%、流动相流速1.2 mL/min、衍生试剂流速0.7 mL/min。样品预处理方式由抽滤提取改进为离心提取,上机前样品pH值无需调节,可提高检测效率。方法操作简便、耗时短,且不受三价铬、样品色度及Cr(Ⅲ)-有机络合物的干扰。方法的精密度和正确度均显著提高,相对标准偏差为1.7%~5.2%,加标回收率均在94.6%~103%。通过与液相色谱-电感耦合等离子体质谱仪对实际样品测定结果的统计学检验发现,结果无显著性差异。方法适用于制革、电镀等富含Cr(Ⅲ)-有机络合物场地中六价铬的测定。In order to solve the problem that Cr(Ⅲ)-organic complex interfere with the determination of hexavalent chromium in polluted sites such as leather making,the chromatographic conditions of the instrument was optimized,the pretreatment method on the basis of the existing standard was improved,an ultra-trace hexavalent chromium analyzer was used to detect hexavalent chromium.The influence of trivalent chromium,chroma and Cr(Ⅲ)-organic complex on hexavalent chromium determination were investigated by adding different concentrations of trivalent chromium,hexavalent chromium and Cr(Ⅲ)-organic complex(low,medium and high)in soil.The results showed that the optimal chromatographic conditions were as follows:the concentration of mobile phase was 0.1 mol/L,the pH of mobile phase was 9,the volume fraction of sulfuric acid was 1%,the flow rate of mobile phase was 1.2 mL/min,and the flow rate of derived reagent was 0.7 mL/min.The pretreatment method of samples was improved from filtration extraction to centrifugal extraction,and the pH of samples did not need to be adjusted before loading,which could improve the detection efficiency.Compared with the current standard,this method was simple and short in operation.Furthermore,it was free from the interference of chromium trivalent,sample chrominance and Cr(Ⅲ)-organic complex.The precision and accuracy of the method were significantly improved,and the relative standard deviations were 1.7%—5.2%,and the recoveries were 94.6%—103%.The results were statistically tested by liquid chromatography-inductively coupled plasma mass spectrometer,and the results showed no significant difference.The method is suitable for the determination of hexavalent chromium in the fields rich in Cr(Ⅲ)-organic complexes such as tannery and electroplating.

关 键 词：六价铬 超痕量六价铬分析仪 Cr(Ⅲ)-有机络合物 制革 电镀 

分 类 号：O657.32[理学—分析化学] X833[理学—化学]