柱后衍生-离子色谱法测定固废中的六价铬方法优化  

Optimization of Post-column Derived Ion Chromatography for Determination of Hexavalent Chromium in Solid Waste

作　　者：田文娟 郭丽 杜维 郑丹 TIAN Wenjuan;GUO Li;DU Wei;ZHENG Dan(Hubei Ecological Environmental Monitoring Center Station,Hubei Wuhan 430072;Wuhan Technology and Business University,Hubei Wuhan 430065,China)

机构地区：[1]湖北省生态环境监测中心站,湖北武汉430072 [2]武汉工商学院,湖北武汉430065

出　　处：《广州化工》2024年第20期110-114,共5页GuangZhou Chemical Industry

摘　　要：建立柱后衍生-离子色谱法测定固体废物中六价铬。参考GB5085.3-2007附录T固体废物六价铬提取方法,从流动相浓度、流动相pH值、衍生化试剂pH值、流动相与衍生化试剂流速比四个方面优化仪器条件。硝酸根浓度为0.1 mol/L,流动相的pH值为9.0,衍生化试剂中含1%浓硫酸,流动相流速为1.2 mL/min,衍生化试剂流速为0.7 mL/min为最佳。六价铬工作曲线线性相关系数(r)大于0.999 8,方法检出限为0.06 mg/kg,测定上限250 mg/kg,测定结果相对误差小于4.0%,实验室内相对标准偏差(RSD,n=6)为0.9%~9.1%,样品加标回收率为74%~92%。本方法检出限低,线性范围宽,准确度高,精密度好,适用于固体废物中六价铬的分析。A post-column derivation-ion chromatography method for the determination of hexavalent chromium in solid waste was established.Refered to GB5085.3-2007 Appendix T solid waste hexavalent chromium extraction method,the instrument conditions were optimized from four aspects:mobile phase concentration,pH value of mobile phase,pH value of derivatization reagent and flow rate ratio of mobile phase to derivatization reagent.The concentration of nitrate was 0.1 mol/L,the pH value of mobile phase was 9.0,the derivated reagent contained 1%concentrated sulfuric acid,the flow rate of mobile phase was 1.2 mL/min,and the flow rate of derivated reagent was 0.7 mL/min.The linear correlation coefficient(r)of chromium VI working curve was greater than 0.9998,the detection limit of the method was 0.06 mg/kg,the upper limit of the determination was 250 mg/kg,the relative error of the measurement results was less than 4.0%,and the relative standard deviation(RSD,n=6)in the laboratory was 0.9%to 9.1%.The recoveries were 74%to 92%.The method has low detection limit,wide linear range,high accuracy and good precision,and is suitable for the analysis of hexavalent chromium in solid waste.

关 键 词：柱后衍生-离子色谱法 固体废物 六价铬 

分 类 号：X833[环境科学与工程—环境工程]