冷原子荧光光谱法测定水泥中的汞.docVIP

热解吸收氢化物发生冷原子荧光光谱法测定水泥中的痕量汞 陆建平，王 丽，卢志勇，梁火辉 （广西大学 化学化工学院，南宁 530004） 摘 要：建立了HG-AFS测定水泥样品中总汞的方法。采用自制的石英管加热处理样品，高锰酸钾溶液吸收释放的Hg0，盐酸羟胺还原过量的高锰酸钾后直接进行测定。试验中优化了仪器的工作参数和试验条件。试样热解温度为550 ℃，加热时间为58 s，试样载气流量为100 mL·min。本方法的检出限为0.020 μg·L，相对标准偏差为1.2%。用国家标准土壤GBW07405验证了方法的准确性，并测定了广西不同地域生产水泥中的汞，回收率为97.1% ～ 106.9%，RSD（n=6）为～。 关键词 氢化物发生；冷原子荧光光谱法；水泥；汞 中图分类号：O657.31 文献表识码：A Determination of Trace Mercury in Cement by Pyrolysis and Absorption —Hydride Generation Cold Vapor Atomic Fluorescence Spectrometry LU Jian-ping, WANG Li, LU Zhi-yong, LIANG Huo-hui (College of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004,China) Abstract A method for the determination of total mercury in cement samples by hydride generation-atomic fluorescence spectrometry (HG-AFS) was developed. The samples were heated inside a self-made quartz tube, the released Hg0 was absorbed by potassium permanganate solution and the superfluous potassium permanganate was reduced by hydroxylamine hydrochloride solution afterwards, then mercury was determined directly. The instrumental parameters and _______________________________________________ 基金项目：广西科技厅资助项目（桂科自0778006-16） 作者简介：陆建平（1955-）， 男，江苏常州人，从事环境中有害物质的识别及测定的研究，教授，博士， e-mail:ljianpi@ experimental conditions were optimized. The temperature of sample pyrolyzer was 550℃, the heating time was 58 seconds and the carrier Ar flow rate was 100mL/min. The method detection limit was 0.020μg/L and RSD was 1.2%. The method was validated by determining mercury in thenational soil standard GBW07405 and applied to determine the mercury content of cements produced in different regions of Guangxi, the values of recovery was in the range of 97.1% ～ 106.9%, the RSD (n=6) was in the range of 0.7% ～ 4.1%. Keywords Hydride Generation; Cold Vapor Atomic Fluorescence Spectrometry; Cement; Mercury 水泥及水泥基复合材料是世界上用量最大的人造材料。在水泥混凝土的制备过程中，各种工业废渣甚至城市固态废弃物的综合利用比比皆是。由于水泥和混凝土中大量使用各种工业废弃物，不可避免地导致混凝土中某些有害物质的含量大大增加，而其中一些含量相对较高的有害物质会从水泥混凝土中释放导致二次环境污染，该问题已引起了国际混凝土界的普遍关注和高度重