粉末进样-直接测汞仪测定铜冶炼渣中微量汞  

Determination of Trace Mercury in Copper Smelting Slag by Powder Introduction-Direct Mercury Analyzer

作　　者：钟坚海 温建荣 张强 郑瑞娟[3] 冯均利 廖彬玲 赖秋祥 ZHONG Jianhai;WEN Jianrong;ZHANG Qiang;ZHENG Ruijuan;FENG Junli;LIAO Binling;LAI Qiuxiang(Technology Center,Xiamen Customs,Xiamen 361026,China;The Testing and Technology Center for Industrial Products,Shenzhen Customs,Shenzhen 518067,China;College of Chemistry and Materials Science,Longyan University,Longyan 364012,China;Zijin Copper Co.,Ltd.,Longyan 364100,China)

机构地区：[1]厦门海关技术中心,厦门361026 [2]深圳海关工业品检测技术中心,深圳518067 [3]龙岩学院化学与材料学院,龙岩364012 [4]紫金铜业有限公司,龙岩364100

出　　处：《理化检验（化学分册）》2022年第12期1446-1448,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：龙岩市科技计划项目(2019LYF13004);厦门海关科研项目(2020XK14);福建省科技计划项目(2021I0032);海关总署科研项目(2020HK256)。

摘　　要：提出了粉末进样-直接测汞仪测定铜冶炼渣中微量汞的方法。在高纯氧气氛围中,0.15 g铜冶炼渣样品经200℃干燥和650℃热分解90 s后,汞被催化分解为汞原子并与齐化管中的金形成金汞齐,于850℃加热释放出汞蒸气,测定其在253.7 nm处的特征吸收。在汞质量为1~20 ng和20~400 ng时,用吸光度与汞的质量建立不同的标准曲线,检出限(3s)为0.044 ng·g^(-1)。3个不同汞含量的铜冶炼渣样品测定结果的相对标准偏差(n=11)为1.7%~3.5%;按标准加入法进行回收试验,回收率为91.2%~97.4%。采用该方法与SN/T 2680-2010对同一样品进行测定,测定结果基本一致。A method for determination of trace mercury in copper smelting slag by powder introduction-direct mercury analyzer was proposed.In the high-purity oxygen atmosphere,0.15 g of the copper smelting slag sample was dried at 200℃and thermally decomposed at 650℃for 90 s.Then mercury was catalytically decomposed into mercury atoms and formed gold amalgam with gold.Mercury vapor was released at 850℃and its characteristic absorption at 253.7 nm was measured.When the mercury mass were 1-20 ng and 20-400 ng,different standard curves were established between the absorbance and mass of mercury,with detection limit(3s)of 0.044 ng·g^(-1).RSDs(n=11)of determined results of three copper smelting slag samples with different mercury contents were in the range of 1.7%-3.5%.Test of recovery was made by the standard addition method,giving results in the range of 91.2%-97.4%.There was no difference in determined results by this method and SN/T 2680-2010.

关 键 词：铜冶炼渣 粉末进样 直接测汞仪 汞 

分 类 号：O657[理学—分析化学]