热解催化-金汞齐化-冷原子吸收法测定锡精矿中汞  

Determination of mercury in tin concentrate by pyrolytic catalysis-gold amalgamation-cold atomic absorption method

作　　者：黄世明 梁海敏 黄贺 伍斯静 韦玉标 容金华 HUANG Shiming;LIANG Haimin;HUANG He;WU Sijing;WEI Yubiao;Rong Jinhua(China Certification&Inspection Group Guangxi Co.,Ltd.,Nanning 530222,China;Guangxi Zhongjian Testing Technology Service Co.,Ltd.,Fangchenggang 538001,China;Fangchenggang Key Laboratory of Ferrous Metal Products Inspection,Fangchenggang 538001,China)

机构地区：[1]中国检验认证集团广西有限公司,南宁530222 [2]广西中检检测技术服务有限公司,广西防城港538001 [3]防城港市黑色金属矿产品检验重点实验室,广西防城港538001

出　　处：《化学分析计量》2024年第2期72-76,共5页Chemical Analysis And Meterage

摘　　要：采用固体进样全自动测汞仪直接测定锡精矿中汞含量。将锡精矿样品直接在样品舟中称重,在氧气气氛中经历干燥和高温热分解,氧气流将汞带入催化管、齐化管并发生定向反应,最后在光学吸收池进行冷原子吸收光谱测定。在干燥温度200℃、干燥时间60 s、热解温度650℃、热解时间30 s条件下,对三个锡精矿样品进行测定,测定值的相对标准偏差为0.87%~2.40%(n=11),加标回收率为95.2%~104%,与国家标准原子荧光光谱法比对,测定结果一致。共存元素干扰实验结果证明,锡虽然熔点低且能与汞发生锡汞齐反应,但在实验条件下对汞的测定没有影响。该方法适用于锡精矿中汞的快速测定。Mercury content in tin concentrate was directly determined by the automatic mercury measuring instrument for solid sampling.The sample of tin concentrate was directly weighed in the sample boat,and underwent drying and high-temperature thermal decomposition in oxygen atmosphere.The oxygen flow carried mercury into the catalytic tube and the homogenizing tube to undergo directional reaction.Finally,cold atomic absorption spectrometry was performed in the optical absorption tank.Under the conditions of drying temperature of 200°C,drying time of 60 s,pyrolysis temperature of 650°C and pyrolysis time of 30 s,three tin concentrate samples were determined.The relative standard deviation of the measured values were 0.87%-2.40%(n=11),and the recovery rate were 95.2%-104%.Compared with the national standard atomic fluorescence spectrometry,the measured results were consistent.The results show that although tin has low melting point and can react with mercury,it has no effect on the determination of mercury under experimental conditions.This method is suitable for the rapid determination of mercury in tin concentrate.

关 键 词：热解催化 金汞齐化 冷原子吸收 锡精矿 汞 

分 类 号：O657[理学—分析化学]