摘要
在使用固体进样测汞仪直接测定硫化铅精矿中汞时,由于试样中硫含量通常较高(高达30%以上),在测定过程中大量硫被氧化造成污染甚至腐蚀固体进样测汞仪的核心部件催化管,导致催化管寿命严重缩短。为解决上述问题,建立了碳酸钙固硫-固体进样测汞仪直接测定硫化铅精矿中汞的分析方法;并对Ca/S比、分解温度、分解时间、齐化时间等参数进行优化。在最优条件下,Hg的含量在2~20 ng和20~500 ng线性范围内回归系数(R^(2))分别为0.9996和0.9998,方法检出限(LOD)为0.006μg/g。对3个典型样品进行测定,相对标准偏差RSD≤9.0%(n=7),加标回收率为96.0%~106%。方法简单、快捷,准确度和精密度高,适合硫化铅精矿中汞的快速测定。
Mercury in lead sulfide concentrate is commonly determined by mercury meter,but the catalytic tube of instrument might be polluted and corroded due to the oxidation of the high content of sulfur(up to more than 30%)in sample,then the life of the direct mercury analyzer-catalytic tube is reduced seriously.In order to solve the problem,a method for direct determination of mercury in lead sulfide concentrate by calcium carbonate sulfur fixation solid injection mercury analyzer was established.The parameters such as Ca/S ratio,decomposition temperature,catalytic time and homogenization time were optimized.Under the optimal conditions,the regression coefficient(R^(2))were 0.9996 and 0.9998 in the linear range of 2-20 ng and 20-500 ng;the detection limit(LOD)of Hg was 0.006μg/g.The results showed that the recoveries of 3 typical samples were in the range of 96.0%-106%(RSD≤9.0%,n=7).The pretreatment process of the method is simple,economical,accuracy and precision,which is suitable for the rapid determination of mercury in lead sulfide concentrate samples.
作者
赵秀荣
张萍萍
罗明贵
乔柱
刘进涛
张新爱
王恒
ZHAO Xiurong;ZHANG Pingping;LUO Minggui;QIAO Zhu;LIU Jintao;ZHANG Xinai;WANG Heng(Lianyungang Customs,Lianyungang,Jiangsu 222042,China;Fangcheng Customs,Fangchenggang,Guangxi 538001,China;Jiangsu University,Zhenjiang,Jiangsu 212013,China)
出处
《中国无机分析化学》
CAS
北大核心
2022年第5期1-6,共6页
Chinese Journal of Inorganic Analytical Chemistry
基金
南京海关科研计划项目(2021KJ04)。
关键词
碳酸钙
硫化铅精矿
固硫剂
固体进样测汞仪
汞
CaCO 3
lead sulfide concentrate
sulfur fixing agent
direct mercury analyzer with solid sampling
Hg
