原子荧光光谱法测定砷锭中汞  

AFS Determination of Mercury in Arsenic Ingot

作　　者：李艳琳[1] 陆建平[1] 倪湖权[1] 谭芳维[1] 石建荣 唐燕葵[3] 

机构地区：[1]广西大学化学化工学院,南宁530004 [2]广西华锑科技有限公司,南宁530007 [3]广西大学环境学院,南宁530004

出　　处：《理化检验（化学分册）》2013年第12期1462-1464,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金(51168001)资助;广西大学试验室建设与试验教学改革项目(20120319)

摘　　要：提出了原子荧光光谱法测定砷锭中汞含量的方法。样品用盐酸-硝酸（1＋1）混合酸溶解，用正丁醇萃取溶液中的汞（Ⅱ）。有机相中的汞（Ⅱ）以10g·L^-1硼氢化钾溶液作还原剂，还原成汞蒸气后以原子荧光光谱法测定其含量。汞的质量浓度在0．15-80μg·L^-1范围内与相应的荧光强度呈线性关系，方法检出限（3s／k）为0．20μg·L^-1。应用此法分析了2件砷锭样品，所得汞含量测定值的相对标准偏差（n=6）小于2％；加标回收率在96．3％～97．2％之间。A method of AFS for the determination of mercury in arsenic ingot was proposed. The sample was dissolved in mixed acid of HCl-HNO3 （1＋1）, and Hg（ Ⅱ ） in the sample solution was extracted into n butyl alcohol. Mercury（ Ⅱ ） in the organic phase was reduced to mercury vapor with 10 g · L^-11 potassium borohydride solution and determined by AFS. Linear relationship between values of fluorescence intensity and mass concentration of mercury was kept in the range of 0.15-80μg · L^-1 , with detection limit （3s/k） of 0.20 μg · L^-1. The proposed method was applied to the analysis of 2 samples of arsenic ingots, giving values of RSD＇s （n=6） less than 2%, and values of recovery found by standard addition method in the range of 96.3 %- 97.2 %.

关 键 词：原子荧光光谱法 砷锭 汞 

分 类 号：O657.3[理学—分析化学]