氢化物发生–原子吸收光谱法测定铅粉中痕量砷、锑  

Determination of Trace Arsenic and Antimony in Lead Powder by Hydride Generation–Atomic Absorption Spectrometry

作　　者：范莉君[1] 郭蓉[1] 廖志海[1] 

机构地区：[1]中国核动力研究设计院核燃料及材料重点实验室,成都610005

出　　处：《化学分析计量》2015年第3期73-75,共3页Chemical Analysis And Meterage

摘　　要：建立氢化物发生–原子吸收光谱法联用测定铅粉中痕量砷、锑的方法。试样用稀硝酸溶解,用5%抗坏血酸溶液作为砷(Ⅴ)、锑(Ⅴ)的预还原剂,5%的硫脲溶液作为其它元素的掩蔽剂,选用1%硼氢化钠溶液作为还原剂,氢化物反应在10%盐酸介质中进行。在优化的试验条件下,砷、锑的质量浓度在0~20 ng/m L范围内与吸光度线性相关,相关系数r2分别为砷0.999 6,锑0.993 8,方法的检出限分别为砷0.40 ng/m L,锑0.75 ng/m L。砷、锑测定结果的相对标准偏差分别为4.96%,6.27%(n=6),铅粉样品加标回收率分别为砷87.6%,锑79.3%。该方法准确可靠,可用于测定铅粉中痕量砷、锑。A method of hydride generation–atomic absorption spectrometry was set up for determination of trace arsenic and antimony in lead powder. Sample was dissolved in nitric acid,ascorbic acid(5%) was used as beforehand reducing agent to reduce the arsenic( Ⅴ) and antimony( Ⅴ). Sulfocarbamide(5%) was used to mask other elements. Sodium borohydride(1%) was used as reducing agent. Hydride generation was reacted in the hydrochloric acid(10%). In the optimizational work condition,arsenic and antimony was linearly with the absorbance during 0–20 ng/m L with the correlation coeffi cient of arsenic 0.999 6, antimony 0.993 8, the detection limit of 0.40 ng/m L for As and 0.75 ng/m L for Sb. RSDs of the determination results were 4.96%,6.27%(n=6) for As and Sb,respectively. The recoveries of As and Sb were 87.6% and 79.3%,respectively. The method is accurate and reliable, it is suitable for determination of trace arsenic and antimony in lead powder.

关 键 词：氢化物发生 原子吸收光谱法 砷 锑 

分 类 号：O657.31[理学—分析化学] TQ320.4[理学—化学]