摘要
提出了用浓硝酸沉淀并分离大量基体钼,ICP AES同时测定钼酸铵中14个杂质元素的方法,考虑了钼基体、酸度、谱线干扰及背景影响等情况。在未引入其它任何试剂的情况下,用硝酸既除去了大量的钼基体,又调整了溶液的酸度,用标准加入法测定钼酸铵中的杂质元素,无需加入高纯基准试剂进行基体匹配,有效降低了分析成本,又消除了由于忽略基准物质中杂质元素的含量给分析测定带来的误差。回收率在85%~112%之间。
ICP-AES method was applied to the determination of 14 elements (Al Bi Ca Cd Co Cr Cu Fe Mg Mn Ni Pb Sb Ti) present as impurities in ammonium molybdate or other polymolybdates. Conditions of analysis (including the choice of analytical spectral lines, effect of acidity of the sample solution, the matrix interference and the working conditions of the instrument) were studied and optimized. To overcome the interference of the matrix element the molybdate sample (2g) was dried at 105℃ and dissolved in water, and then conc. HNO_3 was added to separate molybdate as the light yellow crystalline precipitate of molybdic acid, and the impurity-elements were determined in the filtrate of HNO_3(1+9). The molybdate remained in the filtrate was found to be around 500μg·ml^(-1), the interference of which was then eliminated by the standard addition method. The recoveries of these elements were in the range of 85%~112%.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2004年第9期533-535,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
钼酸铵
杂质元素
ICP-AES法
电感耦合等离子体原子发射光谱
ICP-AES
Ammonium molybdate
Matrix interference
Impurity elements (Al Bi Ca Cd Co Cr Cu Fe Mg Mn Ni Pb Sb Ti)