摘要
提出了氢化物发生-原子荧光光谱法测定锑精矿中痕量硒和铋的方法。用王水溶解样品完全,水浴80℃,加热45 min,硒、铋溶出量最大。在试液中加入酒石酸络合大量锑(Ⅴ)使其保持在溶液中。分取部分试液(1/10)加入浓盐酸使其浓度达5～6 mol·L^(-1),从而不需任何化学分离,直接使锑精矿中痕量硒和铋生成氢化物并进行原子荧光测定。方法的检出限(3s/k)为0.18μg·L^(-1)(硒),0.11μg·L^(-1)(铋)。对两种锑精矿样品按所提出方法分析并以此作基体加入两个不同浓度水平的硒和铋标准,进行方法的准确度和精密度试验,测得回收率分别为97.5%～103.2%和92.0～96.0%,相对标准偏差(n=6)依次为1.4%～2.4%和1.2%～1.7%之间。
Method of HG-AFS for determination of Se and Bi in antimony concentrates was proposed. The sample was effectively dissolved with aqua regia at 80℃for 45 min, rendering maximum extraction and dissolution of selenium and bismuth from the sample. A limited amount of tartaric acid solution （〈2g · L^-1） was added to complex with Sb（V ） and to keep it in solution. An aliquot of the sample solution （1/10） was taken and conc. HC1 was added to make the concentration of HCl to 5- 6 mol· L^-1. The solution was introduced into the intermittent FI-reactor to generate hydrides of Se and Bi which were determined by AFS. Detection limit （3s/k） of the method was determined and values found were 0. 18μg · L^-1 for Se and 0. 11μg · L^-1 for Bi. Accuracy and precision of the method were tested by analyzing 2 ore concentrate samples with addition of standard Se and Bi at 2 different concentration levels, values of recovery in the ranges of 97.5%-103.2% and 92. 0-96. 0% were found for Se and Bi respectively, and values of RSD＇s （n=6） found were ranged from 1.40%-2. 4% （for Se） and 1.2%-1.7% （for Bi）.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2009年第10期1184-1186,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质量技术监督检验检疫总局科研项目(2004IK079)
