氢化物发生-原子荧光光谱法(HG-AFS)测定特硬铅合金中硒和碲

建立了氢化物发生-原子荧光光谱法(HG-AFS)测定特硬铅合金中硒和碲的分析方法。试样经硝酸和酒石酸溶解,硫酸沉淀分离基体铅元素。移取部分试液,在40%盐酸介质中直接用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的硒;另移取部分试液,加入氢溴酸挥发除去砷、锑、锡、硒等元素,在40%盐酸介质中用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的碲。考察了测定的最佳条件、铅及共存元素对测定的影响。测定硒和碲的相对标准偏差分别为7.5%～9.3%和3.6%～13.0%,加标回收率分别为88%～92%和98%～102%。准确度和精密度均能满足分析需要,具有较强的实用性。

Determination of Selenium and Tellurium in Extra Hard Lead Alloy

A hydride generation-atomic fluorescence spectrometry(HG-AFS) method has been established for the determination of selenium and tellurium in extra hard lead alloy.Firstly,the sample was dissolved in nitric acid and tartaric acid,then,the lead was removed from the matrix by sulfuric acid precipitation method.A portion of the solution was taken and selenium was measured by hydride generation-atomic fluorescence spectrometry(HG-AFS) with 40% hydrochloric acid as the medium.Then,another portion of the solution was treated by hydrobromic acid,which resulted in removal of arsenic,antimony,tin and selenium from the solution due to the vaporization of three elements.Tellurium content was measured by hydride generation-atomic fluorescence spectrometry(HG-AFS) in 40% hydrochloric acid.The optimum experimental parameters and the effects of lead and other coexistent elements on the determination of selenium and tellurium were investigated.The relative standard deviations for selenium and tellurium were 7.5%~9.3% and 3.6%~13.0%,respectively.The recoveries of standard addition for selenium and tellurium were 88%~92% and 98%~102%,respectively.The accuracy and precision of the method meet the analysis demands,and the method is relatively practical.