双毛细管在线干扰校正-电感耦合等离子体发射光谱法测定含铀地质样品中微量铅
河南省核工业放射性核素检测中心, 河南 郑州 450002 |
Determination of Trace Lead in Uranium-bearing Geological Samples by Inductively Coupled Plasma-Optical Emission Spectrometry with Double Capillary On-line Interference Correction
Henan Radionuclide Detection Center of Nuclear Industry, Zhengzhou 450002, China |
摘要：应用电感耦合等离子体发射光谱法测定地质样品中的铅时, 基体元素的干扰会使测量结果偏低。本文用氢氟酸、硝酸、高氯酸、盐酸溶解样品, 采用等径双毛细管在线干扰校正的方法测定了含铀地质样品中的微量铅。首先通过双毛细管确定了样品溶液中的Fe、Al对铅有负干扰, 而一定浓度的U、Ba、Ti、Ca、Mn、K、Mg、Na等基体元素没有干扰或可以忽略, 由此在线双毛细管根据样品中Fe、Al的含量使用不同的校正试液建立标准曲线, 测定未知样品时同步进行稀释, 降低了Fe、Al的基体效应。方法检出限为1.5 μg/g, 精密度(RSD)小于5%。与普通干扰校正法相比, 双毛细管在线干扰校正法可根据不同基体的样品使用不同的干扰校正试液, 快速建立标准曲线进行复杂样品的测定, 且避免了二次稀释, 节省试剂, 适合测定基体成分接近的批量样品。
Determination of Trace Lead in Uranium-bearing Geological Samples by Inductively Coupled Plasma-Optical Emission Spectrometry with Double Capillary On-line Interference Correction
ABSTRACT Measured lead contents in geological samples were commonly lower than real values because of matrix elements interference during Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) analyses. In this study, U-bearing geological samples were dissolved by hydrofluoric acid, nitric acid, perchloric acid, and hydrochloric acid. Trace lead was determined by ICP-OES with double capillary on-line interference correction. The interferences of matrix elements on lead were studied using double capillary. Iron and Al had negative interferences on lead, whereas a specific concentration of U, Ba, Ti, Ca, Mn, Mg, K and Na almost had no interferences on lead. The standard curve was established using double capillary according to the contents of Fe and Al in different test solution. The unknown sample was diluted simultaneously, which reduced the matrix effects of Fe and Al. The detection limit was 1.5 μg/g, and the RSD was less than 5%. Compared with the common interference correction method, the double capillary on-line interference correction method can establish a standard curve quickly using different interference correction test solutions according to different matrices. Moreover, sample solution does not need to be secondly diluted, saving the reagent. This method is suitable for rapid determination of batch samples with similar matrices.
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