首页|萃取分离-电感耦合等离子光谱法测定铼酸铵中的杂质元素

萃取分离-电感耦合等离子光谱法测定铼酸铵中的杂质元素

Determination of Impurity Elements in Ammonium Rhenate by Extractive Separation-Inductively Coupled Plasma Spectrometry

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铼酸铵样品具有铼基体高、杂质元素含量低的特点,若不对其进行有效处理,直接消解样品在ICP-AES下进行杂质元素的测定,会使得测定结果不准确及造成设备污染.试验先采用硝酸溶解、酒石酸络合部分杂质离子,后采用磷酸三丁酯(TBP)与三烷基叔胺(N235)混合萃取剂分离,实现了基体铼与杂质元素的分离,消除了基体效应,再采用电感耦合等离子体光谱法(ICP-AES)进行杂质元素的测定.结果表明:Al、As、Bi等杂质元素的检出限为0.008~0.07 ug/mL,方法的测定下限为:0.0003%~0.005%.将试验方法应用于测定实际铼酸铵的样品,测定结果与电感耦合等离子体质谱法(ICP-MS)基本一致,本方法测定杂质元素检测结果的相对标准偏差在5.27%~10.32%,同时经过格拉布斯检验方法判断数据无可疑值,说明磷酸三丁酯-N235体系萃取高价基体铼后,测定铼酸铵中杂质元素的含量满足实验室精密度要求.
Ammonium rhenate samples have the characteristics of high rhenium matrix and low content of impurity ele-ments. If the rhenium matrix is not treated effectively,direct digestion of the sample and determination of impurity elements under ICP-AES will make the determination results inaccurate and cause equipment pollution. In the experiment,some im-purity ions were dissolved by nitric acid and complex with tartaric acid,then tributyl phosphate (TBP) and trialkyl tertiary amine ( N235) were separated by a mixed extractant to achieve the separation of matrix rhenium and impurity elements and eliminate the matrix effect,and then the impurity elements were determined by inductively coupled plasma spectrometry ( ICP-AES) . The results show that the detection limits of aluminum,arsenic,bismuth and other impurities are 0.008~0.07 ug/mL,and the lower limit of the method is 0.0003%~0.005%. The test method was applied to determine the actual ammonium rhenate samples,and the test results were basically consistent with that of inductively coupled plasma mass spectrometry ( ICP-MS) . The relative standard deviation of the test results for the determination of impurity elements was 5.27%~10.32%. The results indicate that the content of impurity elements in ammonium rhenate can meet the requirement of laboratory precision after extraction of rhenium with tributyl phosphate and N235 system.

extraction and separationammonium rhenateICP-AESquantitative detectionimpurity element

展之旺、庞振业、方彦霞、张彦翠

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西北矿冶研究院,甘肃 白银 730900

萃取分离 铼酸铵 ICP-AES 定量检测 杂质元素

2024

甘肃冶金
甘肃省金属学会,西北矿冶研究院

甘肃冶金

影响因子:0.176
ISSN:1672-4461
年,卷(期):2024.46(5)