Huang Dong-Gen, Zhou Wen-Bin, Liu Lei, Quan Shui-Qing, He Zong-Jian, Wan Jin-Bao
School of Environmental Science and Engineering, Key Lab of Poyang Lake Ecology and Bio-resource Utilization, Ministry of Education, Nanchang University, Nanchang 330031, China.
Guang Pu Xue Yu Guang Pu Fen Xi. 2009 Feb;29(2):504-8.
The direct determination method of trace composition, Fe2O3, TiO2, MnO, K2O, Na2O, CaO and MgO, and impurity elements, Pb, Cr, Cd, Cu and As, in kaolin was studied by using inductive coupled plasma mass spectrometry (ICP-MS). After the samples were dissolved completely in HF-HNO3 at low temperature, silicon was volatilized in the form of SiF4 and separated from the solution. Then the solution was continually evaporated to dry to get the solid substance which was dissolved by the nitric acid (1+3). The internal elements 45Sc, 115In and 205Tl were added on line and the effect of matrix, interface and fluctuation of instrument was overcome effectively by using internal standard calibration method. By choosing the optional operating parameters and appropriate isotopes of element to be detected, the influence of mass spectrometry interference was conquered effectively. The effect of temperature in samples preparation on the determination of arsenic was tested. The recovery for spiking sample is in the range from 95.0% to 101.0% and the relative standard deviation is in the range from 1.1% to 2.01%. In order to check the accuracy of the method, the kaolin standard reference material GBW03122 was also analyzed, and the analytical values conformed to standard values. This method has the characteristics of being simple, rapid and accurate, and can be used in the testing of trace composition and impurity elements in kaolin and ceramic product.
采用电感耦合等离子体质谱法（ICP-MS）研究了高岭土中痕量成分Fe2O3、TiO2、MnO、K2O、Na2O、CaO和MgO以及杂质元素Pb、Cr、Cd、Cu和As的直接测定方法。样品在低温下用HF-HNO3完全溶解后，硅以SiF4的形式挥发并与溶液分离。然后将溶液继续蒸发至干得到固体物质，用硝酸（1+3）溶解。在线加入内标元素45Sc、115In和205Tl，采用内标校正法有效克服了基体、接口及仪器波动的影响。通过选择合适的操作参数和待测元素的适当同位素，有效克服了质谱干扰的影响。考察了样品制备温度对砷测定的影响。加标样品回收率在95.0%～101.0%之间，相对标准偏差在1.1%～2.01%之间。为检验方法的准确性，还对高岭土标准物质GBW03122进行了分析，分析值与标准值相符。该方法具有简便、快速、准确的特点，可用于高岭土及陶瓷制品中痕量成分和杂质元素的检测。
