X射线荧光光谱法测定化探样品中主、次和痕量组分

X-RAY FLUORESCENCE SPECTROMETRIC DETERMINATION OF MAJOR, MINOR AND TRACE ELEMENTS IN GEOCHEMICAL SAMPLES

采用粉末样品压片制样,用PW2440X射线荧光光谱仪对化探样品中氯、溴、硫、氧化钠、氧化镁、三氧化二铝、二氧化硅、磷、氧化钾、氧化钙、钛、锰、三氧化二铁、钴、铌、锆、钇、锶、铷、铅、钍、锌、铜、镍、钒、铬、钡、镧、铈、钕、钪、镓、砷、铪等34个组分进行测定。讨论了微量元素的背景选择和谱线重叠校正及氯测定的问题。使用经验系数法和康普顿散射线作内标校正基体效应,经标准物质检验,分析结果与标样值吻合,用GBW07308国家一级标准物质作精密度试验,统计结果RSD(n=12)除砷、钒、镍、铜<6.0%,溴、硫、铈、铪、钕、钪、氧化钠、镧、铬、钴和钍<14.0%以外,其余各组分均小于3.0%。

An X-ray fluorescence spectrometric method for the determination of major, minor and trace elements in geochemical exploration samples was developed. The sample was prepared as a pellet under pressure.Discussion was emphasized on the selection of background position, correction of line overlapping and determination of chlorine. Compton scattering line as the internal standard and empirical coefficients were used for the correction of matrix effect. Three Chinese national reference materials GBW 07301, GBW 07317 and GBW 07423 were selected for the verification of the accuracy of the method and the analytical results were well agreed with the certificate values. A Chinese national primary reference material GBW 07308 with low elements contents was selected for precision test. Statistical results showed that RSDs （n= 12） were better than 3. 0% for major elements and others,except for V, Ni, Cu〈6.0 and for Na2O, La, Cr, Co, Nd, Hf, Ce, S, C1, Br, Th〈14.0％.