矿物效应是影响X射线荧光光谱(XRF)分析硅酸盐地质样品中S元素准确度的主要因素之一。本文在前人研究基础上,采用XRF仪器,运用粉末压片技术制备样品,从压力实验、S的灵敏度实验和质量吸收系数对比实验等方面对S的矿物效应进行了佐证;在此基础上,提出分类校准方案,建立了同一类型土壤和水系沉积物系列S的分析方法。方法检出限为1.36μg/g,相对标准偏差为0.97%~3.2%(RSD,n=10),校准曲线准确度为0.0058%,测量值与认定值比较吻合。该研究有助于进行硅酸盐地质样品中痕量S的XRF分析测试时结果的分析。
Mineralogical effects are one of the major factors impacting the determination accuracy of sulfur in geological samples by X-ray fluorescence spectrometry. In this paper, the sample was deter- mined on X-ray fluorescence spectrometer with pressed powder pellet sample preparation. The experimental evidence of mineralogical effects was described on the basis of previous studies from the aspects, including pressure test, sensitivity test and comparison test of mass coefficients. Accordingly, the paper put forward a program of category calibration, and established an analytical method of sulfur in soil and sediment series by XRF. The detection limit of this method is 1.36 μg/g, the relative standard deviation is 0. 97%- 3.2% (RSD, n= 10), and the accuracy of the calibration curve is 0. 005 8 %. This study would help to analyze the XRF results of trace sulfur in geological silicate samples.