CAJ | 학술논문

X射线荧光光谱法（ XRF）已经应用于石膏等非金属矿物的测定，但由于石膏标准物质匮乏、硫含量较高且在高温易挥发损失，给测定带来了一定困难。本文采用石膏标准物质、高纯硫酸钙和其他国家一级标准物质（土壤、水系沉积物、碳酸盐）配制人工标准物质拟合校准曲线，优化稀释比、熔矿温度等熔融制样条件，用理论α系数校正基体效应，建立了采用XRF同时测定石膏矿中10个主次量元素（硅铝铁钙镁钾钠钛硫锶）的分析方法。样品与四硼酸锂-偏硼酸锂熔剂的稀释比为1：9，在1050℃温度下样品熔融完全。方法检出限为4~135μg/g，精密度（RSD，n＝12）小于3.0%。本方法配制的人工校准样品加强了样品基体的适应性，使用的四硼酸锂-偏硼酸锂熔剂在样品熔融过程中可有效地结合硫，抑制了硫的挥发损失，适用于批量分析硫含量高达12.60%~51.91%的实际石膏矿物。
X사선형광광보법（ XRF）이경응용우석고등비금속광물적측정，단유우석고표준물질궤핍、류함량교고차재고온역휘발손실，급측정대래료일정곤난。본문채용석고표준물질、고순류산개화기타국가일급표준물질（토양、수계침적물、탄산염）배제인공표준물질의합교준곡선，우화희석비、용광온도등용융제양조건，용이론α계수교정기체효응，건립료채용XRF동시측정석고광중10개주차량원소（규려철개미갑납태류송）적분석방법。양품여사붕산리-편붕산리용제적희석비위1：9，재1050℃온도하양품용융완전。방법검출한위4~135μg/g，정밀도（RSD，n＝12）소우3.0%。본방법배제적인공교준양품가강료양품기체적괄응성，사용적사붕산리-편붕산리용제재양품용융과정중가유효지결합류，억제료류적휘발손실，괄용우비량분석류함량고체12.60%~51.91%적실제석고광물。
X-ray Fluorescence Spectrometry( XRF ) technique has been applied to the determination of non-metallic minerals such as gypsum. However,the method is limited due to the lack of certified reference materials and the high content of sulfur and easy volatilization loss of sulfur at high temperature. In order to fit the standard calibration curve,synthetic reference materials were prepared by using gypsum certified reference materials,high purity calcium sulfate and other national primary certified reference materials ( soils, stream sediments, carbonate). A method for the determination of ten major and minor components(Si,Al,Fe,Ca,Mg,K,Ha,Ti, S,Sr)by XRF was proposed. Dilution ratio and melting temperature were optimized and the matrix effect was corrected by a theoreticalαcoefficient. Results show that gypsum can be completely melted when the dilution ratio was 1: 9 and the melting temperature was 1050℃. The detection limits of the method are 4-135 μg/g,and the precision(RSD,n =12)is less than 3. 0%;analytical results of certified reference materials were in good agreement with certified values. The synthetic reference materials for the method expand the adaptability of the sample matrix. The lithium tetraborate-lithium metaborate flux in the melting process could be effectively combined with S,suppressing sulfur volatilization. The method is suitable for batch analysis of the gypsum samples with the sulfur content between 12 . 60% and 51 . 91%.