熔融制样-X射线荧光光谱法测定地质样品中的主次成分

Simultaneous determination of major and minor components in geological sample by XRF with fusion sample preparation

以Li2B4O7,Li BO2和Li F(质量比为45:10:5)为混合熔剂,NH4NO3为氧化剂,Li Br为脱模剂,熔融制作样片,利用岛津1800型X射线荧光光谱分析仪,对土壤、水系沉积物、硅酸盐、白云岩等标准物质拟合校准曲线,建立了X射线荧光光谱法(XRF)同时测定岩石、土壤样品中主次量组分(Si O2,Al2O3,TFe2O3,Mg O,Ca O,K2O,Na2O,M n O,Ti O2,P2O5,Zn O)的快速分析方法。对样品制备以及分析测试过程中的条件(熔剂稀释比例、熔融温度及时间、测定电压电流以及脉冲高度分析)进行了优化,在优化的条件下,对GBW07105,GBW07401进行重复测定,相对标准偏差RSD<2%,相对误差RE<5%。同时对超基性岩、硅酸盐、沉积物、土壤等国家标准样品进行分析,结果与标准参考值有良好的一致性。

A fast and simple approach to directly determine SiO2, Al2O3, TFe2O3, MgO, CaO, K2O, Na2O, MnO, TiO/, P205 and ZnO in rock and soil samples by XRF was developed. This method used glass fuse piece technique with Li2B407, LiBO2 and LiF （mass ratio 45：10：5） as flux, NH4NO3 as oxidant, LiBr as stripping agent. Several experimental parameters were optimized, and analytical figures of merit were evaluated. The components in certified reference material of GBW07105 ,GBW07401 were determined by the proposed method. The relative standard deviation （RSD, n = 12）was less than 2%, and the relative error （RE） was less than 5%. The proposed method was successfully applied to the determination of ultrabasic rock, silicate, stream sediment and soil standard sample, giving a result in consistence with the reference value.