X射线荧光光谱法测定煤灰成分的改进

Modification of the Method of Componental Analysis of Coal Ash by XRFS

样品以四硼酸锂和偏硼酸锂为熔剂,硝酸铵为氧化剂,溴化锂为脱模剂,采用玻璃状熔片法制样。选用标准样品及其标准样品间相混合配制的混合样品制作工作曲线,并以α系数和经验系数法校正元素谱线干扰和基体效应,用X射线荧光光谱法对煤灰中的二氧化硅、氧化铝、氧化铁、氧化钙、氧化镁、五氧化二磷、氧化钾、氧化钠、氧化钛、五氧化二钒、氧化锰和三氧化硫等12种主次组分进行测定。方法分析结果与化学法和电感耦合等离子体原子发射光谱法测定值相符;对同一样品按所建方法分别熔融制备10个熔片进行测定,各组分测定值的相对标准偏差(n=10)在0.06%～2.4%之间。

Twelve components （i. e. , SiO2, Al2O3, Fe2O3, CaO, MgO, P2O5, K2O, Na2O, TiO2, V2O5, MnO and SO3 ） in coal ash were determined by XRFS. The glassy melt of sample of coal ash was obtained by fusion with Li2B4O7 and LiBO2 as flax, NH4 NO3 as oxidant and LiBr as demoulding agent. Standard working curves were prepared by using standard samples and mixtures of standard samples. Interferences due to matrix effects and overlapping of spectral lines were overcomed by the methods of a-coefficient and empirical coefficient. Results of 12 components obtained by the present method were found to check quite well with those obtained by chemical method and ICP-AES. Ten glassy melts were prepared from the same sample of coal ash and the 12 components were determined by the present method, values of RSD＇s （n=10） found were in the range of 0. 06%-2.4%.