建立了熔融制样-X射线荧光光谱法（XRFS）测定火力发电厂烟气脱硫石膏中9种主次量元素（以元素氧化物形式表示）的方法，并用正交试验优化了熔融制样条件。将样品与四硼酸锂-偏硼酸锂混合熔剂（质量比12∶22）按1∶8的质量比混合，加入40 g·L^-1溴化锂溶液0.6 mL，在自动燃气熔样机上于1 050 ℃熔融4.5 min，冷却脱模后即得玻璃样片，在优化的XRFS条件下测定。采用硫酸钙、氧化钙、石膏成分分析标准物质和煤灰成分分析标准物质配制的标准样品系列制作校准曲线，并用理论α系数法校正基体效应。结果显示：9种主次量元素氧化物线性相关系数均大于0.990 0，检出限为0.006 4%~0.059 9%。方法用于2个烟气脱硫石膏样品的分析，2次平行测定值的差值均小于国家标准GB/T 5484-2012规定的重复性限，且测定值和GB/T 5484-2012的基本一致。

A method for the determination of 9 major and minor elements (in the form of element oxides) in flue gas desulfurization gypsum from fossil power plant by XRFS after fusion sample preparation was proposed, and fusion sample preparation conditions were optimized by orthogonal test. The sample was mixed with the mixed flux (m_Li2B4O7:m_LiBO2=12:22) at mass ratio of 1:8, then 0.6 mL of 40 g·L^-1 LiBr solution was added; the mixture was fused at 1 050 ℃ for 4.5 min in an auto sample fusion apparatus. After cooling and demoulding, a glassy slice of the sample was obtained and analyzed under the optimal conditions of XRFS. Reference material series were prepared by using calcium sulfate, calcium oxide, gypsum certified reference materials and coal ash certified reference materials for making calibration curves, and matrix effect was corrected by theoretical α coefficient method. As found by results that the linear correlation coefficients of oxides of 9 major and minor elements were all above 0.990 0, with detection limits in the range of 0.006 4%-0.059 9%. The proposed method was used for analyzing 2 samples of flue gas desulfurization gypsum, and the differences between the results of two parallel determinations were less than repeatability limits specified by the national standard of GB/T 5484-2012, with the determined results in consistency with those obtained by the national standard of GB/T 5484-2012.