建立了熔融制样-X射线荧光光谱法（XRFS）测定含碳及碳化硅的铝镁质、锆质耐火材料中的二氧化锆、三氧化二铝、二氧化硅、氧化钙、氧化镁、三氧化二铁、二氧化钛等含量的方法。将样品置于950 ℃马弗炉内灼烧1 h以除去其中的碳。将四硼酸锂置于铂-金坩埚中熔融，旋转坩埚使熔融态四硼酸锂附着在坩埚壁上，以减少碳化硅对铂-金坩埚的腐蚀。将1.000 0 g碳酸锂、1.000 0 g硝酸锂和0.300 0 g灼烧过的样品混合，置于挂膜处理好的铂-金坩埚中，上面再覆盖2.000 0 g四硼酸锂，在程序升温条件下预氧化以去除样品中的碳化硅。加入溴化锂溶液（脱模剂），在1 120 ℃下熔融20 min，浇入铂-金成型模具中，制成玻璃样片，供XRFS分析。结果显示：7种氧化物的线性相关系数不小于0.999 0，检出限为28~15 123 μg·g^-1；对实际样品重复测定8次，7种氧化物测定值的相对标准偏差均小于4.0%；将方法所得结果与GB/T 16555-2017中化学湿法的进行比较，偏差基本在国家标准方法允许偏差的范围内。

A method for the determination of contents of zirconium dioxide, aluminium oxide, silica, calcium oxide, magnesium oxide, ferricoxide and titanium dioxide in Al-Mg and Zr refractory materials containing carbon and silicon carbide by X-ray fluorescence spectrometry (XRFS) was established. The sample was burned in a muffle furnace at 950 ℃ for 1 h to remove carbon. Lithium tetraborate was fused in a Pt-Au crucible, and the molten lithium tetraborate was adhered to the crucible wall by rotating the crucible to reduce the corrosion of the Pt-Au crucible by silicon carbide. The mixture of lithium carbonate (1.000 0 g), lithium nitrate (1.000 0 g) and calcined sample (0.300 0 g) were placed in the crucible prepared by film-forming process, and the mixture was covered with 2.000 0 g of lithium tetraborate, and preoxidized under temperature programmed condition to remove silicon carbide from the sample. Lithium bromide solution (releasing agent) was added, and the mixture was fused at 1 120 ℃ for 20 min, poured into the Pt-Au formin mould, and the glassy slice of sample obtained was used for analysis by XRFS. The results showed that the correlation coefficients of the 7 oxides were not less than 0.999 0, with detection limits in the range of 28-15 123 μg·g^-1. The prescribed method was used for eight repeated analysis of actual samples, giving RSDs of the determined values less than 4.0%. The method was compared with wet chemical method given by GB/T 16555-2017, and the deviation was basically within the allowable deviation range of the national standard method.