熔融制样-X射线荧光光谱法测定含碳及碳化硅的铝镁质、锆质耐火材料中的7种氧化物  

Determination of Seven Oxides in Al-Mg and Zr Refractory Materials Containing Carbon and Silicon Carbide by X-Ray Fluorescence Spectrometry after Fusion Sample Preparation

作　　者：张琴 周雯闻 ZHANG Qin;ZHOU Wenwen(Zenith Steel Group Co.,Ltd.,Changzhou 213100,China)

机构地区：[1]中天钢铁集团有限公司,常州213100

出　　处：《理化检验（化学分册）》2021年第9期834-839,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：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 123μg·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.

关 键 词：熔融制样 X射线荧光光谱法 氧化物 含碳及碳化硅的铝镁质及锆质耐火材料 

分 类 号：O657.34[理学—分析化学]