X射线荧光光谱法测定钼铝合金中钼

Determination of molybdenum in molybdenum-aluminum alloy by X-ray fluorescence spectrometry

采用氢氟酸、硝酸溶解样品,溶液经红外灯烘干后,以四硼酸锂作熔剂,准确加入1.0mL 30mg/mL溴化锂溶液作脱模剂进行熔融制样,建立了X射线荧光光谱法测定钼铝合金中主量元素钼的方法。采用高纯三氧化二铝和三氧化钼通过熔融制样配制钼铝合金的校准样品并绘制校准曲线,利用理论α系数法进行基体效应的校正。选择Mo的Lα线作为分析线,测定结果不受样片厚度的影响。方法用于德国AlMo65标样和生产用AlMo60内控样的钼含量分析,测定结果与认定值或重量法测定值一致,相对标准偏差(n=7)不超过0.22%。

The sample was dissolved with hydrofluoric acid and nitric acid, and the solution was dried by infrared lamp. Then, the sample was prepared by fusion method with lithium tetraborate as flux and 1.0 mL of 30 mg/mL LiBr solution as releasing agent. Thus, a method for determination of mo- lybdenum （main element） in molybdenum-aluminum alloy was established by X-ray fluorescence spec- trometry. The high-purity aluminum oxide and molybdenum trioxide were fused to prepare the cali- bration samples for molybdenum-aluminum alloy, which were used to plot the calibration curve. The matrix effect was corrected by theoretical a coefficient method. The determination results were not af- fected by the thickness of sample with La line of Mo as the analytical line. The proposed method was applied to the determination of molybdenum in German certified reference material A1Mo65 and inter- nal control sample A1Mo65 for production. The results were consistent with the certified values or those obtained by gravimetric method. The relative standard deviation （RSD, n = 7） was not more than 0.22 %.