材料期刊网

采用熔融方法制样,建立了X射线荧光光谱法(XRF)分析铌铁中铌、钽、铜、钛、铝、磷6种元素含量的检测方法.采用氢氟酸和硝酸溶解试样的前处理方法,保证了溶解反应温和,有效避免了熔融过程中坩埚腐蚀的问题.选用铌铁标准物质,及向标准物质中添加单元素标准溶液和高纯五氧化二铌的方式合成铌铁校准样品系列,拓宽了校准曲线含量范围.实验表明,以四硼酸锂为熔剂,溴化锂为脱模剂,稀释比1∶30,在1 050 ℃下,熔融15 min,制得的玻璃片均匀、表面光滑、无气孔,符合测定要求.采用理论 α 系数和经验系数相结合的方法对样品的组成和含量变化引起的基体效应进行校正.精密度和准确度试验结果显示,各组分测定结果的相对标准偏差(RSD, n=10)为0.26%~1.0%,结果与铌铁标准物质的认定值相符,完全满足日常生产的需要.

A determination method of six elements including niobium, tantalum, copper, titanium, aluminum and phosphorus in ferro-niobium by X-ray fluorescence spectrometry (XRF) was established after sample was prepared with fusion method.The sample was pretreated with hydrofluoric acid and nitric acid.The dissolution reaction was mild, which effectively avoid the corrosion problem of crucible in sample fusion process.The series of ferro-niobium calibration sample composed by ferro-niobium certified reference materials, and the ferro-niobium synthetic samples which were mixed with these certified reference materials, the standard solution of single element and high-purity niobium pentoxide.The content range of calibration curve was broadened.Lithium tetraborate and lithium bromide was used as flux and releasing agent, respectively.The dilution ratio was 1∶30.After fusion at 1 050 ℃ for 15 min, the glass sheet was uniform and smooth without air holes on surface, which could meet the requirement for determination.The matrix effect caused by the change of composition and content of sample was corrected by theoretical α coefficient method combined with empirical coefficient method.The precision and accuracy results indicated that the relative standard deviations (RSD, n=10) of determination results of elements were between 0.26% and 1.0%.The results were consistent with the certified values of ferro-niobium certified reference material.The proposed method could meet the requirement for determination in routine production.