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机构地区:[1]沈阳产品质量监督检验院,沈阳110022 [2]沈阳黎明发动机公司技术中心,沈阳110043
出 处:《理化检验(化学分册)》2016年第10期1218-1222,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:应用X射线荧光光谱法测定了镍基、钴基和铁基合金中质量分数在0.1%~8.50%范围内钽的含量。综合考虑,选择钽元素的Lβ1线作为分析谱线,并选择背景位置2θ为39.50°。在上述3类合金中常含有的铌(其Kβ1线)、铪(其Lβ2线)和钨(其Lβ4线)与钽的Lβ1线有重叠干扰,影响钽的测定。用合适的标准样品分别计算出上述3种元素对钽的重叠干扰系数K,并借助仪器的FP-工作软件用基本参数法消除这3种元素对钽测定的干扰。用所提出的方法分析了钽质量分数在0.015%~4.81%之间的11个标准样品或已知样品,测定结果与认定值或已知值相符。其中2个样品测定值的相对标准偏差(n=7)分别为0.46%(wTa=4.278%)和9.9%(wTa=0.020%)。XRFS was applied to the determination of tantalum (wTa 0.1%-8.50%) in nickel, cobalt and iron based alloys. Through comprehensive consideration, the spectral line of Lβ1 of Ta was chosen as analytical spectral line, and background site of 2θ of 39.50° was selected. Three common alloying elements (i.e. Nb, Hf and W) commonly present in the 3 kinds of alloys were found to interfere the determination of Ta by overlap of their spectral lines of Kβ1 (of Nb), Lβ2 (of Hf) and Lβ4 (of W) with the Lβ1 of Ta chosen for the determination. On the base of values of overlap interfering coefficient K of the 3 elements found by using appropriate standard samples, and by using the FP method with help of the FP-software, the above mentioned interferences were eliminated. 11 standard or known samples were analyzed by the proposed method for their Ta contents ranging from wTa 0.015%-4.81%, the results found were in consistency with the certified values or known values. Test for precision was made on 2 of the 11 samples, giving values of RSD′s (n=7) of 0.46% (wTa=4.278%) and 9.9% (wTa=0.020%).
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