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应用Leco公司TCH600氧氮氢仪,脉冲加热-惰气熔融法对钽铌中氧、氮、氢量同时测定的分析条件进行试验和研究。试验结果表明,氧、氮、氢同时测定时的分析功率为4.6 k W;分析积分时间分别为40、70、45 sec;比较器水平分别为1.0%、1.0%、3.0%。在优化的条件下建立的氧、氮、氢校正曲线,线性好,相关系数均大于0.999 0;测定钛标、钢标、原冶金部行业铌粉中氧、氮、氢标准物质,其测定值与认证值相吻合;样品加标回收率在91.3%~105.0%之间;测定氧、氮、氢含量分别为0.004 8%、0.001 1%、0.000 5%的样品其相对标准偏差(RSD,n=5)分别为2.8%、10.4%、10.0%;氧、氮、氢的测定下限(5LOD)分别为0.001 0%、0.000 5%、0.000 5%。
The conditions for simultaneous determination of oxygen, nitrogen and hydrogen in tantalum and niobium were tested and studied by using Leco TCH600 oxygen-nitrogen analyzer and pulse heating-inert gas fusion method. The experimental results show that the analytical power of simultaneous determination of oxygen, nitrogen and hydrogen is 4.6 k W; the analysis integration time is 40, 70 and 45 sec respectively; the comparator levels are 1.0%, 1.0% and 3.0% respectively. The calibration curves of oxygen, nitrogen and hydrogen were established under optimized conditions with good linearity and the correlation coefficients were both greater than 0.999 0. The standard values of oxygen, nitrogen and hydrogen in niobium powders for titanium, steel, and metallurgical industries were determined. The measured values The recoveries of spiked samples ranged from 91.3% to 105.0%. The relative standard deviations (RSD, n (subscript n)) of samples with oxygen, nitrogen and hydrogen contents of 0.004 8%, 0.001 1% and 0.000 5% = 5) were 2.8%, 10.4% and 10.0% respectively. The lower limit of determination of oxygen, nitrogen and hydrogen was 0.001 0%, 0.000 5% and 0.000 5% respectively.