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本文对应用TCH600氧氮氢分析仪脉冲加热-红外吸收法测定钽、铌中氢量的提取功率、分析积分时间、积分延迟时间、比较器水平、称样量等主要分析参数进行了较详细的试验和研究,结果表明,上述最佳参数分别为45 s,10 s,1%,0.05~0.1g。采用原冶金部行业标准铌粉以及LECO公司钛标中的氢量建立校正曲线。以此建立的分析方法对氢标准物质和样品进行准确度、精密度试验,标准测定值与认定值相吻合,相对标准偏差RSD在2.0%~4.2%之间(n=5)。
In this paper, TCH600 oxynitride analyzer pulse heating - infrared absorption method for the determination of tantalum, niobium in hydrogen extraction power, analysis of integration time, integral delay time, the comparator level, sample size and other major analysis of the parameters of a more detailed The results showed that the optimum parameters mentioned above were 45 s, 10 s, 1% and 0.05 ~ 0.1 g, respectively. Using the original metallurgical industry standard niobium powder and LECO titanium standard in the establishment of the calibration curve of hydrogen. The analytical method established by this method was used to test the accuracy and precision of hydrogen standard materials and samples. The standard measured values were consistent with the certified values. The relative standard deviations (RSDs) ranged from 2.0% to 4.2% (n = 5).