摘要
使用美国力可公司ONH836分析仪对钽丝、钽条、钽锭中氧氮氢量的测定方法进行探讨和研究,对样品中氧氮氢的释放功率、称样量等进行试验。确定测定钽丝、钽条、钽锭中氧、氮、氢量的最佳分析条件:分析功率4.8 kW;氧氮氢分析积分时间分别为40、70、50 s;称样量在0.10~0.15 g之间。在优化的条件下建立氧、氮、氢校正曲线,线性好,相关系数γ均大于0.999 0;测定钛标、钢标中氧、氮、氢标准物质,其测定值与认证值相吻合;测定氧、氮、氢质量分数分别为0.016%、0.002 6%、0.000 5%的样品其相对标准偏差RSD(n=11)分别为5.8%、8.0%、18.4%;并计算了测定的重复限性;确定氧、氮、氢的测定下限(5LOD)分别为0.001 0%、0.000 5%、0.000 5%。方法的准确度和精密度较好。
The ditermination of the contents of oxygen, nitrogen and hydrogen in tantalum wire, tantalum strip and tantalum ingot were discussed and researched by using ONH836 analyzer from Leco Corporation. The release power and the sample weight for the determination of the contents of oxygen, nitrogen and hydrogen were explored. The optimal analysis condition for the determination of the contents of oxygen, nitrogen and hydrogen in this research were confirmed that, the sample weight of 0.10~0.15 g, the analysis power of 4.8 kW and the integral time of 40 s, 70 sand 50 s, repectively. The optimized calibration curves with good linearity for the determination of nitrogen, hydrogen and oxygen were established, the correlation coefficients were all greater than 0.999 0. The measured values of the contents oxygen, nitrogen, and hydrogen in the standard materials of titanium and steel were in conformity with the certified values. When measured values of the contents of oxygen, nitrogen and hydrogen were 0.016%, 0.002 6% and 0.000 5%, the relative standard deviation（RSD, n=11） were 5.8%, 8.0% and 18.4%, respectively. The limits of determination（LOD） for oxygen, nitrogen and hydrogen were 0.001 0%, 0.000 5% and 0.000 5%. The result shows that the precision and accuracy of the method are high.
作者
蒋亚芳
Jiang Yafang(Zhuzhou Cemented Carbide Group Corp. Ltd., Zhuzhou Hunan 412000, China;State Key Laboratory of Cemented Carbide, Zhuzhou Hunan 412000, China;Laboratory of Industrial Product （Cemented Carbide and Tungsten Products） Quality Control and Technical Evaluation, Zhuzhou Hunan 412000, China)
出处
《硬质合金》
CAS
2017年第6期429-435,共7页
Cemented Carbides
关键词
ONH836分析仪
钽丝
钽锭
钽条
氧
氮
氢
ONH836 analyzer, tantalum wire
tantalum strip
tantalum ingot
oxygen
nitrogen hydrogen
