脉冲加热-惰气熔融法同时测定钽、铌中氧、氮、氢量
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摘要
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%。
Using TCH600 Oxygen/Nitrogen/Hydrogen Determinator produced by Leco Corporation, the analysis conditions of pulse heating inert gas fusion method for simultaneous measurement of oxygen, nitrogen and hydrogen contents in tantalum and niobium were tested. The experimental result shows that choosing the analysis power of 4.6 k W, the integral time of 40 s, 70 s and 45 s, the level of comparator of 1.0%, 1.0% and 3.0%, the three elements can be simultaneously measured. In this case the calibration curve established for oxygen, nitrogen and hydrogen measurement has good linearity.The correlation coefficient is greater than 0.999 0. The measured values of the oxygen, nitrogen and hydrogen contents in the standard niobium powder materials used in titanium industry, steel industry and the industry managed by original Ministry of Metallurgical Industry accord with the certified values. All the sample recovery rates are between 91.3% ~105%. When the measured contents of oxygen, nitrogen and hydrogen are 0.004 8%, 0.001 1% and 0.000 5%, the relative standard deviations(RSD, n=5) of the samples are 2.8%, 10.4% and 10.0%, respectively. The detection limits(5LOD) for oxygen, nitrogen and hydrogen are 0.001 0%, 0.000 5% and 0.000 5%.
Using TCH600 Oxygen/Nitrogen/Hydrogen Determinator produced by Leco Corporation, the analysis conditions of pulse heating inert gas fusion method for simultaneous measurement of oxygen, nitrogen and hydrogen contents in tantalum and niobium were tested. The experimental result shows that choosing the analysis power of 4.6 k W, the integral time of 40 s, 70 s and 45 s, the level of comparator of 1.0%, 1.0% and 3.0%, the three elements can be simultaneously measured. In this case the calibration curve established for oxygen, nitrogen and hydrogen measurement has good linearity.The correlation coefficient is greater than 0.999 0. The measured values of the oxygen, nitrogen and hydrogen contents in the standard niobium powder materials used in titanium industry, steel industry and the industry managed by original Ministry of Metallurgical Industry accord with the certified values. All the sample recovery rates are between 91.3% ~105%. When the measured contents of oxygen, nitrogen and hydrogen are 0.004 8%, 0.001 1% and 0.000 5%, the relative standard deviations(RSD, n=5) of the samples are 2.8%, 10.4% and 10.0%, respectively. The detection limits(5LOD) for oxygen, nitrogen and hydrogen are 0.001 0%, 0.000 5% and 0.000 5%.
引文
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[2]裘立奋,王水法.硬质材料和难熔金属气体分析进展[J].硬质合金,1999,16(2):109-113.Qiu Lifen,Wang Shuifa.The development of gas-analysis in hard materials and refractory metals[J].Cemented Carbide,1999,16(2):109-113.
[3]王剑秋,钱铭,周海收,等.脉冲惰气熔化法同时测定金属中的氧氮[J].分析实验室,1998,17(5):75-77.Wang Jiangqiu,Qiang Ming,Zhou Haishou,et al.Determinating oxygen and nitrogen simultaneously in metals with impulse inert gas fusion method[J].Analytical Laboratory,1998,17(5):75-77.
[4]林文泉,何永年.铌合金中氧及氮的同时测定[J].钢铁研究总院学报,1988,8(3):91.Lin Wenquan,He Yongnian.Simultaneous determination of oxygen and nitrogen in niobium alloy[J].Journal of Iron and Steel Research,1998,8(3):91.
[5]石新层,周凯,杨军红.惰气熔融-红外热导法同时测定铌钛合金中氧和氮[J].冶金分析,2010,30(12):30-32.Shi Xinceng,Zhou Kai,Yang Junhong.Simultaneous determination of oxygen and nitrogen in Nb Ti alloy with inert gas fusion-infrared and thermal conductivity method[J].Metallurgical Analysis,2010,30(12):30-32.
[6]方卫,刘伟,杨玉芳.高温钛合金粉中氧氮的同时测定[J].分析试验室,2001,20(6):94-95.Fang Wei,Liu Wei,Yang Yufang.Simultaneous determination of oxygen and nitrogen in titanium alloy powder[J].Chinese Journal of Analysis Laboratory,2001,20(6):94-95.
[7]何雄杰.钛及钛合金中氧和氢的联合测定[J].钛工业进展,2006,23(1):32-34.He Xiongjie.Simultaneous determination of oxygen and hydiogen in titanium and its alloys[J].Titanium Industry Progress,2006,23(1):32-34.
[8]韩维儒,周海收,陈然,等.脉冲熔融-飞行时间质谱法同时测定钨和钽中氧氮氢[J].冶金分析,2014,34(5):20-24.Han Weiru,Zhou Haishou,Chen Ran,et al.Simultaneous determination of oxygen,nitrogen and hydrogen in tungsten and tantalum by pulse heating-time of flight mass spectrometry[J].Metallurgical Analysis,2014,34(5):20-24.
[9]靳晓珠.氧氮分析影响因素探讨[J].广西科学院学报,2006,22(1):499-501.Jin Xiaozhu.Discussion on influence factors of nitrogen and oxygen determination[J].Journal of Guangxi Academy of Sciences,2006,22(1):499-501.
[10]Leco公司.TCH600氧氮氢分析仪说明书[M].Leco Corporation.TCH600 Oxygen/Nitroge/Nydrogen Determinator instruction manual[M].
[11]蒋亚芳,张杰,苏兴智.脉冲加热-红外法测定钽、铌中氢量[J].硬质合金,2010,27(6):376-379.Jiang Yafang,Zhang Jie,Su Xingzhi.Measurement of hydrogen content in tantalum and niobium by pulse heating-infrared absorption method[J].Cemented Carbide,2010,27(6):376-379.
[12]胡少成,沈学静,王蓬.固态金属及合金材料中氧、氮、氢联测技术进展[J].冶金分析,2009,29(11):34-40.Hu Shaocheng,Shen Xuejing,Wang Peng.Development of simultaneous analysis technique for oxygen,nitrogen and hydrogen in solid metals and alloys[J].Metallurgical Analysis,2009,29(11):34-40.