Abstract：The experimental conditions for the determination of nitrogen content in recarburizer by pulse heating inert gas fusion-thermal conductivity method were optimized. It was found that the recarburizer samples must be dried in oven at 100-110 ℃ after preparation. Moreover, the samples after grinding should be treated with 120 μm sieve. The optimized analytical power of instrument was 4.5 kW. The nickel foil should be used as flux to fully release the nitrogen in sample. The standard coal sample with similar composition and structure to the recarburizer was used to plot the calibration curve of nitrogen. The linear correlation coefficient was R2=0.993. The detection limit of nitrogen was 0.000 06%. The low limit of determination was 0.000 2%. The precision test of recarburizer sample was conducted, and the relative standard deviation (RSD, n=7) was not more than 3.4%. The actual samples were determined by the proposed method, and the found results were consistent with those obtained by pulse fusion-time of flight mass spectrometry.
袁辉,孙雪涛,张祖辉.红外吸收法测定低氮低硫增碳剂中的全硫量 [J]. 化学工程师,2013(5):26-28. YUAN Hui , SUN Xue-tao, ZHANG Zu-hui. Determination of total sulfur in low nitrogen and sulfur carburant by high frequency-infrared absorption method [J]. Chemical Engineer, 2013(5):26-28.
[2]
张槐,陈天明.钢中氮含量控制的研究和探讨 [J]. 四川冶金,2009,31(1):7-11. ZHANG Huai, CHEN Tian-ming.Study and probing on controlling nitrogen content in liquid steel and steel strand [J].Sichuan Metallurgy, 2009,31(1):7-11.
[3]
孟小卫.Ti(C,N)中非化合氮的测定 [J]. 硬质合金,2001,18(1):35-38. MENG Xiao-wei.Determination of unreacted-nitrogen in the Ti(C,N) [J].Cemented Carbide,2001,18(1):35-38.
徐本平.脉冲加热-热导法测定钒氮合金中的高含量氮 [J]. 冶金分析,2004,24(6):49-51. XU Ben-ping. Determination of high content nitrogen in vanadium2nitrogen alloy by pulse-heating thermal conductivity [J].Metallurgical Analysis, 2004,24(6):49-51.
[6]
沈学静,王蓬,胡少成.脉冲熔融飞行时间质谱法测定金属材料中氧、氮、氢和氩 [J].分析化学,2011,39(10):1555- 1560. SHEN Xue-jing,WANG Peng, HU Shao-cheng.Simultaneous determination of oxygen,nitrogen,hydrogen and argon in metals by pulse heating and time of flight-mass spectrometric method [J]. Journal of Analytical Chemistry,2011, 39 (10):1555-1560.
[7]
胡少成,沈学静,王蓬,等.脉冲熔融-飞行时间质谱法测定铁材料中的氧、氮和氢 [J].冶金分析,2011,31(7):26-30. HU Shao-cheng,SHEN Xue-jing,WANG Peng,et al. Determination of oxygen, nitrogen and hydrogen in iron and steel by pulse melting-time-of-flight mass spectrometry [J].Metallurgical Analysis, 2011, 31(7) :26-30.
朱跃进,李素娟.惰气熔融法测定镁中氧、氢、氮 [J].冶金分析,2011,31(12):58-61.ZHU Yue-jin,LI Su-juan. Determination of oxygen, hydrogen and nitrogen in magnesium by inert gas fusion method [J]. Metallurgical Analysis, 2011, 31 (12) : 58-61.
[11]
王蓬, 杨帆, 李宏伟, 等.钒氮合金中高氮检测的新方法 [J].钢铁钒钛, 2005 ,26 (3):64-68.WANG Peng, YANG Fan, LI Hong-wei,et al.A new method to analyze nitrogen content of VN alloy [J].Iron Steel Vanadium Titanium,2005,26 (3) :64-68.
[12]
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 Wei-ru, ZHOU Hai-shou, 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.
