脉冲加热惰气熔融-热导法测定增碳剂中氮
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摘要
对脉冲加热惰气熔融-热导法测定增碳剂中氮含量的实验条件进行优化,确定增碳剂样品制备后必须在100~110℃烘箱中烘干,且对样品进行研磨后过120μm筛的样品处理方式;优化后仪器的分析功率设为4.5kW,且使用镍箔做助熔剂,样品中氮的释放比较完全。采用组成和结构与增碳剂很接近的煤标样绘制氮的校准曲线,线性相关系数R2=0.993。氮检出限为0.000 06%,测定下限为0.000 2%。对增碳剂样品进行精密度考察,结果的相对标准偏差(RSD,n=7)不大于3.4%;对实际样品进行测定,结果同脉冲熔融-飞行时间质谱法的测定结果一致。
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 120μm sieve.The optimized analytical power of instrument was 4.5kW.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.
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 120μm sieve.The optimized analytical power of instrument was 4.5kW.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.
引文
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[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 heatingtime of flight mass spectrometry[J].Metallurgical Analysis,2014,34(5):20-24.
[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.
[4]吴建民,孙印青,黄运杰.气相色谱法分析CrMnNSi钢中氮[J].河北冶金,2003(1):25-26.
[5]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.
[8]方南辉,张水菊,段清国,等.低氮增碳剂中氮的检测方法研究[J].江西冶金,2010,30(6):39-46.
[9]中华人民共和国国家质量监督检验检疫总局.GB/T11261-2006钢铁氮含量的测定脉冲加热惰气熔融-红外吸收法[S].北京:中国标准出版社,2006.
[10]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 heatingtime of flight mass spectrometry[J].Metallurgical Analysis,2014,34(5):20-24.