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100～11O℃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R^2=0．993。氮检出限为0．00006％，测定下限为0．0002％。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.
出处
《冶金分析》
CAS
CSCD
北大核心
2015年第11期54-57,共4页
Metallurgical Analysis
关键词
增碳剂
氮
脉冲加热惰气熔融-热导法
graphite recarburizer
nitrogen
pulse heating inert gas fusion-thermal conductivity method
