钢中氧氮氢同时测定方法中氢空白值的控制
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摘要
针对钢中氧、氮、氢同时测定方法中氢测定结果较低温测氢法异常偏高的问题,进行了原因分析并提出了解决的办法。通过比较氢含量极低钢样的两种测定方法的氢结果,得出氧、氮、氢同时测定方法中石墨坩埚的氢杂质是造成上述问题的主要原因。为降低石墨坩埚中的氢杂质,实验提出将坩埚于450~480℃加热处理48h用于日常分析,分析系统的氢空白值从0.69μg/g降低至0.12μg/g,同时提高了方法的精密度,11次空白值的标准偏差为0.06μg/g。按实验提出的方法对氢空白进行控制后,钢中氧、氮、氢同时测定方法中氢的分析结果与低温单独测氢法一致;钢中1.2~6.8μg/g的氢测定结果,相对标准偏差(RSD,n=5)在1.0%~12.2%,满足炼钢炉前分析的要求。
During the simultaneous determination of oxygen,nitrogen and hydrogen in steel,the found results of hydrogen was abnormally higher than those obtained by low temperature hydrogen measurement method.The cause was analyzed and the solution was proposed.The steel sample with very low content of hydrogen was determined by these two methods.The results indicated that the hydrogen impurity in graphite crucible was the main reason to cause the problem above during the simultaneous determination of oxygen,nitrogen and hydrogen.In order to reduce the hydrogen impurity in graphite crucible,the crucible was thermally treated at 450-480℃for 48 hbefore routine analysis.The blank value of hydrogen in analysis system was reduced from 0.69μg/g to 0.12μg/g.Meanwhile,the precision of method was also improved.The standard deviation of blank value(n=11)was 0.06μg/g.The hydrogen blank was controlled using the experimental method,and the analysis results of hydrogen during simultaneous determination of oxygen,nitrogen and hydrogen in steel were consistent with those obtained by low temperature hydrogen measurement method.When the hydrogen content in steel was in range of 1.2-6.8μg/g,the relative standard deviations(RSD,n=5)were between 1.0% and 12.2%,which could meet the requirements of ladle analysis.
During the simultaneous determination of oxygen,nitrogen and hydrogen in steel,the found results of hydrogen was abnormally higher than those obtained by low temperature hydrogen measurement method.The cause was analyzed and the solution was proposed.The steel sample with very low content of hydrogen was determined by these two methods.The results indicated that the hydrogen impurity in graphite crucible was the main reason to cause the problem above during the simultaneous determination of oxygen,nitrogen and hydrogen.In order to reduce the hydrogen impurity in graphite crucible,the crucible was thermally treated at 450-480℃for 48 hbefore routine analysis.The blank value of hydrogen in analysis system was reduced from 0.69μg/g to 0.12μg/g.Meanwhile,the precision of method was also improved.The standard deviation of blank value(n=11)was 0.06μg/g.The hydrogen blank was controlled using the experimental method,and the analysis results of hydrogen during simultaneous determination of oxygen,nitrogen and hydrogen in steel were consistent with those obtained by low temperature hydrogen measurement method.When the hydrogen content in steel was in range of 1.2-6.8μg/g,the relative standard deviations(RSD,n=5)were between 1.0% and 12.2%,which could meet the requirements of ladle analysis.
引文
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[2]王仪康,李培基,冼爱平,等.重轨钢除氢工艺探讨[J].钢铁,1993,28(1):56-63.WANG Yi-kang,LI Pei-ji,XIAN Ai-ping,et al.Surery on hydrogen removal technique for heavy rail steel[J].Iron and steel,1993,28(1):56-63.
[3]李培基,冼爱平,王仪康,等.U71Mn重轨钢中的白点与含氢量[J].金属学报,1992,28(10):445-447.LI Pei-ji,XIAN Ai-ping,WANG Yi-kang,er al.Flakes and hydrogen content in U71Mn heavy rail steel[J].Acta Metallurgica Sinica,1992,28(10):445-447.
[4]Nonhlangabezo Mabho,Karin Bergers,Jorg Flock,et al.Determination of diffusible and total hydrogen concentration in coated and uncoated steel using melt and solid extraction techniques[J].Talanta Part I,2010,82:1298-1305.
[5]王蓬,王海舟.金属中氢的分析技术进展[J].冶金分析,2007,27(3):37-44.WANG Peng,WANG Hai-zhou.Recent progress in analytical technologies of hydrogen in metal[J].Metallurgical Analysis,2007,27(3):37-44.
[6]朱跃进.金属中气体分析现状与未来[J].冶金分析,2014,34(3):19-23.ZHU Yue-jin.The status quo and prospect of gas analysis in metal[J].Metallurgical Analysis,2014,34(3):19-23.
[7]唐权民,张祖辉,王文焱.TCH-600氧、氮、氢分析仪在唐钢的应用[J].光谱实验室,2006,23(3):503-505.TANG Quan-min,ZHANG Zu-hui,WANG Wen-yan.Technical character of TCH-600 O,N and H analyzer and its comprehension application[J].Chinese Journal of Spectroscopy Laboratory,2006,23(3):503-505.
[8]何永年,林文泉.轴承钢中氧和氮的测定[J].冶金分析(Metallurgical Analysis),1989,9(5):38-41.
[9]张长均,王蓬,黄小峰,等.氧氮氢气体分析仪的石墨坩埚升温过程研究[J].冶金分析,2010,30(11):71-73.ZHANG Chang-jun,WANG Peng,HUANG Xiao-feng,et al.Research on temperature process of graphite crucible in oxygen,nitrogen and hydrogen analyzer[J].Metallurgical Analysis,2010,30(11):71-73.
[10]朱跃进,李素娟,邓羽,等.金属中氧氮氢联测技术的应用[J].冶金分析(Metallurgical Analysis),2008,28(增2):1024-1026.