钢中氧氮氢同时测定方法中氢空白值的控制  

Control of hydrogen blank value in simultaneous determination of oxygen,nitrogen and hydrogen in steel

作　　者：钟华[1] 

机构地区：[1]攀钢集团研究院有限公司、钒钛资源综合利用国家重点实验室,四川攀枝花617000

出　　处：《冶金分析》2016年第5期12-15,共4页Metallurgical Analysis

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45O～480℃加热处理48h用于日常分析，分析系统的氢空白值从O．69μg／g降低至O．12μg／g，同时提高了方法的精密度，11次空白值的标准偏差为O．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．O％～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.

关 键 词：氧 氮 氢 钢 氢空白值 石墨坩埚 预处理 

分 类 号：TF701.3[冶金工程—钢铁冶金]