摘要
在脉冲加热-红外吸收热导法测定钢铁材料中氧氮系列研究的基础上,通过对仪器分析气路的快速转换,实现了单台仪器快速测定氧氮和氢3种气体元素。实验主要对测氢的脉冲加热条件、助熔剂和坩埚的影响等进行考察,确定分析功率为2 300 W、加1片锡片助熔、使用套坩埚为氢测定的最佳分析条件。通过对氧、氮和氢标准样品的测定,建立了方法的校准曲线。利用对空白的标准偏差计算得氧氮和氢的检出限分别为0.000 027%、0.000 021%和0.000 015%,氧氮分析范围为0.000 09%~0.2%和0.000 07%~0.2%,氢的分析范围为0.000 05%~0.05%。对氧、氮和氢含量较低的钢标准样品进行精密度考察,结果的相对标准偏差(RSD,n=11)均小于5%;用于钢铁实际样品的测定结果与其他仪器所得结果一致,完全满足钢铁材料中气体元素的分析要求。
Based on the determination of oxygen and nitrogen in steel material by pulse heating-infrared absorption and thermal conductivity method,fast determination of oxygen,nitrogen and hydrogen was realized by individual instrument through fast switching of carrier gas.The effect of pulse heating condition,flux and crucible was mainly studied to determine the optimum analysis conditions,including 2 300 W of analysis power,adding 1tin sheet for fusion and the application of outer-inner crucible for determining hydrogen.Calibration curve was drawn by determining oxygen,nitrogen and hydrogen standard sample.By calculating the standard deviation of blank reagent,the detection limit of oxygen,nitrogen and hydrogen was obtained as 0.000 027%,0.000 021% and 0.000 015%,respectively.The analysis scope of oxygen,nitrogen and hydrogen was 0.000 09%-0.2% and 0.000 07%-0.2%;and the analysis scope of hydrogen was 0.000 05%-0.05%.Sample with low amount of oxygen,nitrogen and hydrogen was conducted with precision study,with RSD(n=11)of these three elements were less than 5%.The testing results of practical steel sample were consistent with those of other instrument,meeting the requirement of gas analysis in steel material.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第10期32-36,共5页
Metallurgical Analysis
关键词
脉冲加热
熔融
红外吸收法
热导法
钢铁
氧
氮
氢
pulse heating
fusion
infrared absorption method
thermal conductivity method
iron and steel
oxygen
nitrogen
hydrogen
