金属中气体元素分析典型案例  

Typical case study on analysis of gaseous element in metal

作　　者：朱跃进[1] 朱瑛才[1] ZHU Yuejin;ZHU Yingcai(Institute of Metal Research,Chinese Academy of Sciences,Shenyang 110016,China)

机构地区：[1]中国科学院金属研究所,辽宁沈阳110016

出　　处：《冶金分析》2022年第1期1-9,共9页Metallurgical Analysis

摘　　要：金属中气体元素分析已经存在60余年,其检测方法不同于其他化学元素。论文列举5个典型案例(铝中氢、金属中氩、金属中氦、稀土钢中氢、(铝)镁中氧),以进行技术交流和讨论。铝中氢作为金属中气体分析之最难当之无愧,有研究尝试简化铝中氢分析方法,期望像钢样那样快速准确地得到结果,比如应用现有通用的脉冲熔融法反复试验上百次,未能成功,改用高频(或管式炉)热抽取法后,才做到测试铝中氢与钢中氢同样简单。借助于脉冲质谱法定氩(联测)仪建立了金属中氩可靠的分析方法,该方法已应用10余年。金属中氦的测定通过自行研制快速接口附件,在现用的定氢仪上完成。稀土钢中氢分析出现"零峰值"现象,国内3家资深单位3台仪器上全都不出氢峰。理论上分析是稀土影响,通过对比熔融法和抽取法,提供稀土干扰钢中氢分析的证据,应用热抽取法样品不熔可将稀土污染的干扰降至最低,得到稀土钢中氢峰。镁的化学活性强,脉冲熔融法测定镁中氧的过程中挥发污染干扰极其严重,尝试过用此类仪器分析镁中氧含量,最终达到国内出关数据与国外入关数据一致,此后专机专用并执行专属技术方案,解决了镁中氧检测的难题。The analytical method of gaseous elements in metal has already existed for more than 6 years. The detection methods are different from those for other chemical elements. Five typical cases(hydrogen in aluminum, argon in metal, helium in metal, hydrogen in rare earth steel, and oxygen in aluminum or magnesium) were listed for technical exchange and discussion. Among the analysis of gases in metals, the analysis of hydrogen in aluminum is the most difficult. Some researchers tried to simplify the analysis method of hydrogen in aluminum. It was expected to obtain the results rapidly and accurately like that in steel. For example, the commonly used impulse fusion method was tested a hundred times, but it was not successful. Then high frequency(or tubular furnace) heating extraction was adopted, which made the testing of hydrogen in aluminum simple like that of hydrogen in steel. With the aid of legal argon co-detector by impulse mass spectrometry, the reliable analysis method of argon in metal was established. The proposed method has been used for more than ten years. For the determination of helium in metal, the fast interface attachment were usually self-developed and the testing was conducted in the existing hydrogen determinator. The phenomenon of "zero peak value" occurred in the analysis of hydrogen in rare earth steel. The peak of hydrogen was not observed in three instruments from three domestic senior departments. Theoretically, it was due to the influence of rare earths. The fusion method and extraction method were compared to provide the evidence that the analysis of hydrogen in steel was interfered by rare earths. The sample was not melted in thermal extraction method, thus reducing the interference of rare earth pollution to the minimum level, and the peak of hydrogen in rare earth steel could be obtained. The chemical activity of magnesium was strong. During the determination of oxygen in magnesium by impulse fusion method, the interference of volatile pollution was very serious. Some researchers tried

关 键 词：铝中氢 金属中氩 金属中氦 稀土钢中氢 镁中氧 脉冲熔融法 高频热抽取法 

分 类 号：O659.2[理学—分析化学] TF82[理学—化学]