摘要
在一次改造脉冲-热导氢测定仪的基础上,进行二次改造使其具备程序升温功能,应用两次改造后的不同组合,开展了金属中氦和氢热释放的研究。实验结果表明:金属中氦的热释放符合固溶态气体的释放特征,氦在样品熔点附近快速释放,未见高温分解的化合物峰;金属中氢提取未见缓慢热释放图谱,说明氢在固体中的扩散和迁移相对缓慢,固溶态的氢在样品熔点附近快速释放。两种仪器两次改造组合的分析发现脉冲热导法无法区分氦和氢,氦和氢同时释放构成同一个峰,因此,富氦样品必须应用脉冲红外等其他方法定氢,才能确保氢分析的准确性。由于日常普通样品贫氦,考察了7种普通金属中氦含量,探明其值均小于仪器检测限,不会影响到氢的定量分析结果。
On the basis of first transformation of impulse-thermal conductivity hydrogen analyzer, its secondary transformation was performed to make it have the temperature programming function. By use of different combinations of the two transformed analyzers , the release of helium and hydrogen in metal was investigated. The results showed that the heat release of helium in metals accorded with the release characteristics of solid solution gases. The release of helium was rapid near the melting point of sample and the peaks of compound decomposed under high temperature did not appear. The slow heat release spectrum for extracting hydrogen in metal was not found, indicating that the diffusion and migration of hydrogen in solid was relatively slow. The release of hydrogen in solid solution state was rapid near the melting point. The analysis by the combination of two instruments after twice transformation showed that the impulse-thermal conductivity method could not separate helium from hydrogen. The helium and hydrogen released simultaneously to form one peak. Therefore, the hydrogen in rich helium sample should be determined by other methods such as pulse infrared to guarantee the accuracy. However, the content of helium in common samples was lower. The content of helium in seven common metals was determined. The results were all lower than the detection limit, so the quantitative analysis of hydrogen was not affected.
出处
《冶金分析》
CAS
CSCD
北大核心
2009年第6期28-31,共4页
Metallurgical Analysis
基金
沈阳市科技局2006年资助项目(06M3831)
关键词
脉冲加热
程序升温
氦
氢
释放
脉冲热导法
脉冲红外法
impulse heating
programmed temperature
helium
hydrogen
release
impulse-thermal conductivity method
impulse infrared method
