脱氮热导法测定钛中氩

Determination of argon in titanium by nitrogen-removing thermal conductivity

钛及其合金对气体元素溶解度高,氩作为保护性气体在钛基材料制备过程中可能进入钛材料从而对其性能产生影响。实验将自制脱氮快速转换装置应用于现有的脉冲热导气体分析仪,转换装置脱氮效率高达97%以上,氮的干扰可量化、可排除,从而实现了钛中氩的准确测定。脱氮热导-程序升温法确定钛中氩可以在1 400℃完全释放,氩为非化合态。将脱氮热导法与色谱热导法及飞行时间质谱法对比,氩测定结果一致,因此,脱氮热导法可作为主要参比方法,辅助飞行时间质谱法同时测定金属中氢、氧、氮和氩的新方法建立和完善。

Titanium and its alloy have high solubility to gas elements. As protective gas, argon may dissolve in titanium materials during the preparation of titanium-based materials and exerted impact on their properties. A self-made nitrogen-removing device was configured onto an existing impulse thermal conductivity gas analyzer, which could realize nitrogen-removing efficiency over 97%. Since the interference of nitrogen could be quantified and removed, accurate determination of argon in titanium was achieved. It was determined through nitrogen-removing thermal conductivity-programmed temperature method that argon in titanium could be completely released at 1 400 ℃ and argon existed in non-compound state. The determination results were consistent with those by chromatographic thermal conductivity method and time-of-flight mass spectrometry. The proposed method could provide as reference method in the establishment and perfection of the simultaneous determination of hydrogen, oxygen, nitrogen and argon by time-of-flight mass spectrometry.