为解决惰性气体氩分析困难及氩分析参考物质稀缺的问题,自制了标准气体校准装置,并配制了不同体积的定量管,利用标气注入接口通入标准气体进行仪器的校准,建立了脉冲惰气熔融-质谱法测定钛合金及纳米合金粉中氩的分析方法.结果表明,氩的绝对质量和Ar+(m/z=40)谱线的离子计数呈良好的线性关系,方法线性范围为0.000010%~0.10%,检出限为0.000006%.方法用于钛合金和纳米合金粉中氩的测定,测得结果与脉冲熔融热导法测得值或理论计算值一致,相对标准偏差均小于14%.%To overcome the difficults of the analysis of inert gas argon and the scarcity of argon reference materials, a kind of standard gas calibration device was designed and quantitative pipes of different volumes were prepared to conduct calibration by feeding standard gas through standard gas injection interface. Simultaneously, a novel determination method of argon in titanium alloy and nano-alloy powder was established by pulse inert gas fusion-mass spectrometry. The results indicated that the absolute quality of argon showed good linear relationship with ion count of Ar+ (m/z = 40) spectral line. The linear range was 0. 000 010%-0. 10% and the detection limit was 0. 000 006%. This proposed method was applied to the determination of argon in titanium alloy and nano-alloy powder. The results were consistent with those obtained by pulse fusion thermal conductivity method or theoretical calculated value, and the relative standard deviations were all less than 14%.
展开▼