惰气熔融-红外吸收法测定钽钨合金中氢

通过对助熔剂、称样量、分析功率和积分时间的研究,建立了惰气熔融-红外吸收法测定钽钨合金中氢含量的方法。实验结果表明,称取0.15 g钽钨合金样品,放入镍囊,投入脱气后的石墨套坩埚中,设置分析功率为4 000 W,积分时间为60 s,可实现惰气熔融-红外吸收法对钽钨合金中氢含量的测定。方法检出限为0.000 03%,定量限为0.000 1%。将实验方法应用于钽钨合金样品中氢含量的测定,结果的相对标准偏差(RSD,n=11)为16.5%。按照实验方法对另一钽钨合金样品中氢含量进行测定,并加入适量钛标样GBW(E)020187进行加标回收试验,得加标回收率为94%~101%。

Determination of hydrogen in tantalum-tungsten alloy by inert gas fusion-infrared absorption method

A method for the determination of hydrogen content in tantalum-tungsten alloy by inert gas fusion-infrared absorption was established. The flux,sample mass, analytical power and integral time were optimized. The experimental results showed that the content of hydrogen in tantalum-tungsten alloy could be determined by inert gas fusion-infrared absorption method under the following conditions: 0.15 g of tantalum-tungsten alloy sample was transferred into nickel capsules, and then put into graphite crucible after degassing; the analytical power was controlled at 4 000 W; the integral time was 60 s. The limit of detection and limit of quantification was 0.000 03% and 0.000 1%, respectively. The proposed method was applied for the determination of hydrogen content in tantalum-tungsten alloy sample, and the relative standard deviation (RSD, n=11) of determination results was 16.5%. The content of hydrogen in another tantalum-tungsten alloy sample was determined according to the experimental method. Proper amount of titanium standard sample (GBW(E)020187) was added for the recovery test. The recoveries were between 94% and 101%.