惰性气体熔融-热导／红外法同时测定钛合金中氧氮氢

Simultaneous determination of oxygen,nitrogen and hydrogen in titanium alloys by inert gas fusion-thermal conductivity/infrared method

以合适的钛合金标准样品绘制校准曲线，用惰性气体熔融-热导／红外法测定，建立了钛合金中氧、氮和氢的同时测定方法。确立了最佳实验条件：对于0．13～0．15g试样，镍篮助熔剂的用量为lg，分析功率为0．55kW。氧、氮和氢的线性范围分别为0．000l％～0．1％、0．000l％～0．01％和0．00005％～0．002％（质量分数），方法检出限分别为0．000045％、0．000061％和0．000018％（质量分数）。采用实验方法测定钛合金实际样品中氧、氮和氢，测定结果与国家标准方法（GB／T4698．7～201l和GB／T4698．15-2011）的测定结果基本一致，相对标准偏差（RSD，n=6）在0．14％～4．6％范围。

A method for simultaneous determination of oxygen,nitrogen and hydrogen in titanium alloy was established by inert gas fusion-thermal conductivity/infrared method.The calibration curve was plotted by use of appropriate standard samples of titanium alloy.Through testing,the optimal test condictions was determined:the amount of fluxing agent nickel basket was 1g for 0.13-0.15 g of sample and the analysis power was 0.55 kW.The linear ranges of oxygen,nitrogen and hydrogen were 0.000 1%-0.1%,0.000 1%-0.01% and 0.000 05%-0.002%(mass fraction),and their detection limits were 0.000 045%,0.000 061% and 0.000 018%(mass fraction),respectively.The experimental method has been applied to the determination of oxygen,nitrogen and hydrogen in practical titanium alloy,whose results were consistent with those of national standard method(GB/T4698.7-2011 and GB/T4698.15-2011),with relative standard deviation(RSD,n=6)within the range of 0.14 %-4.6 %.