惰气熔融红外/热导法测定钽钨合金中氧和氮

通过锉刀锉去样品表面污物、丙酮清洗、自然风干方式对样品进行预处理,在高纯镍篮中加入样品,建立了惰气熔融红外/热导法测定钽钨合金中氧和氮含量的检测方法。探讨了助熔剂、分析功率、称样量等对试验结果的影响,实验选择在助熔剂为镍篮,分析功率为5.0 kW,称样量约为0.10 g的条件下进行。使用钛合金标样GBW(E)020188进行校准,以另一锆合金标样AR640进行验证,标样中氧和氮的测定结果分别在标准值范围之内。在优化的条件下进行测定,氧和氮的检出限分别为0.000 13%和0.000 04%,定量限分别为0.000 44%和0.000 13%。按照实验方法对钽钨合金进行分析,氧和氮测定结果的相对标准偏差(RSD,n=11)分别为6.6%和11.2%,加标回收率分别为93%～102%和95%～103%。

Determination of oxygen and nitrogen in tantalum-tungsten alloy by inert gas fusion infrared absorption-thermal conductivity method

The tantalum-tungsten alloy sample was pretreated by removing surface dirt with a file followed by rinsing with acetone and natural air drying. Then the sample was added into high purity nickel basket. The detection of oxygen and nitrogen in tantalum-tungsten alloy by inert gas fusion infrared absorption-thermal conductivity method was established. The effects of flux, analytical power and sample mass on the analysis results were discussed. The following experimental conditions were selected: the flux was nickel basket, the analytical power was 5.0 kW, and the sample mass was about 0.10 g. Titanium alloy standard sample GBW(E)020188 was used for calibration, and another zirconium alloy standard sample AR640 was used for verification. The determination results of oxygen and nitrogen in the standard sample were within the range of standard values. Under the optimized conditions, the limits of detection of oxygen and nitrogen were 0.000 13% and 0.000 04%, and the limits of quantification were 0.000 44% and 0.000 13%, respectively. The proposed method was applied for the analysis of tantalum-tungsten alloy. The relative standard deviations (RSD, n=11) of determination results of oxygen and nitrogen were 6.6% and 11.2%, respectively. The recoveries were 93%-102% and 95%-103%, respectively.