惰气熔融-红外/热导法同时测定锆合金中氧和氮

测定锆合金中氧和氮的方法多为单独测定,操作繁琐,故实验提出了锆合金中氧和氮同时测定的方法。称取0.06g锆合金样品,放入镍篮,投入脱气后的石墨套坩埚中,控制分析功率为5.0kW,氧和氮积分时间分别为40s和60s,以锆合金标样AR640建立校准曲线,实现了惰气熔融-红外/热导法对锆合金中氧和氮含量的同时测定。氧和氮的方法测定下限分别为0.000 7%和0.000 2%。采用实验方法对2个锆合金实际样品中氧和氮进行测定,氧和氮测定结果的相对标准偏差(RSD,n=11)分别为1.5%~4.4%和7.6%~8.6%。按照实验方法测定锆合金标样BCR-276中氧和氮,测定结果与认定值基本一致。

Simultaneous determination of oxygen and nitrogen in zirconium alloy byinert gas fusion-infrared and thermal conductivity method

Oxygen and nitrogen in zirconium alloy is singly determined in most methods, so the operation is very complicated. The simultaneous determination of oxygen and nitrogen in zirconium alloy was proposed. 0.06 g of zirconium alloy sample was put into nickel basket, which was then transferred into graphite duplex crucible.The analytical power was controlled at 5.0 kW. The integral time for oxygen and nitrogen was 40 s and 60 s, respectively. The calibration curve was established using zirconium alloy standard sample AR640, realizing the simultaneous determination of oxygen and nitrogen in zirconium alloy by inert gas fusion-infrared and thermal conductivity method. The low limit of determination for oxygen and nitrogen was 0.000 7% and 0.000 2%, respectively. The proposed method was applied to the determination of oxygen and nitrogen in two actual zirconium alloys. The relative standard deviations (RSD, n=11) for oxygen and nitrogen were 1.5%-4.4% and 7.6%-8.6%, respectively. The content of oxygen and nitrogen in zirconium alloy standard sample BCR-276 was determined according to the experimental method, and the found results were basically consistent with the certified values.