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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0.0007%和0.0002%。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。

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 pro-posed .0 .06 g of zirconium alloy sample was put into nickel basket ,which was then transferred into graph-ite duplex crucible .The analytical power was controlled at 5 .0 kW .The integral time for oxygen and nitro-gen 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 nitro-gen 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 ox-ygen 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 .

参考文献

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