惰气熔融-红外吸收/热导法测定非晶锆基合金中氧和氮

非晶锆基合金的发展结合了金属和玻璃等学科,具有广泛的应用领域,准确测定其中的氧和氮含量,可有效开展产品研发过程中的质量控制。称取0.07～0.08 g样品,采用镍篮做助熔剂,设定分析功率为6.0 kW,采用锆合金标准样品校准仪器,使用石墨套坩埚进行测定,建立了惰气熔融-红外吸收/热导法测定非晶锆基合金中氧和氮的测定方法。选择与非晶锆基合金中氧和氮含量较匹配的锆合金标准物质,采用单标准点校准程序进行系数校正,用锆合金标准物质以及钛合金标准物质进行验证试验,结果表明,氧和氮的测定结果基本在认定值的扩展不确定度(k＝2)区间内。结果表明:在选定的实验条件下,方法的检出限分别为氧0.000 048%,氮0.000 066%,方法的定量限分别为氧0.000 16%,氮0.000 22%。对两组非晶锆基合金样品进行精密度试验,氧和氮测定结果的相对标准偏差(RSD,n=9)均小于5%;按实验方法对非晶锆基样品进行加标回收试验,氧的回收率为98%～103%,氮的回收率为95%～102%。

Determination of oxygen and nitrogen in amorphous zirconium base alloy by inert gas fusion-infrared absorption/thermal conductivity method

The development of amorphous zirconium based alloy combined with disciplines such as metal and glass, and it had a wide range of applications. The accurate determination of oxygen and nitrogen contents could effectively guide the quality control in product development process. 0.07-0.08 g of sample was wrapped with a nickel basket as flux. The analytical power was set at 6.0 kW. The instrument was calibrated with certified reference material of zirconium alloy. Therefore, a determination method of oxygen and nitrogen in amorphous zirconium based alloy was established by inert gas fusion-infrared absorption/thermal conductivity method with graphite double-crucible. The certified reference material of zirconium alloy matching the content of oxygen and nitrogen in amorphous zirconium base alloy was selected for coefficient correction by the single standard point calibration procedure. The verification tests were conducted with the certified reference materials of zirconium alloy and titanium alloy. The results showed that the determination results of oxygen and nitrogen were basically within the expanded uncertainty (k=2) range of the certified values. The results showed that the limit of detection was 0.000 048% for oxygen and 0.000 066% for nitrogen respectively under the selected experimental conditions. The limit of quantification was 0.000 16% for oxygen and 0.000 22% for nitrogen, respectively. The precision tests of two groups of amorphous zirconium based alloy samples were conducted. The relative standard deviations (RSDs, n=9) of determination results of oxygen and nitrogen were all less than 5%. The standard addition recovery test of amorphous zirconium based alloy sample was performed according to the experimental method. The recoveries for oxygen and nitrogen were 98%-103% and 95%-102%, respectively.