Determination of oxygen and nitrogen in amorphous zirconium base alloy by inert gas fusion-infrared absorption/thermal conductivity method
MA Lan1, ZHANG Juncheng2, LIAN Weijie1, JIA Jianping1, WEN Tieli3
1. Ningbo Sub-academy of National Weapons Science Research Academy, Ningbo 315103, China; 2. Ningbo Iron&Steel Co.,Ltd, Ningbo 315807, China; 3. Inner Mongolia Metal Material Research Institute,Baotou 014030, China
Abstract：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.
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