Abstract:The application of “direct-dropping” in the analysis of oxygen, nitrogen and hydrogen in metal powder sample was discussed in detail. “Drect-dropping” was different from the traditional “packaging”, which was mainly reflected in the mode of sample dropping. “Direct-dropping” of sample avoided the influence of blank of packaging materials, and it could be applied for the analysis of oxygen, nitrogen and hydrogen in metal powder sample such as high temperature alloy, iron and steel, nickel and copper. The difference of blank between “direct-dropping” and nickel foil/tin foil as well as nickel capsule/tin capsule was firstly investigated. The results showed that the blank of “direct-dropping” was lowest, and the blank of nickel capsule was the second low. The “direct-dropping” was calibrated with the certified reference materials of JK47 iron powder and 502-903 columnar steel. Many application examples of powder samples of high temperature alloy were listed and the advantages of “direct-dropping” were obvious. Eight representative samples from six different materials were selected for the comparison tests between “direct-dropping” and nickel capsule/tin capsule “packaging”. The determination results of the above two methods were basically consistent. However, “direct-dropping” was not applicable for the analysis of oxygen and nitrogen in “flux-dependent” powder samples such as titanium, zirconium, niobium and chromium. Titanium powder and titanium block samples were used as study object: when the sample was directly dropped without package of flux, the analysis of oxygen and nitrogen would be seriously interfered and the error might be in the orders of magnitude. But “direct-dropping” could be used for the analysis of hydrogen, which was also suitable for the “flux-dependent” samples. The determination of hydrogen was not affected by the mode of sample dropping. Only when the metal powder sample was packaged with tin, the determination results of hydrogen were slightly different of a little higher. It should be noted that the “direct-dropping” was forbidden for the analysis of oxygen, nitrogen and hydrogen in active metal sample such as magnesium and aluminum neither for powder or block samples. Or else, the “direct-dropping” might cause the contamination of active metals or the failure of instrument
王蓬,张中豪.脉冲加热-红外吸收法分析锡铅粉末中氧的浴料选择[J].冶金分析,2005,25(4):87-88.WANG Peng,ZHANG Zhong-hao.Determination of oxygen in Sn/Pb powder by impulse-heating infrared absorption method and selection of the bath[J].Metallurgical Analysis,2005,25(4):87-88.
[4]
钱庆长,骆友健.脉冲加热红外吸收法测定雾化铜粉中氧[J].冶金分析,2004,24(6):44-46.QIAN Qing-chang,LUO You-jian.Determination of oxygen in nebulized copper powder by pulse heating and infrared absorption method[J].Metallurgical Analysis,2004,24(6):44-46.
[5]
高鹏,金小成,段双,等.直投法测定高温合金粉末中氧氮氢含量[J].冶金分析,2018,38(增刊):41-43.GAO Peng,JIN Xiao-cheng,DUAN Suang,et al.Determination of O,N,H in superalloy powders by direct-sample-dropping method[J].Metallurgical Analysis,2018,38(Supp.):41-43.
[6]
方卫,刘伟,杨玉芳.高温钛合金粉中氧氮的同时测定[J].分析试验室,2001,20(6):94-95.FANG Wei,LIU Wei,YANG Yu-fang.Simultaneous determination of oxygen and nitrogen in titanium alloy powder[J].Chinese Journal of Analysis Laboratory,2001,20(6):94-95.
朱跃进,李素娟.惰气熔融法测定镁中氧、氢、氮[J].冶金分析,2011,31(12):58-61.ZHU Yue-jin,LI Su-juan.Determination of oxygen, hydrogen and nitrogen in magnesium by inert gas fusion method[J].Metallurgical Analysis,2011,31(12):58-61.
[10]
朱跃进.五元浴在氧氮测定中的应用[J].分析试验室,2004,24(增刊):207-209.ZHU Yue-jin.Application of 5-elememt bath in determination of oxygen and nitrogen[J].Chinese Journal of Analysis Laboratory,2004,24(Supp.):207-209.