IR Spectrometric Determination of Oxygen in TinTitanium Alloy with Fusion of Sample in Inert Gas Atmosphere
摘 要
称取锡钛合金0.07 g置于镍囊中,投入TC 600氧氮测定仪中已造好镍浴的石墨坩埚中,在氦气氛中,在4.5 kW功率条件下,于脉冲炉中将样品熔融,样品中的氧在高温条件下与碳反应生成一氧化碳和少量二氧化碳,其中一氧化碳通过热的稀土氧化铜转化成二氧化碳,然后进入红外检测池进行检测并换算成氧含量。以锡钛合金为基体加入已知含氧量的钛标准样品,按方法进行回收试验,测得回收率在85.0%~119%之间。对同一锡钛合金进行8次测定,测定值在0.017 9%~0.020 8%之间,相对标准偏差为9%。
Abstract
A portion of SnTi alloy (0.07 g) was placed in a small nickel capsule, which was introduced into molten nickel bath in a graphite crucible located in the pulse furnace of the TC 600 oxygen and nitrogen analyzer. The sample was fused in the furnace at 4.5 kW with Ni as flux, and CO with a little of CO2 was formed by the reaction of O2 of the sample with C of the crucible under high temperature. When passing over the hot REbearing copper oxide, CO was converted into CO2 and its absorbance was measured by the IR detector, and the amount of CO2 found was converted into O2 content of the sample. Precision of the method was tested by analyzing a same SnTi alloy for 8 determinations, giving result of O2 contents (w%) range from 0.017 9% to 0.020 8% and value of RSD of 9%. Recovery was tested by addition of Ti standard sample with known O2 content to the matrix of SnTi alloy, values of recovery found were in the range of 85% to 119%.
中图分类号 O657.33
所属栏目 工作简报
基金项目
收稿日期 2013/5/11
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联系人作者王宽(kwang83@163.com)
备注王宽(1983-),男,陕西汉中人,助理工程师,硕士,主要研究方向为金属材料中气体成分分析。
引用该论文: WANG Kuan,LI Bo,SUN Baolian,WANG Hui,LIANG Qinghua,ZHENG Wei. IR Spectrometric Determination of Oxygen in TinTitanium Alloy with Fusion of Sample in Inert Gas Atmosphere[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(6): 737~739
王宽,李波,孙宝莲,王辉,梁清华,郑伟. 惰性气体中熔融试样-红外光谱法测定锡钛合金中氧含量[J]. 理化检验-化学分册, 2014, 50(6): 737~739
被引情况:
【1】刘攀,杜丽丽,唐伟,李治亚, "无机固态材料中气体元素分析的现状与进展",理化检验-化学分册 51, 131-136(2015)
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参考文献
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【3】李明正,郭增强,杨芸.红外吸收光谱法测定钼中氧[J].理化检验化学分册, 2008,44(11):1117-1119.
【4】BECK E J, CLARK F E. Determination of oxygen by the inert gas diffusion method using graphite capsules[J]. Anal Chem, 1961,33(12):1767-1770.
【5】INOUE R, SUITO H. Determination of oxygen in ironaluminum alloy by inert gas fusioninfrared absorptiometry[J]. Materials Transactions, 1991,32(12):1164-1169.
【6】周海收,王启芳.稀土金属钕和镝中氧氮的测定方法研究[J].分析试验室, 2005,24(3):79-81.
【7】蒋启翠.高频燃烧红外吸收法测定钢铁中微量碳硫[J].冶金分析, 2005,25(4):95-96.
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