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本文设计了测定金属中氧的一种新型热源装置,对一些稀有金属中氧的测定、同真空熔化法作了对照试验,结果基本上一致,同标样结果也一致。本法不用高真空、液氮和价值昂贵的高频感应炉热源。装置简单价廉,操作方便快速,稳定性和重现性好。称样0.1克左右,含量在0.3—0.05％,相对平均偏差为士10％,8小时可完成40多个试样。适用于小型稀有金属工厂生产控制分析。本法系将试样装在带盖石墨盒内,石墨盒夹在两个铜电极之间,在特制玻璃加热室内通入纯氩气,经石墨盒通交流低压电脉冲,瞬间通电3—4秒。通电周期末端温度即达3000℃以上。析出的一氧化碳,通过石墨盒的热壁析出,随氩载气通过转化剂定量地氧化为二氧化碳。生成的二氧化碳用甲醇丙酮体系非水滴定法测定,然后计算其含氧量。
In this paper, a new type of heat source device for the determination of oxygen in metals was designed. The determination of oxygen in some rare metals was compared with the vacuum melting method. The results were basically the same and the same with the standard samples. This method does not require high vacuum, liquid nitrogen and expensive high-frequency induction furnace heat. Device is simple and inexpensive, easy to operate, good stability and reproducibility. Weigh about 0.1 grams, the content of 0.3-0.05%, the relative average deviation of ± 10%, 8 hours to complete more than 40 samples. Suitable for small rare metal factory production control analysis. This law is mounted on a sample with a graphite box, graphite box sandwiched between two copper electrodes, in a special glass heating chamber into the pure argon, through the graphite box through the exchange of low-voltage electrical pulse, the instantaneous power 3-4 second. Power cycle end temperature that is up to 3000 ℃. The precipitated carbon monoxide precipitates through the hot wall of the graphite box and is quantitatively oxidized to carbon dioxide with the carrier gas of the argon through the converter. The generated carbon dioxide is measured by non-aqueous titration with methanol-acetone system, and then the oxygen content is calculated.