惰性气体中熔融试样-红外光谱法测定锡钛合金中氧含量

IR Spectrometric Determination of Oxygen in Tin-Titanium Alloy with Fusion of Sample in Inert Gas Atmosphere

称取锡钛合金0.07g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4.5kW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%。

A portion of Sn-Ti alloy(0.07g)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 600oxygen and nitrogen analyzer.The sample was fused in the furnace at 4.5kW with Ni as flux,and CO with a little of CO2 was formed by the reaction of O2of the sample with C of the crucible under high temperature.When passing over the hot RE-bearing copper oxide,CO was converted into CO2and its absorbance was measured by the IR detector,and the amount of CO2found was converted into O2content of the sample.Precision of the method was tested by analyzing a same SnTi alloy for 8determinations,giving result of O2contents(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 O2content to the matrix of Sn-Ti alloy,values of recovery found were in the range of 85%to 119%.