稀土系储氢合金中氧量的测定
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摘要
采用脉冲-红外吸收法测定稀土系储氢合金中氧含量,通过不同功率与积分时间的比较,确定了仪器的测定条件。在此条件下,实验了不同的助熔剂和样品称样量对氧量测定的影响,确定了最佳的助熔剂与合适的样品称样量范围。采用氧含量范围合适的钛合金标样做工作曲线,多次测定空白,计算得到方法的检出限为0.0030%。对于氧含量为0.05%和0.2%的样品,相对标准偏差分别为7.4%和2.0%,满足分析检测的要求。对不同系列储氢合金样品分别做加标回收实验,不含镁的样品回收率在93%~103%之间,含镁量不同的样品(~1%Mg、~2%Mg)回收率分别为72%~92%、63%~80%。因此,本方法不适合测定含镁的储氢合金样品,但可以准确快速测定氧范围为0.0050%~0.x%的不含镁稀土系储氢合金样品。
The oxygen content in rare earth hydrogen storage alloy was measured by impulse-infrared absorption method.The measurement conditions were determined by comparing the power and integration time. The effects of different fluxes and sample weights on the determination of oxygen were tested and the optimum range of flux and sample weights were determined.The calibration curve was established by titanium alloy standard withsuitable oxygen content range. By determining the blank value many times,the detection limit of the method was obtained 0. 0030%. For the samples with oxygen contents of 0. 05%and 0. 2%,the relative standard deviations(RSDs) were 7. 4% and 2% respectively,which satisfied the requirements of analysis. The recovery experiments of different series hydrogen storage alloy samples were done respectively.The recoveries of samples without magnesium were between 93% and 103%,and the recoveries of samples with different magnesium contents were72% to 92%(about 1% Mg) and 63% to 80%(about 2% Mg) respectively. Therefore,this method is not suitable for the determination of Mg-containing hydrogen storage alloy samples,but can be used for accurate and rapid determination of oxygen between 0. 0050% and 0.X% in the rare earth hydrogen storage alloy samples without magnesium.
The oxygen content in rare earth hydrogen storage alloy was measured by impulse-infrared absorption method.The measurement conditions were determined by comparing the power and integration time. The effects of different fluxes and sample weights on the determination of oxygen were tested and the optimum range of flux and sample weights were determined.The calibration curve was established by titanium alloy standard withsuitable oxygen content range. By determining the blank value many times,the detection limit of the method was obtained 0. 0030%. For the samples with oxygen contents of 0. 05%and 0. 2%,the relative standard deviations(RSDs) were 7. 4% and 2% respectively,which satisfied the requirements of analysis. The recovery experiments of different series hydrogen storage alloy samples were done respectively.The recoveries of samples without magnesium were between 93% and 103%,and the recoveries of samples with different magnesium contents were72% to 92%(about 1% Mg) and 63% to 80%(about 2% Mg) respectively. Therefore,this method is not suitable for the determination of Mg-containing hydrogen storage alloy samples,but can be used for accurate and rapid determination of oxygen between 0. 0050% and 0.X% in the rare earth hydrogen storage alloy samples without magnesium.
引文
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