制样方法对测定钒铝中间合金中钒铁硅碳氧的影响

Effect of sample preparation on determination of vanadium,iron,silicon,carbon and oxygen in vanadium-aluminum master alloy

研究了钒铝中间合金(简称钒铝合金)的制样方法对样品中钒、铁、硅、碳和氧测定结果的影响。确定了样品的保存和制备方法:样品需置于干燥器中保存;选择一次破碎量为40g,对于含钒量在55%及以下的钒铝合金样品,控制破碎时间为2s,含钒量大于55%的钒铝合金样品控制破碎时间为5s,可将样品破碎至-0.147mm。随机取AlV55和AlV85合金试样,对各元素进行5次测定,比较制样前后各元素测定结果及其精密度的变化情况,并对元素钒和氧进行了加标回收试验。结果表明:制样后样品的均匀性得到了明显改善,保证了各元素尤其是氧和钒测定结果的重现性和准确性。对随机抽取的10批AlV55样品按拟定的方法制样和测定,进行实验室间数据比对,一致性较好。

The effect of sample preparation on the determination results of vanadium,iron,silicon,carbon and oxygen in vanadium-aluminum master alloy was investigated.The storage and preparation methods of sample were determined：the sample should be kept in desiccators; the breaking time was 2 and 5 s for 40 g of vanadium-aluminum master alloy sample with vanadium content no more than 55% and more than 55%,respectively,then the sample could be broken to-0.147 mm.The determination results and precision before and after sample preparation were compared by determination of AlV55 and AlV85 alloy samples which were randomly selected for 5 times,while,the recovery tests of vanadium and oxygen were also conducted,The results showed that the uniformity of sample was significantly improved after preparation.The repeatability and accuracy of determination results especially for oxygen and vanadium could be guaranteed.The randomly selected 10 batches of AlV55 samples were prepared and determined according to the experimental method.The inter-laboratory data were compared,which indicated the good consistency.