惰气熔融-热导法测定铝钒合金中氮

目前铝钒合金中氮的测定方法没有相应的国家标准或者行业标准,因此建立了测定铝钒合金中氮含量的方法。对惰气熔融-热导法测定铝钒合金中氮的分析条件进行了探讨。称取0.07g铝钒合金样品,放入镍篮,投入脱气后的石墨套坩埚中,控制分析功率为5.0kW,氮积分时间为60s,以钛合金标样进行仪器校准,可实现惰气熔融-热导法对铝钒合金中氮含量的测定。方法检出限为0.00012%,以空白标准偏差的10倍计算出氮的定量限为0.0004%。采用实验方法对两个铝钒合金实际样品中氮进行测定,测定结果的相对标准偏差(RSD,n=11)为6.9%~11%,加标回收率在94%~107%。

Determination of nitrogen in aluminum-vanadium alloy by inert gas fusion-thermal conductivity method

At present, there is no corresponding national standard or industrial standard for the determination of nitrogen in aluminum-vanadium alloy. Consequently a method for the determination of nitrogen in aluminum-vanadium alloy by inert gas fusion-thermal conductivity was established. The optimum experimental conditions for the analysis of nitrogen were investigated. In experiments, 0.07g of sample was put into the nickel basket, which was then transferred into graphite crucible after degassing. The analysis power was controlled at 5.0kW and the analysis time of nitrogen was 60s. The instrument was calibrated using standard aluminum-vanadium alloy sample. The proposed inert gas fusion-thermal conductivity method was applicable for the determination of nitrogen content in aluminum-vanadium alloy. The limit of detection was 0.00012%. The limit of quantification was 0.0004%, which was calculated by 10 times of standard deviation of the blank. The method was adopted to determine the nitrogen content in two aluminum-vanadium alloys. The relative standard deviation (RSD, n=11) of results were between 6.9% and 11%. The spiked recoveries were between 94% and 107%.