摘要
称取0. 5 g金属铪样品置于瓷坩埚中,加入0. 3 g纯铁和1. 5 g钨锡粒助熔剂,设定高频燃烧红外碳分析功率为80%,吹扫和延迟时间均为10 s,比较水平为2,以钢铁碳标准物质样单点校准设备,绘制校准曲线,并用标准物质验证曲线准确性,建立金属铪中碳含量的测定方法,测量范围为0. 001%~0. 040%。采用该方法对2个厂家的金属铪中碳含量进行测定,测定结果的相对标准偏差不大于8%,在2个金属铪样品中加入钢铁碳标样进行加标回收试验,回收率在85%~106%之间。
0.5 g of sample,0.3 g of pure iron and 1.0 g of tungsten-tin particles were added into the crucible. The instrumental parameters were set as follows: the high frequency poweris 80%,both the purge and delay time is 10 s,and the comparator level is 2. The single-point calibration curve was established using the standard sample of carbon in steel and it was confirmed by another standard sample. As a result,the determination method of carbon in hafniummetal by high frequency combustion-infrared absorption method was established,with the determination range of 0. 001% ~ 0. 040%. The proposed method was applied to the determination of carbon in two kinds of hafniummetal samples from different companies. The relative standard deviations( RSD)of determination results were not larger than 8%. In addition,standard sample of steel was added to two samples of hafnium metal to carry out recovery tests. The results show that the recovery rate was between 85% and 106%.
引文
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