高频燃烧-红外吸收法测定金属铪中碳含量研究
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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%.
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
[1]全国钢标准化技术委员会.GB/T 223.71-1997钢铁及和金化学分析方法管式炉内燃烧后重量法测定碳含量[S].北京:中国标准出版社,1997.
[2]中国航空综合技术研究所,北京航空材料研究院.HB 5220.2-2008高温合金化学分析方法第2部分:气体容量法测定碳含量[S].北京:中国航空综合技术研究所,2008.
[3]鲍翠娥.高频红外吸收法测定金属铼中碳含量[J].硬质合金,2007,24(3):178-180.
[4]鲍翠娥.高频红外法测定钴、钽、锆中碳含量[J].硬质合金,2009,26(3):184-187.
[5]荣金相,王水法.高频红外法测定钨粒中痕量碳硫研究[J].冶金分析,2004,24(z):351-354.
[6]刘淑珍.高频红外碳硫分析助熔剂选择[J].冶金分析,1991,11(5):45-47.
[7]陈国举,王祝华.高频燃烧红外吸收法测定电解镍钴铜的微量碳硫[J].冶金分析,2004,24(z):382-384.
[8]马光强,谢辉.硫酸钡重量法测定冰铜中总硫[J].冶金分析,2014,34(3):73-76.
[9]宋维第,孙莹,陈明.感应燃烧红外吸收法测定镍基高温合金中痕量硫[J].冶金分析,2004,24(4):57-59.
[10]ASTM E1941-2010难熔、易熔金属及其合金碳含量标准测定方法[S].宾夕法尼亚西西康舍霍肯:美国材料测试协会,2010.
[2]中国航空综合技术研究所,北京航空材料研究院.HB 5220.2-2008高温合金化学分析方法第2部分:气体容量法测定碳含量[S].北京:中国航空综合技术研究所,2008.
[3]鲍翠娥.高频红外吸收法测定金属铼中碳含量[J].硬质合金,2007,24(3):178-180.
[4]鲍翠娥.高频红外法测定钴、钽、锆中碳含量[J].硬质合金,2009,26(3):184-187.
[5]荣金相,王水法.高频红外法测定钨粒中痕量碳硫研究[J].冶金分析,2004,24(z):351-354.
[6]刘淑珍.高频红外碳硫分析助熔剂选择[J].冶金分析,1991,11(5):45-47.
[7]陈国举,王祝华.高频燃烧红外吸收法测定电解镍钴铜的微量碳硫[J].冶金分析,2004,24(z):382-384.
[8]马光强,谢辉.硫酸钡重量法测定冰铜中总硫[J].冶金分析,2014,34(3):73-76.
[9]宋维第,孙莹,陈明.感应燃烧红外吸收法测定镍基高温合金中痕量硫[J].冶金分析,2004,24(4):57-59.
[10]ASTM E1941-2010难熔、易熔金属及其合金碳含量标准测定方法[S].宾夕法尼亚西西康舍霍肯:美国材料测试协会,2010.