样品经盐酸(1+1)和硝酸(1+1)分解后,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定三氧化二钒和五氧化二钒中钾、钠、磷、硫、铁杂质元素的含量.采用基体匹配消除主量元素钒对杂质元素的干扰,优化了测定工作条件,确定钾、钠、磷、硫、铁的分析谱线分别为766.490 nm、589.592 nm、178.284 nm、182.034 nm、259.940 nm.测定氧化钾、氧化钠、磷、硫、铁的检出限分别为0.020 mg/L、0.012 mg/L、0.008 mg/L、0.010 mg/L、0.002 mg/L.方法用于标准样品和实际样品的分析,测定结果分别同认定值及其他方法的测定结果相吻合,相对标准偏差(n=11)为0.54%～4.0%.
The samples were dissolved in hydrochloric acid(1+1) and nitric acid(1+1). The impure elements in vanadium trioxide and vanadium pentoxide including potassium, sodium, phosphorus, sul-fur and iron were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The effects of vanadium could be eliminated by matrix matching. The working conditions were opti-mized. The analytical line were determined:K 766. 490 nm;Na,589. 592 nm;P,178. 284 nm;S,182. 034 nm;Fe, 259. 940 nm. The determination results of standard samples and actual samples were in good agreement with the certified values and those obtained by other methods. The relative standard devia-tion(n=11) was 0.54%-4.0%.
参考文献
| [1] | 黄道鑫.提钒炼钢[M].北京:冶金工业出版社,2002 |
| [2] | YB/T 5331-2006.YB/T 5331-2006.五氧化二钒化学分析方法:共沉淀-萃取钼蓝分光光度法测定磷量[S].,2006. |
| [3] | YB/T 5335-2006.YB/T 5335-2006.五氧化二钒化学分析方法:原子吸收分光光度法测定氧化钾和氧化钠量[S].,2006. |
| [4] | 陈德.火焰原子吸收法连续测定钒氧化物中的钾、钠、铁[J].重庆工业高等专科学校学报,2002(04):39-41. |
| [5] | 辛仁轩.等离子体发射光谱分析[M].北京:化学工业出版社,2005 |
| [6] | 闻向东,赵希文,文斌,周正伦.电感耦合等离子体原子发射光谱法测定萤石中低含量二氧化硅[J].冶金分析,2008(03):61-63. |
| [7] | 王志萍,李晖,刘军,王晓艳.电感耦合等离子体原子发射光谱法测定钨铁中铜锰硅[J].冶金分析,2008(11):40-42. |
| [8] | 贾林.电感耦合等离子发射光谱法测定生铁中多元素[J].冶金分析,2004(z1):90-92. |
| [9] | 侯列奇,李洁,卢菊生.电感耦合等离子体原子发射光谱法测定高纯铌中微量钽[J].理化检验-化学分册,2008(05):425-426. |
| [10] | 杨毅.ICP-AES在冶金分析中的应用[J].云南冶金,2007(04):62-67,77. |
| [11] | 刘宁;杜文虎 .ICP-AES中四十种常见元索光谱干扰的研究及较正[J].光谱学与光谱分析,1992,12(05):47-53. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%