EDTA差减滴定法测定钼精矿和钼焙砂中钼含量  

Determination of Molybdenum Content in Molybdenum Concentrates and Molybdenum Calcine by EDTA Difference Titration

作　　者：周煜[1] 谭艳山[1] 牛春林[1] 罗春华[1] 李玉仙[1] 万仲建[1] 李美菊[1] 高丽媛[1] 彭建凤[1] 朱利亚[1,2] 

机构地区：[1]云南铜业股份有限公司,云南大理675600 [2]贵研资源(易门)有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106

出　　处：《云南冶金》2012年第4期53-56,共4页Yunnan Metallurgy

基　　金：昆明贵研铂业股份有限公司横向合作基金资助项目(Q/GY-GL-14-06-2010)

摘　　要：用盐酸羟胺还原钼(Ⅵ)至钼(Ⅴ),EDTA络合钼(Ⅴ)及共存离子,锌盐滴定过量EDTA求得合量。于等量试液中不加盐酸羟胺,EDTA络合共存离子,滴定至近终点用酒石酸钾钠掩蔽钼(Ⅵ),锌盐滴定过量EDTA求得分量。二者之差即为钼量。2%～5%钨(Ⅵ)、铬(Ⅵ)或钒(Ⅴ)等共存离子不干扰测定。测定10.00～15.00 mg钼,相对误差-0.20%～+0.20%,测定37%～57%的钼含量,相对标准偏差0.10%～0.15%,样品加标准回收率99.60%～100.80%。方法结果准确度与钼酸铅重量法的一致,但本法选择性好、分析快速。Firstly, the reduction from molybdenum （ Ⅵ ） to molybdenum （ Ⅴ） by employing hydroxylamine hydrochloride, and complexation of molybdenum （ Ⅴ） and co - existent ions by EDTA were conducted, and then the resultant was obtained by titrating exces- sive EDTA with zinc Salt. Secondly, based on complexation of co -existent ions without hydroxylamine hydrochloride in equivalent test solu- tion, molybdenum （ Ⅵ） was masked with potassium sodium tartrate at the titration end - point, after that, the component was got by titrating excessive EDTA with zinc salt. The difference of the resultant and the component was molybdenum content. The determination was not inter- fered by coexistent ions of tungsten （ Ⅵ ） with more than 2% -5% content, chromium （Ⅵ） or vanadium （ Ⅴ ）. For determining 10. 00 - 15.00 mg molybdenum and molybdenum with 37% -57% content, the relative error and the relative standard deviation were -0. 20% - ＋ 0. 20% and 0. 10% -0. 15%, respectively. The standard recovery of samples was 99.60% - 100.80%. The result accuracy of the pro- posed method was consistent with that of lead molybdate gravimetry, but it was of good selectivity and rapid determination.

关 键 词：钼 钼精矿和钼焙砂 EDTA差减滴定法 

分 类 号：O655.2[理学—分析化学]