Abstract:Ferromolybdenum is mainly used as molybdenum additive in steelmaking process. The content of iron in ferromolybdenum will affect the composition of final steel. Through the composition analysis of the commercially available ferromolybdenum certified reference materials and ferromolybdenum samples, it was found that the main element of molybdenum and a small amount of nickel and copper in the samples would interfere with the determination of iron by potassium dichromate titration. The samples were treated by acid dissolution-sodium hydroxide precipitation separation or sodium peroxide alkali fusion to separate the main interfering element of molybdenum during sample decomposition. If the content of nickel or copper in ferromolybdenum sample solution was not less than 1 mg, their interference with the determination could be ignored, and the content of iron in sample solution could be directly determined by potassium dichromate titration. If the content of nickel or copper was more than 1 mg, their interference could not be ignored, and they should be removed by ammonia precipitation before determination of iron by potassium dichromate titration. Consequently, the determination of iron in ferromolybdenum by potassium dichromate titration was realized by converting the results. After the actual samples and certified reference materials of ferromolybdenum were treated by acid dissolution-sodium hydroxide precipitation separation and sodium peroxide alkali fusion respectively, iron were determined by potassium dichromate titration. For the actual samples, the relative standard deviation (RSD, n=11) of determination results was 0.25% and 0.24%,respectively. For the certified reference materials, the determination results of the two methods were consistent with standards values, and the relative errors of two methods were 0.043%-0.16% and 0.025%-0.19%, respectively.
[1] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 5059.1—2014 钼铁 钼含量的测定 钼酸铅重量法、偏钒酸铵滴定法和8-羟基喹啉重量法[S].北京:中国标准出版社,2014. [2] 李延彪.解析8-羟基喹啉重量法测定钼铁中的钼[J].铁合金,2018,49(4):46-48. LI Yanbiao.Parsing 8-hydroxyquinoline gravimetric method for determination of molybdenum in ferromolybdenum[J].Ferro-alloys,2018,49(4):46-48. [3] 杨利峰,刘国军,吴志鸿,等.氢化物发生-电感耦合等离子体原子发射光谱法测定钼铁中砷锡锑铋[J].冶金分析,2020,40(2):53-58. YANG Lifeng,LIU Guojun,WU Zhihong,et al.Determination of arsenic,tin,antimony and bismuth in ferromolybdenum by hydride generation-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2020,40(2):53-58. [4] 张凤萍,马骏,王振宇,等.电感耦合等离子体原子发射光谱法测定钼铁中硅、锰、铬、镍元素[J].山西化工,2019,39(2):45-46,50. ZHANG Fengping,MA Jun,WANG Zhenyu,et al.Determination of silicon, manganese, chromium and nickel in ferromolybdenum by inductively coupled plasma atomic emission spectrometry[J].Shanxi Chemical Industry,2019,39(2):45-46,50. [5] 王献科,李玉萍,李莉芬.释放螯合滴定法测定钼铁中的铁含量[J].中国钼业,2000(1):38-40. WANG Xianke,LI Yuping,LI Lifen.Released chelatometry determination of iron in ferromolybdenum[J].China Molybdenum Industry,2000(1):38-40. [6] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 223.7—2002 铁粉 铁含量的测定 重铬酸钾滴定法[S].北京:中国标准出版社,2002. [7] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 223.73—2008 钢铁及合金 铁含量的测定 三氯化钛-重铬酸钾滴定法[S].北京:中国标准出版社,2008. [8] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 223.70—2008 钢铁及合金 铁含量的测定 邻二氮杂菲分光光度法[S].北京:中国标准出版社,2008. [9] 国防科学技术工业委员会.HB 5220.30—2008 高温合金化学分析方法 第30部分 邻菲啰啉吸光度法测定铁含量[S].北京:中国航空综合技术研究所,2008. [10] 国家国防科技工业局.HB 20241.7—2016 高温合金化学成分光谱分析方法 第7部分 电感耦合等离子体原子发射光谱法测定铝、钴、铜、铁、锰、钼、钛含量[S].北京:中国航空综合技术研究所,2016. [11] 苗晓焕,冯振华.重铬酸钾滴定法测定废杂铜中的铁含量[J].中国无机分析化学,2021,11(4):67-71. MIAO Xiaohuan,FENG Zhenhua.Determination of iron in scrap copper by dichromate titration method[J].Chinese Jorunal of Inorganic Analytical Chemistry,2021,11(4):67-71. [12] 蒋晓光,王艳君,王彩云,等.硫代硫酸钠滴定法连续测定铜磁铁矿中铜和铁[J].化学分析计量,2015,24(3):22-26. JIANG Xiaoguang,WANG Yanjun,WANG Caiyun,et al.Continuous determination of copper and iron in copper magnetite by sodium thiosulfate titration[J].Chemical Analysis and Meterage,2015,24(3):22-26. [13] 吴雪英,魏雅娟,刘晓玲,等.EDTA滴定法测定再生锌原料中铁[J].冶金分析,2016,36(5):53-57. WU Xueying,WEI Yajuan,LIU Xiaoling,et al.Determiantion of iron in regenerated zinc raw material by EDTA titration method[J].Metallurgical Analysis,2016,36(5):53-57.