硫氰酸盐分光光度法测定钛及钛合金中钼量
|
摘要
采用硫酸溶解试样,以铜离子为催化剂,以硫脲为还原剂,基于钼(V)与硫氰酸盐生成橙红色络合物,建立了钛及钛合金中钼量的硫氰酸盐分光光度法.对试验条件如催化剂、还原剂、显色剂溶液用量进行了优化,同时考察了最大吸收波长、溶解酸种类、共存离子、显色体系酸度对钼测定的影响.在最佳试验条件下,钼含量在0.10%～16.0%范围内与其吸光度值成线性关系.按照试验方法开展了加标回收试验,回收率为96.4%～103.1%;并对6种钛合金试样进行钼含量测定,相对标准偏差(RSD,n=11)为0.7%～2.0%,测试结果与ICP-AES法测定一致.
A thiocyanate spectrophotometric method for the determination of molybdenum in titanium and titanium alloys was established by dissolving the sample with sulfuric acid, using copper ion as catalyst and thiourea as reducing agent and forming orange-red complex based on molybdenum(V) and thiocyanate. The experimental conditions such as the amount of catalyst, reductant and chromogenic agent solution were optimized, and the effects of maximum absorption wavelength, types of dissolved acids, coexisting ions and acidity of chromogenic system on the determination of molybdenum were investigated. Under the optimum experimental conditions, the molybdenum content in the range of 0.10%～16.0% has a linear relationship with its absorbance value. The standard addition recovery test was carried out in accordance with the test method, and the recovery rate was 96.4%～103.1%. The molybdenum content of six titanium alloy samples was determined, and the relative standard deviation(RSD, n=11) was 0.7%～2.0%. The test results were consistent with those determined by the method of ICP-AES.
A thiocyanate spectrophotometric method for the determination of molybdenum in titanium and titanium alloys was established by dissolving the sample with sulfuric acid, using copper ion as catalyst and thiourea as reducing agent and forming orange-red complex based on molybdenum(V) and thiocyanate. The experimental conditions such as the amount of catalyst, reductant and chromogenic agent solution were optimized, and the effects of maximum absorption wavelength, types of dissolved acids, coexisting ions and acidity of chromogenic system on the determination of molybdenum were investigated. Under the optimum experimental conditions, the molybdenum content in the range of 0.10%～16.0% has a linear relationship with its absorbance value. The standard addition recovery test was carried out in accordance with the test method, and the recovery rate was 96.4%～103.1%. The molybdenum content of six titanium alloy samples was determined, and the relative standard deviation(RSD, n=11) was 0.7%～2.0%. The test results were consistent with those determined by the method of ICP-AES.
引文
[1] 孙宝莲,李波,王国栋,等.硫氰酸盐光度法测定氨浸渣中的钼[J].稀有金属材料与工程,2009,38(12):2253-2256.
[2] 徐志昌,张萍.硫氰酸盐比色测定钼的方法研究[J].中国钼业,2012,36(4):22-26.
[3] 蒋克旭,邓桂春,姚琳,等.硫氰酸盐分光光度法测定钼精矿的含钼量[J].稀有金属与硬质合金,2010,38(4):52-55.
[4] 乔蓉,易凤兰.ICP-AES法测定钼铁中的钼元素含量[J].金属材料与冶金工程,2016,44(1):54-57.
[5] 李延超,李来平,张新,等.电感耦合等离子体原子发射光谱法测定碳化钼催化剂中钼[J].冶金分析,2014,34(11):61-64.
[6] 李娜,刘鹏宇,颜广炅,等.ICP-MS法测定磁致冷材料-钆硅锗系合金中Mo、Mn、Al、V、Ni、Cu、Ga、Fe[J].分析实验室,2009,26(8):59-61.
[7] 王芸,肖吉群.EDTA返滴定法测定铀钼合金中钼含量[J].中国无机分析化学,2014,4(3):57-60.
[8] 李波,周恺,孙宝莲,等.X射线荧光光谱法测定钼铝合金中钼[J].冶金分析,2013,33(9):42-45.
[9] QU W,ZHOU C Y,CAI L L,et al.Study on determination of molybdenum in molybdenum concentrate by atom absorption spectrometry indirectly[J].光谱学与光谱分析,2017,37(3):984-989.
[10] 李延彪.解析8-羟基喹啉重量法测定钼铁中的钼[J].铁合金,2018,259(4):46-48.
[11] 杨冬,包永明,安利佳.酸性水溶液中硫氰酸钥(V)配合物的研究[J].光谱学与光谱分析,2003,23(2):337-339.
[2] 徐志昌,张萍.硫氰酸盐比色测定钼的方法研究[J].中国钼业,2012,36(4):22-26.
[3] 蒋克旭,邓桂春,姚琳,等.硫氰酸盐分光光度法测定钼精矿的含钼量[J].稀有金属与硬质合金,2010,38(4):52-55.
[4] 乔蓉,易凤兰.ICP-AES法测定钼铁中的钼元素含量[J].金属材料与冶金工程,2016,44(1):54-57.
[5] 李延超,李来平,张新,等.电感耦合等离子体原子发射光谱法测定碳化钼催化剂中钼[J].冶金分析,2014,34(11):61-64.
[6] 李娜,刘鹏宇,颜广炅,等.ICP-MS法测定磁致冷材料-钆硅锗系合金中Mo、Mn、Al、V、Ni、Cu、Ga、Fe[J].分析实验室,2009,26(8):59-61.
[7] 王芸,肖吉群.EDTA返滴定法测定铀钼合金中钼含量[J].中国无机分析化学,2014,4(3):57-60.
[8] 李波,周恺,孙宝莲,等.X射线荧光光谱法测定钼铝合金中钼[J].冶金分析,2013,33(9):42-45.
[9] QU W,ZHOU C Y,CAI L L,et al.Study on determination of molybdenum in molybdenum concentrate by atom absorption spectrometry indirectly[J].光谱学与光谱分析,2017,37(3):984-989.
[10] 李延彪.解析8-羟基喹啉重量法测定钼铁中的钼[J].铁合金,2018,259(4):46-48.
[11] 杨冬,包永明,安利佳.酸性水溶液中硫氰酸钥(V)配合物的研究[J].光谱学与光谱分析,2003,23(2):337-339.