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.
作者
杨平平
田新娟
李波
YANG Ping-ping;TIAN Xin-juan;LI Bo(Department of Technical Quality, Xi'an Hantang Analysis and Testing Company Limited, Xi'an710016,China;College of Chemistry & Materials Science, Northwest University, Xi'an 710069 ,China;Institute of Coalbed Gas Development Engineering, Xi'an Research Institute CompanyLimited of China Coal Science and Technology Group, Xi'an 710054, China)
出处
《西安文理学院学报（自然科学版）》
2019年第3期70-74,共5页
Journal of Xi’an University(Natural Science Edition)
基金
西北有色金属研究院生产技术开发课题(JK1602)
关键词
硫氰酸盐
分光光度法
钼
钛及钛合金
thiocyanate
spectrophotometry
molybdenum
titanium and titanium alloys
