过氧化钠熔融-硫氰酸铵差示光度法测定钼精矿和钼焙砂中钼  

Determination of molybdenum in molybdenum concentrate and molybdenum calcine by sodium peroxide fusion-ammonium thiocyanate differential spectrophotometry

作　　者：周煜[1] 谭艳山[1] 朱利亚[1,2] 牛春林[1] 罗春华[1] 李玉仙[1] 万仲建[1] 王前会[1] 

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：《冶金分析》2012年第9期68-72,共5页Metallurgical Analysis

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：研究了用过氧化钠在高铝坩埚中700℃熔融样品5～10min,用硫氰酸铵差示光度法测定了钼精矿和钼焙砂中钼含量的方法。对样品的熔融条件、样品溶液的制备条件和测定条件进行了优化。通过加入无水乙醇消除了MnO24-的干扰,采用三氯化铁溶液沉淀吸附和酒石酸钠掩蔽的方式消除了钨(Ⅵ)、铬(Ⅵ)和钒(Ⅴ)等其它共存离子的影响。结果表明,于吸收波长λ=480nm处,钼质量浓度在14.0～26.0μg/mL范围内符合比尔定律,检出限为4.2×10-2μg/mL。将本法用于钼精矿管理样品GLY-01、钼精矿和钼焙砂生产样品中钼的测定,测定值与参考值或重量法测得结果一致,相对标准偏差(RSD,n=11)为0.10%～0.14%。In a high-alumina crucible, sample was fused at 700 ℃ with sodium peroxide for 5-10 mi nutes, then the content of molybdenum in molybdenum concentrate and molybdenum calcine was de termined by ammonium thiocyanate differential spectrophotometry. The conditions for sample fusion, sample solution preparation and determination were optimized. The interference of MnO4^2- was elimi- nated by addition of absolute ethyl alcohol, and the impact of tungsten （VI）, chromium （VI）, vanadi- um （ V ） and other coexisting ions was eliminated by precipitation adsorption with ferric trichloride so- lution and sodium tartrate masking. The results showed that at the absorption wavelength of 480 nm, the mass concentration of molybdenum conformed to Beefs law within the range of 14. 0 to 26.0μg/mL, and the detection limit was 4.2 × 10 ^-2μg/mL. This method has been used for the determination of molyb- denum in molybdenum concentrate run samples GKY-01, the production samples of molybdenum con- centrate and molybdenum calcine. It was found that the results were in accordance with the reference values or those obtained by gravimetric method, and the relative standard deviations （RSDs, n= 11） were 0.10 %-0.14 %.

关 键 词：钼 钼精矿 钼焙砂 硫氰酸铵差示光度法 熔融 过氧化钠 

分 类 号：O657.32[理学—分析化学]