酸溶-硫氰酸钾分光光度法测定矿石中钼  

Spectrophotometric Determination of Molybdenum in Ores with Acid-Dissolution and Potassium Thiocyanate

作　　者：王冀艳[1] 闫红岭[1] 刘勉[1] 李振[1] 钟莅湘[1] 李艳华[1] 

机构地区：[1]河南省岩石矿物测试中心,郑州450001

出　　处：《理化检验（化学分册）》2016年第12期1400-1403,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：河南省两权价款项目豫国土资函([2015]258号-01)

摘　　要：测定了6种不同矿样中的钼含量。取矿样样品（0．200O-0．5000g）在聚四氟乙烯烧杯中，先加入氢氟酸5mL和硝酸5mL，于280℃加热蒸干，再加硫酸5mL，于330℃加热至冒白烟。冷却，将溶液和沉淀一起移至50mL容量瓶中，加水至刻度，摇匀。分取其上清液，按硫氰酸盐光度法测定其钼含量。钼的线性范围为0．02-4．0mg·L^-1，方法的检出限（3s）为0．12mg·L^-1。应用所提出方法测定了4种矿石标准物质（GBW07238，GBW07241，GBW07282，GBW07164）中钼的含量，测定值与认定值相符，测定值的相对标准偏差（n=11）在2．6％-6．2％之间。Molybdenum in 6 kinds of ores was determined. A portion of the ore sample （0. 200 0-0.5000g） was placed in a PTFE beaker and heated with 5 mL of HF and 5 mL of HNOa at 280℃ until to dryness. 5 mL of H2SO4 were then added and heated again at 330℃ until fuming. After cooling, the solution together with the precipitate was transferred to a 50 mL volumetric flask and diluted to mark with water. An aliquot of the supernatant was taken and its molybdenum content was determined by the SCN--photometric method. Linearity range of molybdenum was found between 0.02 mg·L^-1 and 4. 0 mg·L^-1 with detection limit （3s） of 0. 12 mg·L^-1. Molybdenum in 4 CRM＇s （GBW 07238, GBW 07241, GBW 07282, GBW 07164） of different ores was determined by the proposed method, giving results in consistency with the certified values. Values of RSD＇s （n=11） found were ranged from 2.6% to 6.2%.

关 键 词：分光光度法 钼 矿石 硫氰酸钾 酸溶 

分 类 号：O657.32[理学—分析化学]