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目前测定铝土矿石中微量钽大部分是采用有机溶剂萃取富集并与其他元素分离,在有机相中比色。由于有机溶剂挥发,污染环境,我们针对铝土矿中含钛量较高,又严重干扰钽测定的特点,采用丹宁-硫酸,动物胶沉淀分离大部分钛,并提高显色酸度抑制钛的显色,以草酸掩蔽铌,以水杨基荧光酮-钽-溴代十六烷基的三元络合物方法进行测定,灵敏度可达0.05ppm。 (一)试剂 1.称取水杨基荧光酮(邻羟基苯芴酮,分子式为C_(10)H_(12)O_6)0.02克,加1∶1盐酸1毫升,摇匀后,加入30毫升乙醇,待全部溶解后以水稀释至1000毫升。 2.称取20克丹宁在1000毫升5％硫酸液中加热使其溶解。 (二)分析手续称取0.2克矿样于瓷坩埚中,加3克焦硫酸钾置于500—600℃马弗炉中熔融20分钟,取出稍
At present, most of trace tantalum in bauxite ore is determined by organic solvent extraction and enrichment with other elements for colorimetric determination in organic phase. Due to the volatile organic solvents, polluting the environment, we aim at the high content of titanium in bauxite and seriously interfere with the determination of tantalum. We use tannin-sulfuric acid and animal glue to separate most of the titanium and improve the color- Color, with oxalic acid masking niobium, with salicylfluorone - tantalum - bromo hexadecyl ternary complex method for the determination of sensitivity up to 0.05ppm. (A) Reagents 1. Weigh 0.02g salicyl fluorone (o-hydroxybenzofluorenone, molecular formula C_ (10) H_ (12) O_6), add 1ml 1: 1 hydrochloric acid, shake, add 30ml ethanol , Until all dissolved diluted with water to 1000 ml. 2. Weigh 20 grams of tannin dissolved in 1000 ml of 5% sulfuric acid to heat. (B) analysis procedures Weigh 0.2 grams of ore samples in porcelain crucible, add 3 grams of potassium pyrophosphate placed 500-600 ℃ muffle furnace melting for 20 minutes, remove slightly