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稀土黄颜料是一种用在陶瓷、搪瓷等产品着色的无毒色素,至今未见有报导其组分的测定方法。特别是其中的稀土总量的测定,对生产工艺、产品质量等都有较大意义。锆英石中锆与稀土的分离方法有:铜铁试剂-氯仿、PMBP-苯萃取分离;氟化物分离;草酸盐分离,这些方法繁琐或有毒。据文献,本文试验了用钽试剂分离锆与稀土,较好地解决了稀土黄颜料中稀土总量的测定。本法简单、无毒,且准确度较好。一试样的熔解称焦硫酸钾、氟化氢钾各2克,混匀,放入铂坩埚,称试样约0.1克和熔剂混合,在低温加热约5分钟,高温熔融(加热至熔融状态或熔块呈白色),移下冷至室温,加浓硫酸约2.5毫升,加热赶氟15分钟,冷后将铂坩埚带盖放入250毫升烧杯中,用热水约100毫升溶解熔块,洗净坩埚,试液转入500毫升量瓶中,冷却,稀释。按同样方法得—空白溶液。
Rare earth yellow pigment is a kind of non-toxic pigment which is used in coloring of ceramics, enamel and other products. So far, no method has been reported for the determination of its components. In particular, the determination of the total amount of rare earth, the production process, product quality, etc. have great significance. Zirconium zirconium and rare earth separation methods are: copper and iron reagent - chloroform, PMBP-benzene extraction separation; fluoride separation; oxalate separation, these methods cumbersome or toxic. According to the literature, this paper tested the separation of zirconium and rare earth with tantalum reagent to solve the determination of the total amount of rare earth in the rare earth yellow pigment. This law is simple, non-toxic, and accurate. A sample of molten potassium pyrrolysulfate, potassium bifluoride each 2 grams, mix, placed in a platinum crucible, said about 0.1 grams of the sample and the flux mixed, heated at low temperature for about 5 minutes, high temperature melting (heating to the molten state or melt Block is white), remove the cold to room temperature, add about 2.5 ml of concentrated sulfuric acid, heated to catch fluorine for 15 minutes, cold platinum crucible with a lid into a 250 ml beaker, with hot water about 100 ml dissolve the frit, wash Crucible, test solution into 500 ml volumetric flask, cooled, diluted. The same way - blank solution.