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试样经盐酸溶解后直接用EDTA滴定化合锆。单体锆呈不溶状态析出,不干扰测定。另一份试样以盐酸一氢氟酸溶解化合锆和单体锆,加入过量的铝离子,消除F~-的干扰,用EDTA滴定总锆量.方法简单、快速、终点明显、结果较为满意。一试剂锆标准溶液:称取光谱纯二氧化锆0.2702克,置于干的50毫升瓷坩埚中,加焦硫酸钾8克,混匀。于800℃温度熔融20～30分钟,冷却。用(1+9)盐酸100毫升浸出熔融物。加热至溶液澄清,冷却后移入500毫升量瓶中,以(1+9)盐酸稀至刻度,摇匀。吸取上
The sample was dissolved in hydrochloric acid directly titrated with EDTA zirconium. Monomer zirconium was insoluble state precipitation, does not interfere with the determination. Another sample of hydrofluoric acid dissolved hydrofluoric acid zirconium and zirconium monomer, adding excessive aluminum ions, eliminating the interference of F ~ - titration of total zirconium with EDTA method is simple, fast, the end point is obvious, the results are more satisfactory . A reagent zirconium standard solution: Weigh spectral pure zirconium dioxide 0.2702 grams, placed in a dry 50 ml porcelain crucible, add potassium pyrophosphate 8 grams, mix. Melt at 800 ℃ for 20 ~ 30 minutes and cool. The melt was leached with 100 ml of (1 + 9) hydrochloric acid. Heated to clarify the solution, after cooling into 500 ml volumetric flask, dilute (1 +9) hydrochloric acid to the mark, shake well. Draw on