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目前,我国各合成氨厂在分析醋酸铜氨液中总铜含量时,普遍采用氧化-还原碘量法。此方法费时、成本高。本文采用络合滴定法,以紫脲酸氨为指示剂直接测定醋酸铜氨溶液中总铜量,方法简便、快速,满足了生产的需要。 (一)主要试剂紫脲酸氨指示剂:氯化钠(二级)预先在600℃灼烧2小时,50份氯化钠与1份紫脲酸胺(固体)混匀;乙二胺四乙酸二钠盐标准溶液(二级),0.05M,用标准氧化锌标定。 (二)分析方法取原铜液10毫升,用蒸馏水稀释至100毫升。从中取出1毫升放入250毫升三角瓶内,摇动后,加100毫升蒸馏水,少量紫脲酸胺指示剂,滴加5%硫酸至黄色或黄绿色,再加少许固体氯化铵,然后,以0.05MEDTA,滴至蓝色或蓝紫色为终点。
At present, China’s ammonia plant in the analysis of copper acetate ammonia solution in the total copper content, the general use of oxidation - reduction of iodine method. This method is time-consuming and costly. In this paper, the complexation titration method is used to directly determine the total copper content in the cupric acetate ammonia solution by using the ammonia urethane as an indicator, and the method is simple and rapid and meets the production needs. (A) the main reagent Purple urea ammonia indicator: sodium chloride (second grade) pre-fired at 600 ℃ for 2 hours, 50 parts of sodium chloride and 1 parts of urea (urea) Acetic acid disodium salt standard solution (secondary), 0.05M, calibrated with standard zinc oxide. (B) analysis method Take the original copper solution 10 ml, diluted with distilled water to 100 ml. Remove 1 ml and put it into a 250 ml Erlenmeyer flask. After shaking, add 100 ml of distilled water, a small amount of urethane amine indicator, add 5% sulfuric acid to yellow or yellowish green, add a little solid ammonium chloride, 0.05MEDTA, dropping to blue or blue purple as the end point.