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一、本文就苯芴酮光度法测定微量Sn时的温度、分散剂、稳定剂、显色剂浓度等作了进一步的条件试验,提出了适合该类试样中Sn测定的用量。二、选择在7N H_2SO_4—0.5N KI介质中,以苯萃取SnI_4,从TiO_2中分离微量Sn,以10%H_3SO_4—3%H_2O_2(10:1)混合液反萃取,可使Sn与大量干扰元素很好分离。三、采用(NH_4)_2SO_4—H_2SO_4高温下溶解TiO_2样品,溶解后的浓溶液经过冷冻处理,然后直接进行萃取。最后在1.2N左右H_2SO_4介质中,以聚乙烯醇为分散剂,苯芴酮光度法测定Sn,应用于实际分析,灵敏度、再现性均令人满意,相对标准偏差约为32.20%。
First, in this paper, benzofluorenone spectrophotometric determination of trace Sn temperature, dispersant, stabilizer, developer concentration and other conditions were tested, put forward suitable for this type of sample Sn determination of the amount. In the medium of 7N H_2SO_4-0.5N KI, SnI_4 was extracted with benzene, Sn was separated from TiO_2, and stripped with 10% H_3SO_4-3% H_2O_2 (10: 1) Very well separated. Third, using (NH_4) _2SO_4-H_2SO_4 high temperature dissolved TiO_2 sample, the concentrated solution after the solution was frozen, and then directly extracted. Finally, in the 1.2 N H 2 SO 4 medium, polyvinyl alcohol was used as the dispersant and phenyl fluorenone spectrophotometric method was used to determine Sn. The sensitivity and reproducibility were all satisfactory with the relative standard deviation of 32.20%.