邻氯苯基荧光酮光度法测定聚烯烃树脂中的钛

Determination of Titanium in Polyene Resins and Steel by 2,3,7-Trihydroxy-9-O-Chlorophenylfluorenone Spectrophotometry

研究了以邻氯苯基荧光酮-十六烷基三甲基溴化铵为显色体系,在表面活性剂十六烷基三甲基溴化铵存在下,钛(Ⅳ)和邻氯苯基荧光酮所形成橙红色的络合物,实验结果表明,在酸性介质中钛(Ⅳ)最大吸收波长位于560nm,含量在0～12μg/25mL范围内符合比尔定律,其表观摩尔吸光系数ε_(560)=1.2×10~5L·mol^(-1)·cm^(-1)。聚烯烃树脂的人工合成样中钛(Ⅳ)的平均回收率为101.9%,相对标准偏差为0.36%。采用抗坏血酸掩蔽剂消除了被测样中干扰离子的影响,实验结果表明聚乙烯和聚丙烯中钛(Ⅳ)的含量分别为0.1760μg·g^(-1)、0.6855μg·g^(-1),其加标平均回收率分别为101.7%、99.8%。相对标准偏差分别为1.48%、2.43%。本方法选择性好,灵敏度高,简便易行。

By using the CTMAB as surfactant, the 2,3,7-Trihydroxy-9-O-Chlorophenyl fluorenone-CTMAB as chromogenic agent, Ti（IV） can form a orange colour colored complex with 2,3,7-Trihydroxy-9-O-Chlorophenylfluorenone. The experimental results indicated that in acid medium the maximum absorption wavelength was 560 nm, the apparent molar absorption was 1.2×10~5L·mol^-1 and following Beer＇s law the linear range was 0-- 12 μg/25mL. The average recovery rate of Ti（IV） of synthetic polyene resins sample was 101.9%. The relative standard deviation was 0.36%. Ascorbic acid solution was used as reducer to eliminate the effect of interference during the course of determination. The results indicated that the contents of Ti（ IV ）in polyethylene and polypropylene were 0.1760 lμg·g^-1, 0.6855 μg.g^-1. The average recoveries rates were 101.7% and 99. 8%. The relative standard deviation were 1.48% and 2.43%. This method is selective, sensitive and simple.