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出 处:《理化检验(化学分册)》2009年第9期1048-1050,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:浙江省自然科学基金资助项目(Y405377)
摘 要:采用高效液相色谱法同时测定均三甲苯及其氧化生成的均苯三甲酸、3,5-二甲基苯甲酸和5-甲基-1,3苯二甲酸的含量。对色谱分离测定条件做了试验并予以优化。以SHIMADZUC_(18)色谱柱(150 mm×4.6 mm,5μm)为分离柱,以甲醇、水和pH 5.0乙酸盐缓冲溶液以体积比79比20比1的混合溶液为流动相,在检测波长为225 nm处进行测定。均三甲苯和3个氧化产物质量浓度在一定范围内与其峰面积呈线性关系,标准加入回收率分别在99.5%~100.4%,99.7%~100.8%,99.6%~100.8%和99.3%~101.0%之间,相对标准偏差(n=6)均小于2.0%。HPLC was applied to the determinations of the main oxidation and intermediate products of mesitylene, including trimesic acid, mesitylenic acid and 5-methyl-1, 3-benzenedicarboxylic acid. The conditions for separation and determination by HPLC were tested and optimized. The SHIMADZU 1218 column (150 mm×4. 6 mm, 5 μm) was used as stationary phase, and a mixed solution of methanol, water and pH 5. 0 acetate buffer solution (mixed in the a ratio of 79 to 20 to 1) was used as mobile phase. UV-detection at 225 nm was adopted in the determination. Linear relationships between the values of peak area and mass concentration of mesitylene, trimesic acid, mesitylenic acid and 5-methyl-1, 3-benzenedicarboxylic acid in definite ranges were obtained. The values of recovery found by standard addition method were in ranges of 99. 5%- 100. 4%, 99. 7%- 100. 8%, 99. 6%-100. 8% and 99. 3%--101.0% respectively. The values of RSD's (n=6) were less than 2. 0%.
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