摘要
用高效液相色谱法分析精对苯二甲酸残渣,考察了适宜的操作条件。实验结果表明,在采用阴离子交换柱作分析柱,浓度为0.2 mol/L的磷酸二氢铵缓冲液为流动相、体积分数为10%的甲醇作有机改性剂、用磷酸调试样pH为6～7、检测波长为240 nm的最佳条件下,分离效果最好,对羧基苯甲醛、苯甲酸、对甲基苯甲酸、邻苯二甲酸、对苯二甲酸、间苯二甲酸、1,2,4-苯三酸、1,3,5-苯三酸的加标回收率分别为98.39%,98.81%,98.66%,97.73%,98.93%,98.90%,98.25%,98.40%。相对标准偏差分别为0.87%,0.49%,0.76%,0.88%,0.71%,0.46%,0.63%,0.47%,方法的检出限分别为0.1,0.2,0.1,0.4,0.1,0.4,0.6,2.0 mg/L,线性范围分别为0.88～17.50,1.48～29.60,1.47～29.30,1.34～26.80,1.79～35.80,2.70～53.90,2.98～59.50,3.00～59.90 mg/L。
The residue of pure terephthalic acid was analyzed by high performance liquid chromatography. The experimental results show that the separation effect is the best under the optimum operating conditions of using negative ion exchange column as working column, NH4H2PO4 solution with 0.2 mol/L of concentration as mobile phase, methanol solution with 10% of volume fraction as organic modifier, adjusting pH between 6 to 7 with H3PO4 and wavelength for detection 240 nm. The recovery of added standard 4-carboxy-benzaldehyde, benzoic acid, p-toluic acid, phthalic acid, terephthalic acid, isophthalic acid, 1,2,4-Benzenetricarboxylic and 1,3,5-Benzenetricarboxylic is 98.39%, 98.81%, 98.66%, 97.73%, 98.93%, 98.90%, 98.25% and 98.40%, respectively; The relative standard deviation is 0.87%, 0.49%, 0.76%, 0.88%, 0.71%, 0.46%, 0.63% and 0.47%, respectively; The detection limit is 0. 1, 0. 2, 0. 1, 0. 4, 0. 1, 0. 4, 0. 6, 2. 0 mg/L, respectively; And the linear range is 0.88 - 17.50, 1.48 - 29.60, 1.47 - 29.30, 1.34 - 26.80, 1.79 - 35.80, 2.70 - 53.90, 2.98 - 59.50, 3.00 - 59.90 mg/L, respectively.
出处
《化工环保》
CAS
CSCD
北大核心
2008年第1期85-88,共4页
Environmental Protection of Chemical Industry
关键词
高效液相色谱法
精对苯二甲酸
残渣
分析方法
high performance liquid chromatography
pure terephthalic acid
residue
analytical method
