Biotechnology Research Lab., Faculty of Petroleum and Chemical Engineering, Razi University, Kermanshah 67149-67346, Iran.
Biotechnology Research Lab., Faculty of Petroleum and Chemical Engineering, Razi University, Kermanshah 67149-67346, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Apr 15;1083:146-159. doi: 10.1016/j.jchromb.2018.03.009. Epub 2018 Mar 8.
The present study evaluates the capability of ion exclusion chromatography (IEC) of short chain aliphatic carboxylic acids using a cation exchange column (8% sulfonated cross-linked styrene-divinylbenzene copolymer) in different experimental conditions. Since one of the prerequisites to the development of an efficient carboxylic acid separation process is to obtain the optimum operational conditions, response surface methodology (RSM) was used to develop an approach to evaluate carboxylic acids separation process in IEC columns. The effect of the operating conditions such as column temperature, sulfuric acid concentration as the mobile phase, and the flow rate was studied using Central Composite Face (CCF) design. The optimum operating conditions for the separate injection of lactic acid and acetic acid is temperature of 75 °C, sulfuric acid concentration of 0.003 N for both acids and flow rate of 0.916 (0.886) mL/min for acetic acid (lactic acid). Likewise, the optimum conditions for the simultaneous injection of acetic and lactic acid mixture are the column temperature of 68 °C, sulfuric acid concentration of 0.0003 N, and flow rate of 0.777 mL/min. In the next step, the adsorption equilibria of acetic acid and lactic acid on the stationary phase were investigated through a series of Frontal Analysis (FA), Frontal Analysis by Characteristic Points (FACP), and using Langmuir isotherm model. The results showed an excellent agreement between the model and experimental data. Finally, the results of thermodynamic studies proved that the IEC process for separation of acetic and lactic acid is a spontaneous, feasible, exothermic, and random process with a physical adsorption mechanism. The results of the current paper can be a valuable information in the stages of designing IEC columns for separation of aliphatic carboxylic acids.
本研究评估了在不同实验条件下使用阳离子交换柱(8%磺化交联苯乙烯-二乙烯基苯共聚物)进行短链脂肪族羧酸的离子排斥色谱(IEC)的能力。由于开发有效的羧酸分离过程的前提之一是获得最佳操作条件,因此使用响应面法(RSM)来开发一种评估IEC 柱中羧酸分离过程的方法。通过中心复合面(CCF)设计研究了操作条件(如柱温、硫酸浓度作为流动相和流速)的影响。分别注射乳酸和乙酸的最佳操作条件是温度为 75°C,两种酸的硫酸浓度均为 0.003N,流速为 0.916(0.886)mL/min 用于乙酸(乳酸)。同样,同时注射乙酸和乳酸混合物的最佳条件是柱温 68°C,硫酸浓度为 0.0003N,流速为 0.777mL/min。在下一步中,通过一系列前沿分析(FA)、特征点前沿分析(FACP)以及使用 Langmuir 等温线模型研究了乙酸和乳酸在固定相上的吸附平衡。结果表明模型与实验数据之间具有极好的一致性。最后,热力学研究的结果证明,IEC 过程用于分离乙酸和乳酸是自发的、可行的、放热的和随机的过程,具有物理吸附机制。本研究的结果可为设计用于分离脂肪族羧酸的 IEC 柱的各个阶段提供有价值的信息。