摘要
Abstract
With the increasing application of liquid chromatography in fields such as pharmaceutical analysis and biological separation,the requirements for key mobile-phase solvents have become increasingly stringent.Chromatographic-grade acetonitrile,which is one of the most commonly used solvents,must meet rigorous standards for ultraviolet(UV)transmittance,baseline stability,and batch-to-batch consistency.Industrial-grade acetonitrile was employed as the raw material.A purification process integrating oxidation,adsorption,and rectification was systematically implemented.A removal method for trace water in acetonitrile,a critical impurity affecting the UV performance,was thoroughly investigated.Challenges associated with water removal,including its strong interactions and potential azeotropic behavior,were analyzed and discussed.Furthermore,key operational parameters for the rectification column,namely,the flooding velocity and pressure drop,were examined and optimized to ensure stable and efficient operation,enabling the continuous,multi-batch production of high-purity chromatographic-grade acetonitrile on a pilot scale.The obtained product exhibited exceptional performance;the UV absorbance was as low as 0.002～0.026 across the 195～280 nm wavelength range,accompanied by a flat and clean baseline free from extraneous peaks.Notably,the absorbance at the highly demanding 190 nm wavelength was consistently controlled below 0.015.A comprehensive evaluation confirmed that all critical performance indicators of the product surpassed those of commercially available Merck products.Practical application demonstrated that this technical route features a rational process design,stable and reliable operation,and excellent product quality.This method was particularly suitable for the large-scale production of high-purity chromatographic-grade acetonitrile.This study provided reliable technical support and a viable material solution for high-end analytical and detection applications,offering a competitive alternative for domestic supply in this specialized sector.关键词
分子筛/色谱乙腈/活性炭/精馏/吸附Key words
molecular sieves/chromatographic-grade acetonitrile/activated carbon/distillation/adsorption分类
化学化工
