Abstract: Chromatographic analysis represents a prevalent technique within modern instrumental analysis. Chromatography, encompassing both gas and liquid chromatographic methods, is a fundamental component of instrumental analysis experiment course in higher education institutions. Despite their shared separation principles, gas chromatography (GC) and liquid chromatography (LC) exhibit distinct characteristics and applications. Leveraging the comparative teaching method, this study involves the execution of chromatographic separation of benzene, toluene and m-xylene using both GC and LC instruments within the framework of an instrumental analysis experimental course. This comparative approach facilitates a deeper understanding and appreciation of chromatographic techniques among students by elucidating the theoretical underpinnings, experimental conditions, operational methodologies, and outcomes associated with each method. Furthermore, this pedagogical strategy serves as a preparatory step for students’ future research endeavors.