Performance Study of Carbon–Clad Zirconia Stationary Phase in High Temperature Reversed–Phase High Performance Liquid Chromatography

Abstract

Prestasi turus zirkonia tersalut karbon (CCZ) telah dikaji bagi pemisahan sebatian ujian (benzaldehid, benzamida, nitrobenzena, dan toluena) dan alkil aril keton (asetofenon, propiofenon, butirofenon, dan valerofenon) dalam sistem kromatografi cecair prestasi tinggi fasa terbalik (RP–HPLC) pada suhu tinggi (100°C–160°C) menggunakan fasa bergerak dengan pelarut organik berkomposisi rendah dan lOO% air tulen. Mekanisme pemisahan yang lebih baik dan masa analisis yang lebih pendek diperolehi apabila pengoperasian sistem pada suhu tinggi dijalankan. Lakaran keluk Van’t Hoff yang linear bagi turus CCZ membuktikan bahawa tiada perubahan mekanisme penahanan terhadap sebatian analit terpilih pada julat suhu yang dikaji. Siri homolog alkil aril keton telah digunakan sebagai skala indeks penahanan dalam pembangunan indeks penahanan dalam sistem RP–HPLC suhu tinggi. Walaupun faktor muatan sebatian ujian itu amat dipengaruhi oleh perubahan suhu turus, namun perubahan nilai indeks penahanan sebatian berkenaan adalah kecil. Kata kunci: Karbon tersalut zirkonia, kromatografi cecair prestasi tinggi pada suhu tinggi The performance of carbon–clad zirconia (CCZ) stationary phase was evaluated for the separations of test compounds (benzaldehyde, benzamide, nitrobenzene, and toluene) and alkyl aryl ketones (acetophenone, propiophenone, butyrophenone and valerophenone) at high temperature (100°C–160°C) in reversed–phase high performance liquid chromatography (RP–HPLC) using low compositions of organic modifier and 100% pure water as eluent. Improved separation mechanism and faster analysis time were achieved during high operating temperatures. Van’t Hoff plots were linear for the investigated CCZ column, which showed that over the temperature range, no changes occurred in the retention mechanism. The use of alkyl aryl ketone homologs as a retention index scale in high temperature RP–HPLC was investigated. Although the retention factors of the test compounds were greatly affected by increasing the column temperature, there were only slight variations in their respective retention index values. Key words: Carbon-clad zirconia, high temperature high performance liquid chromatography