Methacrylate monolithic columns of 320 μm I.D. for capillary liquid chromatography

• Published in: Journal of Chromatography A Vol. 946; no. 1; pp. 99 - 106
• Main Authors: Coufal, Pavel, Čihák, Martin, Suchánková, Jana, Tesařová, Eva, Bosáková, Zuzana, Štulı́k, Karel
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 08.02.2002; Elsevier
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Exact sciences and technology; Methacrylate; Other chromatographic methods; Monolithic columns; Stationary phases, LC; Methacrylate; Capillary column; Performance evaluation; Anthracene; Flow rate; Toluene; Monolithic column; HPLC chromatography; Retention factor; Experimental study; Retention time; Porous material; Operating conditions; Phenol; Ultraviolet detector; Aniline; Plate efficiency; Preparation; Height equivalent to a theoretical plate; Radical copolymerization; Uracil; Butyl methacrylate copolymer; Stationary phase
• ISSN: 0021-9673
• DOI: 10.1016/S0021-9673(01)01570-9

Monolithic capillary columns (320 μm I.D.) were prepared for capillary liquid chromatography (CLC) by radical polymerization of butylmethacrylate (BMA) and ethylenedimethacrylate (EDMA) in the presence of a porogen solvent containing propan-1-ol, butane-1,4-diol and water. The influence of the contents of the porogen solvent and EDMA in the polymerization mixture on the monolith porosity and column efficiency was investigated. The composition of the polymerization mixture was optimized to attain a minimum HETP of the order of tens of μm for test compounds with various polarities. The separation performance and selectivity of the most efficient monolithic column prepared was characterized by van Deemter curves, peak asymmetry factors and Walters hydrophobicity and silanol indices. It was demonstrated that the 320-μm I.D. monolithic column exhibited CLC separation performance similar to that observed for 100- and 150-μm I.D. monolithic columns reported in the literature; moreover, the 320-μm I.D. column was easier to operate in CLC and exhibited a higher sample loadability.