Methacrylate-based monolithic column was prepared in fused-silica capillary (80 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer; ethylene dimethacrylate as crosslinker; 1-propanol, 1,4-butanediol, and water as porogenic solvents. The monolith matrix was modified with trimethylamine to create strong anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by using Scanning Electron Microscope (SEM). This column had good mechanical stability and permeability. The effects of various mobile phases for separation of inorganic anions were investigated. Iodate, bromate, nitrite, bromide, and nitrate were separated within 11 min using 100 mM potassium chloride as mobile phase and detected at 210 nm. This method showed good precision of retention time, acceptable linearity and good sensitivity. Under the optimum condition, the RSD of the retention time was in the range of 1.09% -1.75% (n = 6). The calibration curve showed linear relationships between the peak area and the concentration. The limits of detection (LOD) and the limits of quantitation (LOQ) were between 0.08 -0.18 mM and 0.26 -0.61 mM, respectively. This method was applied to the determination of inorganic anions in tap water and ground water samples.
This research describes preparation and characterization of long alkyl chain methacrylate-base monolith for using as stationary phase in capillary liquid chromatography. Preparation of monolithic column were used dodecylmethacrylate as monomer, ethylene dimethacrylate as crosslinker and used a binary porogenic solvent consist of 1.4-butanediol and other 4 various porogen: ethanol, 1-propanol, isoamyl alcohol and isobutyl alcohol. The monolith column were prepared in 100 × 0.32 mm i.d. capillaries column and were optimized in effect of various mobile phase and effect of concentration of mobile phase for separation alkyl benzene compound. Morphology of monolithic column were characterized using scanning electron microscopy. Permeability of column (K o) was measured by pumping water through to the column with different linear flow rate. The resulting monolithic column with 1.4-butanediol and 1-propanol as porogen have good performed in separation of alkyl benzene compound with acetonitrile-water (80:20) as mobile phase.
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