A hybrid monolithic column was prepared using octavinyloctasilasesquioxane (OVS) as a monomer, benzoyl peroxide/dimethylacetamide (BPO/DMA) as initiator, ethylene glycol dimethacrylate (EDMA) as cross-linker, 1-dodecanol as porogenic agent and dimethylbenzene as cosolvent. A tidy skeleton, much bigger specific surface area (22.4 m2/g) and lower swelling property of the monolithic column with OVS added than the one without OVS added were determined with Scanning Electron Microscopy (SEM), Nitrogen adsorption/desorption measurements (BET) and swelling test with elute of different concentration of acetonitrile in water. Fourier-transform infrared spectra (FTIR) was taken to characterize the composition of groups. Moreover, a better separation performance for benzene series compounds under reversed phase liquid chromatography (RPLC) mode was obtained using the monolithic columns with OVS added than those without.
Poly(N-isopropylacrylamide-co-hexanediol diacrylate-co-ethylene dimethacrylate) [poly(NIPAAm-co-HDDA-co-EDMA)] monolithic column was prepared via in situ polymerization reaction. In order to investigate the porous properties of the monoliths prepared, the morphology was characterized by the scanning electron microscopy; the chemical group of the monolithic column was confirmed by a Fourier transform infrared spectroscopy method. The surface area was 39.1 m/g by the nitrogen adsorption-desorption experiment. With methanol as the mobile phase, the permeability of the monolithic column was calculated as 3.2330 × 10 m Then it was used as the stationary phase of high performance liquid chromatography. The results indicted that poly(NIPAAm-co-HDDA-co-EDMA) monolithic column was good to separate small molecules by controlling the temperature. Column efficiency for p-chloronitrobenzene was 4,680 plates/m. Repeatability was defined by determining run-to-run and column-to-column variation of the retention times of aromatic compounds, expressed as relative standard deviation (RSD = standard deviation/mean × 100%), and the values were <0.58% and 3.1%, respectively.
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