Fluorinated monolithic column for CEC

Abstract

In order to overcome the drawbacks associated with particle-based fluorinated stationary phases, a fluorinated cationic monolith was successfully synthesized by the in situ copolymerization of a 45% monomer mixture and 55% porogens with thermal initiation using 0.1% initiator with respect to the monomer mixture. The monomer mixture was composed of perfluorododecyl acrylate (49.75%), ethylene dimethacrylate (49.75%), and 0.5% of the quaternary amine acrylic monomer supporting an anodal electroosmotic flow. A tertiary porogenic solvent system consisting of 40% 1-propanol, 40% 1-octanol, and 20% 1-dodecanol was used. The resulting monolith column showed good characteristics in terms of morphology, permeability (pressure drop was 4.8-25.7 MPa between 5 and 25 μL/min), and the electroosmotic mobility (3.68 (±0.05)×10(-4) cm(2) v(-1) s(-1)). The monolith was tested for the separation of four phenolic compounds, three aromatic hydrocarbons, and one fluorine-containing compound. Good efficiencies (up to 135,000 (±4000) plate/m and resolution up to 2.6 (±0.1)) with short analysis time (< 9 min for tau-fluvalinate, <7 min for four phenolic compounds, and <12 min for three aromatic hydrocarbons) and good stability (1.0-1.5% RSD for intraday, 1.2-1.6% RSD for interday, and 3.9-5.0% RSD for column-to-column) were obtained.

Organic–inorganic hybrid fluorous monolithic capillary column for selective solid‐phase microextraction of perfluorinated persistent organic pollutants

“…), whereas column C (30% monomer mixture) possessed the best permeability with only 850 psi at a flow rate of 6 μL/min (200 μm i.d.× 100 mm, mobile phase: ACN). This was because the density of the monolith skeleton increased with decreasing through‐pore size as the ratio of the monomer stock solution increased .…”

“…Since it was reported that the 1‐octanol played an important role on the preparation of a polymer monolithic column , the column preparation was initially examined with a polymerization mixture consisting of 70% porogens (40% 1‐propanol, 40% 1‐octanol, and 20% 1‐dodecanol) and 30% monomer mixture. 1‐Propanol acts as a microporogen that would affect the surface area, and 1‐dodecanol acts as a macroporogen that would affect the through‐pore size distribution , whereas 1‐octanol would reduce the size of voids and increase the surface area . The ratio of microporogen (1‐propanol) to macroporogen (1‐octanol and 1‐dodecanol) was kept constant at 40:60, and the amount of 1‐octanol was varied from 20 to 40%.…”

“…The inner surface was then functionalized with acrylate groups to facilitate monolith attachment using the reaction procedure described by Aree Choodum et al. . Briefly, the capillary was first flushed with a solution of γ‐MAPS (20%, v/v) in acetone, and then reacted in an oven at 60°C with both ends sealed.…”

“…Compared with particle‐phase sorbents, porous polymer monolithic materials have unique properties such as continuous porous structure, high porosity, and large through‐pore size with small‐size skeletons, resulting in high specific surface area with good column permeability . To synthesize monolithic fluorous phase sorbents, different strategies were proposed . However, all of the fluorous monolith materials were pure organic polymers, which were always swelled by organic solvents, limiting their applications to a great degree.…”

Development of fluorous porous polymer monolith (FPPM) for the capillary electrochromatographic separation of fluorous analytes based on fluorous–fluorous interaction

“…No uorous analyte was used. Choodum et al 23 thermally fabricated a uorous monolith from 1H,1H,2H,2H-peruorodecyl acrylate (PFDA), EDMA, and [2-(methacryloyloxy) ethyl]trimethylammonium methyl sulfate (METAM), the latter being a positively charged component to generate electroosmotic ow for CEC. Polar phenolic compounds (hydroquinone, phenol, and catechol), nonpolar aromatic hydrocarbons (benzene, toluene, and xylene) and only one uorine-containing compound, tau-uvalinate, were separated by the FPPM column.…”