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Visible light initiated polymerization of styrenic monolithic stationary phases using 470 nm light emitting diode arrays
Author(s) -
Walsh Zarah,
Levkin Pavel A.,
Jain Vijay,
Paull Brett,
Svec Frantisek,
Macka Mirek
Publication year - 2010
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200900624
Subject(s) - polymerization , materials science , monolithic hplc column , capillary electrochromatography , monolith , capillary action , analytical chemistry (journal) , divinylbenzene , styrene , chromatography , polymer , chemistry , copolymer , composite material , biochemistry , catalysis
Poly(styrene‐ co ‐divinylbenzene) monolithic stationary phases have been synthesized for the first time by photoinitiated polymerization. An initiator composed of (+)‐( S )‐camphorquinone/ethyl‐4‐dimethylaminobenzoate/ N‐ methoxy‐4‐phenylpyridinium tetrafluoroborate was activated using a 470 nm light emitting diode array as the light source. Spatially controlled polymerization of styrenic monoliths has been achieved within specific sections of a 100 μm id polytetrafluoroethylene‐coated fused‐silica capillary using simple photo masking. The sharpness of the edges was confirmed by optical microscopy, while SEM was used to verify a typical porous, globular morphology. Flow resistance data were used to assess the permeability of the monoliths and they were found to have good flow through properties with a flow resistance of 0.725 MPa/cm at 1 μL/min (water, 20°C). Conductivity profiling along the length of the capillary was used to assess their lateral homogeneity. Monoliths which were axially rotated during polymerization were found to be homogeneous along the whole length of the capillary. The monolithic stationary phases were applied to the RP gradient separation of a mixture of proteins. Column fabrication showed excellent reproducibility with the retention factor ( k ) having a RSD value of 2.6% for the batch and less than 1.73% on individual columns.