Monodisperse porous poly(vinyl acetate-co-divinylbenzene) particles by single-stage seeded polymerization: A packing material for reversed phase HPLC

A single‐stage swelling and polymerization method was proposed for the synthesis of monodisperse porous poly(vinyl acetate‐co‐divinylbenzene) [poly(VAc‐co‐DVB)] particles with different VAc/DVB feed ratios. The particles obtained with the VAc/DVB feed ratio of 50:50 v/v had a narrow pore size distri...

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Veröffentlicht in:Journal of separation science 2006-05, Vol.29 (7), p.936-944
Hauptverfasser: Çaglayan, Berna, Unsal, Ender, Çamli, S. Tolga, Tuncel, Murvet, Tuncel, Ali
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Sprache:eng
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Zusammenfassung:A single‐stage swelling and polymerization method was proposed for the synthesis of monodisperse porous poly(vinyl acetate‐co‐divinylbenzene) [poly(VAc‐co‐DVB)] particles with different VAc/DVB feed ratios. The particles obtained with the VAc/DVB feed ratio of 50:50 v/v had a narrow pore size distribution exhibiting a sharp peak at 30 nm. Based on this distribution the mean pore size and the specific volume were determined as 12 nm and 1.39 mL/g, respectively. The specific surface area of poly‐(VAc‐co‐DVB) particles was found to be 470 m2/g. These properties make poly(VAc‐co‐DVB) particles a promising support for potential HPLC applications. Poly(vinyl alcohol‐co‐divinylbenzene) [poly(VA‐co‐DVB)] particles were then obtained by the basic hydrolysis of poly(VAc‐co‐DVB) particles. The hydroxyl groups on poly(VA‐co‐DVB) particles have a suitably reactive functionality for surface grafting or derivatization protocols aiming at synthesizing various HPLC packings. The examination of poly(VA‐co‐DVB) particles by confocal laser scanning microscopy showed the homogeneous distribution of hydroxyl functionality in the particle interior. As a starting point, the chromatographic performance of plain material, poly(VAc‐co‐DVB) particles produced with VAc/DVB feed ratio of 50:50 (v/v) was tested by a commonly utilized chromatographic mode, reversed phase chromatography. Poly(VAc‐co‐DVB) particles were successfully used as packing material in the RP separation of alkylbenzenes with resolutions higher than 1.5. Theoretical plate numbers up to 17 500 plates/m were achieved. No significant change both in the chromatographic resolution and column efficiency was observed with increasing flow rate. The chromatography showed that poly(VAc‐co‐DVB) particles were a suitable starting material for the synthesis of chromatographic packings for different modes of HPLC.
ISSN:1615-9306
1615-9314
DOI:10.1002/jssc.200500499