Characterization of Polymer Monoliths Containing Embedded Nanoparticles by Scanning Transmission X-ray Microscopy (STXM)

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• 作者：R. Dario Arrua ; Adam P. Hitchcock ; Wei Boon Hon ; Marcia West ; Emily F. Hilder
• 刊名：Analytical Chemistry
• 出版年：2014
• 出版时间：March 18, 2014
• 年：2014
• 卷：86
• 期：6
• 页码：2876-2881
• 全文大小：283K
• 年卷期：v.86,no.6(March 18, 2014)
• ISSN：1520-6882

文摘

The structural and chemical homogeneity of monolithic columns is a key parameter for high efficiency stationary phases in liquid chromatography. Improved characterization techniques are needed to better understand the polymer morphology and its optimization. Here the analysis of polymer monoliths by scanning transmission X-ray microscopy (STXM) is presented for the first time. Poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) [poly(BuMA-co-EDMA)] monoliths containing encapsulated divinylbenzene (DVB) nanoparticles were characterized by STXM, which gives a comprehensive, quantitative chemical analysis of the monolith at a spatial resolution of 30 nm. The results are compared with other methods commonly used for the characterization of polymer monoliths [scanning electron microscopy (SEM), transmission electron microscopy (TEM), mercury porosimetry, and nitrogen adsorption]. The technique permitted chemical identification and mapping of the nanoparticles within the polymeric scaffold. Residual surfactant, which was used during the manufacture of the nanoparticles, was also detected. We show that STXM can give more in-depth chemical information for these types of materials and therefore lead to a better understanding of the link between polymer morphology and chromatographic performance.