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Abstract: A spectroscopic investigation of the binding of mono- and diketones to template-functionalized network copolymers of styrene-m- diisopropenylbenzene is reported. Quantitative analysis of the binding modes of a substrate molecule (1,3-diacetylbenzene) to a difunctional polymer site was obtained by empirical calibration of FT-IR and C-13 CP/MAS NMR data. The two spectroscopic techniques provide a consistent representation of the manner in which 1,3- diacetylbenzene binds to the difunctionalized polymer site. The analysis also provides an opportunity to quantify site isolation within the polymer and the fidelity with which the functionalized site is maintained by the network polymer. Time-dependent binding studies yield information that aids in the analysis of the method by which template-functionalized polymers affect their recognition properties and calls attention to fundamental differences that exist in binding phenomena between naturally occurring macromolecules (proteins) and synthetic high polymers