Miniaturized catalysis: monolithic, highly porous, large surface area capillary flow reactors constructed in situ from polyhedral oligomeric silsesquioxanes (POSS)† †Electronic supplementary information (ESI) available. See DOI: 10.1039/c5cy00510h Click here for additional data file.
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چکیده
Equipment Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) were performed with a Crossbeam 1540 XB electron microscope to probe the morphological dry-state properties of the prepared materials and existence of desirable chelated palladium functionality. Liquid chromatographic measurements were performed with a 1290 Infinity UHPLC instrument from Agilent Technologies (Agilent, Vienna, Austria). A packed, reversed-phase C18 silica-based chromatographic column (Rapid Resolution HD Eclipse Plus C18, 2.1 mm x 50 mm, particle size 1.8 µm) from Agilent (Vienna, Austria) was used for determination of conversions and yields. Monolith modification procedures as well as catalytic reactions were all performed in flow-through mode by means of a syringe pump (Sigma-Aldrich, Vienna, Austria). Back pressure and porosity measurements of the pristine monolith were performed in 75/25 acetonitrile/water (%, v/v) with a nano-LC instrument (ThermoFischerScientific, Vienna, Austria) featuring a 4 nL injection valve and a UV detector with a 3 nL detection cell volume. For porosity measurements, uracil in 75/25 acetonitrile (%, v/v) was injected and the
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