The correct response to your changes of the experimental conditions will be presented directly and can momentarily be used for planning the next experimental step. • Rapid catalyst screening |
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Experiment The experiment below describes a screening test of a fast initiator system for the emulsion polymerization of vinyl acetate at 55°C. The initiator system was composed of hydroperoxide, a catalytic metal ion and ascorbic acid. The pressure syringe from ChemiSens was used for small additions of reactants through a rubber septum into the reactor. The hydroperoxide was used as a water solution. To minimize the thermal disturbances from the additions, the syringe was easily preheated in the CPA thermostatting bath. A. The first addition of hydroperoxide resulted in a slow response. Probably due to residuals of inhibitor in the monomer. B. By increasing the concentration of the metal ion catalyst (vanadium-oxo-sulfate) the activity of the initiator system was promoted. C. A new addition of hydroperoxide gave a pronounced rate peak. D. To further increase the initiator activity a new addition of the metal ion catalyst was made. E, F. By further additions of both hydroperoxide and more metal ion catalyst the system was easily tested for suitable half-life times for the initiator system. |
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