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85034517936
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note
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Typical polymerizations are as follows. Solution: A dry roundbottom flask was charged with CuBr and dNbpy. The flask was sealed with a rubber septum and was cycled between vacuum and argon three times to remove the oxygen. Degassed monomer and solvent were added using degassed syringes. The flask was immersed in an oil bath held by a thermostat at the desired temperature and allowed to stir until the mixture became homogeneous. Then, BPO, dissolved in a small amount of monomer, was added dropwise. At timed intervals, samples were withdrawn from the flask using a degassed syringe and added to THF. Bulk: To a dry glass tube with copper halide and dNbpy under argon was added a solution of BPO dissolved in the monomer. Three freezepump-thaw cycles were performed, and the tube was sealed under vacuum and placed in an oil bath held by a thermostat at the desired temperature. The polymerization was stopped by cooling the tube in ice-water. Afterward, the tube was opened and the contents were dissolved in THF.
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note
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The calculated molecular weight Mn,Cai = ([M]o/[BPO]0) x (MW)o x conversion, where [MJo and [BPO]o represent the initial concentrations of monomer and BPO and (MW)o is the molecular weight of the monomer. The apparent initiator efficiency = Mn,ca/^n,SEC, includes both the intrinsic initiator efficiency and any contribution from termination of the growing chains.
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0030662031
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