Method for determining chloroformate concentration

摘要

The molar concentration of chloroformate in an organic chloroformate solution is determined by adding an excess of a monohydroxyaromatic compound, water and a catalytic amount of a 4-dialkylaminopyridine such as 4-dimethylaminopyridine, titrating with aqueous base and taking as the end point the volume of base which achieves complete conversation of chloroformate groups to monoaromatic carbonate groups, as shown by a rapid rise in the pH of the aqueous phase of more than two points to a value in the range of 7-9. This method is particularly applicable to the determination of bischloroformate molar concentration in systems to be converted to cyclic polycarbonate oligomers. Conversion may be effected by condensation in the presence of a trialkylamine and aqueous base in the amount of about 3 moles per mole of bischloroformate.