Determination and Characterization of Unreacted Hydroxyl Groups in a Cross-Linked Poly(ortho ester) (original) (raw)

1994, Analytical Chemistry

A method is presented for the identification and quantitative determination of unreacted hydroxyl groups in a cross-linked poly(ortho ester) derived from the diketene acetal 3,9-bis-(ethylidene-2,4,8,1O-tetraoxaspiro[5.5]undecane), (A)-1,2,6hexanetriol, 1,641exanedio1, and tetraethylene glycol. This method involves exhaustive derivatization of unreacted hydroxyl groups in the intact polymer in advance of mild hydrolysis followed by gradient HPLC analysis. Each of the derivatized polymer components was synthesized and characterized, and evidence is presented demonstrating that exhaustive derivatization has occurred.