Matyjaszewski, K.; Nakagawa, Y. Macromol. Rapid Commun. 1997, 18, 1057-1066. Sodium azide was however used instead of trimethylsilyl azide in the derivatization reaction of the bromide end group into the azide one. The amine functionality of PS was estimated by the fraction of the chains that reacted with anth-PMMA-PA (12K) in dry THF at 50 °C for 48 h. The anhydride/NH2 molar ratio was 5 or higher. Just before SEC-UV analysis, a few drops of phenylisocyanate were added to the reaction mixture in order to complete (if necessary) the amine consumption. Detection of anthracene at 366 nm allowed for the direct quantification of the anth-PMMA-PA conversion into diblock and, thus, of the PS end-functionality.
Moon, B.; Hoye, T.R.; Macosko, C.W. Submitted to Polymer.