Azido-functionalized poly(ethylene glycol) (PEG) derivatives are finding ever-increasing applications in the areas of conjugation chemistry and targeted drug delivery by their judicious incorporation into nanoparticle-forming polymeric systems. Quantification of azide incorporation into such PEG polymers is essential to their effective use. H-1 Nuclear Magnetic Resonance (NMR) analysis offers the simplest approach; however, the relevant adjacent azide-bearing methylene protons are often obscured by the PEG manifold signals. This study describes the synthesis of 1,2,3-triazole adducts from their corresponding PEG azides via a convenient, mild click reaction, which facilitates straightforward NMR-based quantitative end-group analysis. This method was found to be compatible with many examples of bifunctional azido PEGs with molecular weights ranging from 2 to 18 kDa bearing a variety of functional groups. (C) 2016 The Authors. Journal of Polymer Science Part A: Polymer Chemistry Published by Wiley Periodicals, Inc.