NIR spectroscopy is a valuable tool for many industries, especially those that need rapid moisture analysis. NIR absorption spectroscopy has not been applied to highly branched (or dendritic) polymers such as hyperbranched polymers and dendrimers. Our research investigates the advantages and disadvantages of using NIR absorption spectroscopy to quantitate the hydroxyl functional group density, called Hydroxyl Number, simultaneously with the analysis of water content in a dendritic polymer sample. Hydroxyl-surface dendrimers are expensive which presents a sample size problem, and they are highly soluble in protic solvents which interferes with analysis. This research will demonstrate a methodology to overcome these challenges which allows the simplicity, ease, and quantitative power of NIR spectroscopy to be applied to dendritic polymer analysis.