Diffuse reflectance FTIR (DRIFT) was established as a high throughput characterization method for classic copolymer systems. Four different methyl methacrylate-based polymer libraries with styrene, N-vinylpyrrolidone, 4-vinylpyridine, or 2-carboxyethyl acrylate as comonomers were synthesized using an automated/robotic synthesizer platform, and analyzed by ¹H NMR and DRIFT. By multivariate data analysis both data sets were compared and correlations with R² between 0.9373 and 0.9971 could be achieved. By this means high throughput screening of comonomer contents of these polymer libraries was enabled.