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Nuclear magnetic resonance (NMR) spectroscopy is used to investigate the chemical composition of organic aerosol in terms of functional group distribution with a special focus on secondary organic aerosol (SOA) formation. The knowledge of the functional group composition is a benchmark for understanding how SOA components partition into the particulate phase and undergo chemical transformation. The paper presents a new chemical derivatization procedure coupled to proton NMR (H-1 NMR) analysis for the specific determination of total carbonylic groups in atmospheric aerosol samples, which couples with the procedure for determination of total carboxylic acid groups described in a previous work. A first deployment of the combined techniques for the analysis of PM10 samples collected in the Po Valley in the warm season shows that the concentration in the particulate phase of total carbonyls varies and covaries with respect to those of carboxylic acids and of less-oxidized functional groups. The proposed methodology provides the breakdown of the oxygenated fraction of the organic aerosol into major functional groups through well-established chemical methods and can be used to benchmark the more sensitive and widely used aerosol mass spectrometric techniques.