Chemical reactions at surfaces play crucial roles in many important processes, such as catalysis or bioanalytics. However, methods to analyze the structure and structural changes due to chemical reactions of molecules at a surface under ambient conditions are limited. Traditional NMR spectroscopy, the primary tool for molecular structural analysis, cannot detect weak signals from molecular surface layers. However, highly sensitive NV-quantum sensors are ideal for observing NMR signals from thin nanoscale films. Here this technique is applied to perform molecular structural analysis of surfaces and interfaces. Our first results demonstrate that NV-centers can detect NMR signals from self-assembled monolayers (SAM) and their formation kinetics under chemically relevant conditions (Figure 1). This work was performed in collaboration with Ian Sharp from the WSI. We are currently developing this technique towards studies of surface organic frameworks (MOF), catalytic systems, lipid bilayers, and 2D materials.