The use of diethanolamine/DMSO-d 6 as viscous binary solvent is reported for the individualization of low-polarity mixture components by heteronuclear ViscY NMR experiments under spin diffusion conditions. Solvent viscosity induces the slowing down of molecular tumbling, hence promoting magnetization transfer by dipolar longitudinal cross-relaxation. As a result, all 1 H nuclei resonances within the same molecule may correlate in a 2D NOESY spectrum, giving access to mixture analysis. We state the individualization of four low-polarity chemical compounds dissolved in diethanolamine/DMSO-d 6 solvent blend using homonuclear selective 1D and 2D 1 H and 19 F NOESY and HOESY experiments and heteronuclear