In recent experiments we accidentally observed the onset of nanophase segregation in concentrated LiCl-water solutions by increasing dilution, in the deeply undercooled regime. We could assign an unexpected extra-signal observed in Traansient Grating spectra to the formation of clusters of most likely pure water of nanometre size (3-5 nm). This result was further corroborated by SANS and SAXS experiments, but the high background contribution from the cryostat prevented a quantitative analysis of the size and cluster distribution. Here we propose to take advantage of the unique Q-range of the Nimrod spectrometer to measure in a single scan the onset of the observed heterogeneities, and the evolution of the cluster distribution. The observation of nanophase segregation could provide an alternative interpretation to the highly debated liquid-liquid transition observed in aqueous solutions