Formation evaluation of unconventional reservoirs is Challenging due to, the coexistence of different phases such as, kerogen, bitumen, movable and bound light hydrocarbon and water. Current low-frequency (0.05 T) nuclear magnetic resonance (NMR) laboratory and logging method's are incapable of quantitatively separating the different phases. We demonstrate the utility of high-field (9.4 T) NMR 2D T-1-T-2, measurements for separating hydrocarbon and the clay-interacting aqueous phases in shale based on the difference in the frequency dependence of the spin lattice relaxation time. Furthermore, we demonstrate Na-23 NMR as a promising complementary technique to conventional H-1 NMR for shale fluid typing, taking advantage of the fact that sodium ions are only present in the aqueous phase. We validate high-field (9.4 T) Na-23-H-1 NMR relaxometry for assessing brine-filled porosity and brine salinity in various porous materials, including porous glass, conventional rocks, clays, and shale, and apply it for differentiating hydrocarbon versus aqueous components and also the clay-associated versus free water in Eagle Ford shale cores. This work lays the groundwork for developing future downhole Na-23-H-1 NMR logging techniques.