Hanang volcano is the southern volcano of, the southern area of the east part of the East African Rift (the North Tanzanian Divergence) and represents volcanic activity of the first stage of continental break-up. In this study, we investigate glassy melt inclusions in nepheline phenocrysts to constrain the late stage of Mg-poor nephelinite evolution and the behaviour of volatiles (CO2, H2O, S, F, Cl) during magma storage and ascent during early stage rifting. The melt inclusions have a green silicate glass, a carbonate phase and a shrinkage bubble free of gas phase indicating that carbonatite:silicate (18:82) liquid immiscibility occurred during nephelinite magmatic evolution. The silicate glasses have trachytic composition (Na + K/Al = 1.6–7.2, SiO2 = 54–65.5 wt%) with high CO2 (0.43 wt% CO2), sulfur (0.21–0.92 wt% S) and halogens (0.28–0.84 wt% Cl; 0.35–2.54 wt% F) contents and very low H2O content (<0.1 wt%). The carbonate phase is an anhydrous Ca-Na-K-S carbonate with 33 wt% CaO, 20 wt% Na2O, 3 wt% K2O, and 3 wt% S. The entrapped melt in nepheline corresponds to evolved interstitial CO2-rich phonolitic composition (Na + K/Al = 6.2–6.9) with 6 ± 1.5 wt% CO2 at pressure of 800 ± 200 MPa after crystallization of cpx (17%), nepheline (40%) garnet (6.5%) and apatite (1.7%) from Mg-rich nephelinitic magma. During ascent, immiscibility in phonolitic melt inclusions leads to Ca-Na carbonate melt with composition within the range of carbonate melt from Oldoinyo Lengai and Kerimasi, in equilibrium with trachytic silicate melt (closed-system, P < 500 MPa). The CO2-rich phonolitic melt inclusions from Hanang volcano may represent an early stage of differentiation before Na‑carbonatitic magmatism observed at Oldoinyo Lengai.