Unaltered metasediments of the Mary Kathleen Fold Belt are composed predominantly of layered amphibolite-facies scapolitic calc-silicate rocks in which minimal infiltration of externally derived fluids occurred during regional metamorphism. There were substantial differences in volatile activities between different layers in the layered sequences, in particular: aCO2/aH2O inferred from reaction progress estimates and analysis of biotite-clinopyroxene-fluid phase relations; aNaCl/aH2O inferred from scapolite compositions; and aHCl/aH2O inferred from biotite compositions. In one outcrop in which a clinopyroxene-producing reaction dominated, differences in approximate XCO2of up to 0.25 occurred between several samples collected over 50 metres. Variations in aH2O/aHCl of up to one order of magnitude are inferred at 1 to 50 m scales from biotite-Cl contents, and variations in NaCl contents of scapolite from 0.0 to up to 0.6 Cl atoms in the Cl-CO3-SO4 site reflect a large variation of aNaCl in the coexisting fluid at similar scales. Most calcsilicate layers internally buffered fluid compositions in the H2O-CO2-NaCl-HCl system. Local occurrences of NaCl-rich scapolite suggest that some layers may have been in equilibrium with halite during early prograde metamorphism. At peak metamorphic temperatures, disolution of halite was complete but layers containing high-NaCl scapolite continued to buffer fluid at high values of aNaCl. Fluid immiscibility does not appear to have affected the progress of the devolatilization reactions. Although fluid was predominantly internally buffered, moderate quantities of fluid were released by prograde mineral reactions in many layers, up to 30 cm3 fluid per 100 cm3 rock. Numerous episodes of fluid escape were required, probably via microfractures, such that the released fluid did not obviously influence reaction progress in the layers through which it passed. The anomaly of beautifully preserved internal buffering signatures and the requirement for produced fluid locally to pass across layers in a deforming rock sequence suggest that the escaping fluid did not leave any readily observable tracks. This is explained by rapid rates of fracture propogation and fluid migration therein. This internally buffered system contrasts strongly with adjacent calc-silicate rocks that show evidence for infiltration of externally derived fluids at high fluid/rock ratios, and highlights the broad range of fluid behaviour that can be expected in deforming, heterogeneous rock sequences.