We have developed a closed-system combustion technique and utilized it to progressively oxidize a gas-rich, highly carbonaceous acid residue and a fine-grained (<4 μm) matrix sample from the Allende C3V meteorite and analyze the released gases mass spectrometrically. For the residue complete gas mobilization occurs at temperatures below 600°C. The temperature interval over which most of the gases are released coincides with that for combustion of most of the carbon. Release is primarily due to chemical attack rather than thermal activation of the gases. There are somewhat different oxidation thresholds for the heavy gases (Ar, Kr, and Xe) and the light gases (He, Ne), indicating chemically different sites for the two groups. Relative enhancement of isotopically anomalous components near 600°C is as large as in any open-system oxidation method. Differential combustion of the matrix sample reveals three distinct outgassing peaks, the first matching the release from the carbonaceous residue (“combustibles”), the second attributed to sulfides, and the third tentatively assigned to silicates. They comprise about 53%, 7% and 40% of the total heavy gases respectively. While the “sulfides” exhibit a small fission-like component, the Xe in the “silicates” appears isotopically uniform with roughly AVCC composition. The “combustibles” of the matrix contain relatively less excess 129Xe than the residue, perhaps indicating that ∼10% of the total 129Xe in the residue was acquired from “silicates” by redistribution during acid treatment. We cannot rule out the possibility that planetary gases assigned to “sulfides” or “silicates” actually reside in carbonaceous phases somehow sheltered within soluble mineral assemblages, or in acid-soluble carbonaceous phases resistant to oxidation. Integrated releases below and above 600°C during the matrix combustion exhibit virtually identical heavy gas elemental composition, implying similar fractionation during planetary gas entrapment in various materials or in the same material in various environments.
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