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In this paper, time-of-flight secondary ion mass spectrometry (ToF-SIMS) was investigated as a tool for analyzing changes on mineral grains (siderite and ankerite) caused by dissolution and precipitation processes. Carbon dioxide capture and sequestration is a technique investigated for its possible employment in the reduction of the amount of anthropogenic CO2 gas emitted into the atmosphere. Deep saline aquifers are one option for storing CO2 gas streams produced, e.g. by the combustion of fossil fuels at power plants. These gas streams contain different impurities depending on their origin, among them O2, NOx, SOx in addition to CO2. Geochemical experiments under in-situ pressure and temperature conditions of possible geological storage sites were performed, and preparation techniques for the solid products were developed for 3D analysis. The results show that it is possible to analyze the alterations that occur on the surface of siderite grains during CO2 or CO2/O2 exposures under CO2 storage site conditions.