Samples of cretaceous limestone have been treated with three application methods (poultice, immersion and brushing) using different concentrations of ammonium oxalate solution (AmOx) and varying treatment time in order to test the efficiency of surface and in-depth formation of a protective layer of calcium oxalate (CaOx). Synchrotron-based microanalytical techniques (SR-µXRD with 12.5 µm × 7.5 µm (H × V ) probe size, SR-µFTIR with 10 µm × 10 µm and 8 µm × 20 µm probe sizes) and laboratory µFTIR, XRD and SEM have been employed for analysis of the treated samples. Synchrotron-based techniques showed variations in the CaOx distribution along the surface on a micrometer scale. All treatments resulted in the