This study was devoted to the evaluation of the effectiveness of Fenton catalysts, based on magnetically-concentrated portions of iron oxide-rich sand fractions from two magnetic Ultisols, derived from volcanic materials of southern Chile. The samples were labeled according to the municipality where the sample sites are geographically located, namely Metrenco and Collipulli, and were characterized with Mossbauer spectroscopy at 298 K and saturation magnetization (σ) measurements. Mossbauer data revealed a complex magnetic hyperfine structure for these magnetic portions from both soil-sand materials, suggesting relatively complex mineral assemblages. The monitored rate of H2O2 decomposition via heterogeneous Fenton reaction revealed that materials from the Collipulli soil are more efficient Fenton catalyst than are those from the Metrenco soil. The reasons for these differences are from now on being explored on basis of a more detailed chemical investigation of these samples.