Iron(II) oxide determination in rocks and minerals

The determination of FeO of geologic materials by modern instrumental methods (such as atomic absorption spectroscopy (AAS), inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray fluorescence (XRF), etc.) cannot distinguish between different oxidation states of elements. In many cases, the oxidation state of Fe has to be known in order to perform several chemical calculations (norms, etc.) and discuss the reactions that occur during weathering, hydrothermal alteration and other processes. A modified Wilson method is proposed, giving reproducible results in a much shorter time than the classical method. Back-titration with potassium dichromate and an Fe(II) and ammonia sulphate solution is used, after dissolution of the sample powder in a heated HF/H3PO4 mixture and an ammonium vanadate solution. This modified method, tested with several international reference materials, gives reliable results, equivalent to the ones cited in the literature for the reference materials.