A new method for the identification and quantification of magnetite-maghemite mixture using conventional X-ray diffraction technique

Talanta. 2012 May 30:94:348-52. doi: 10.1016/j.talanta.2012.03.001. Epub 2012 Mar 7.

Abstract

The electrical explosion of Fe wire in air produced nanoparticles containing the binary mixture of magnetite (Fe(3)O(4)) and maghemite (γ-Fe(2)O(3)). The phase identification of magnetite and maghemite by the conventional X-ray diffraction method is not a simple matter because both have the same cubic structure and their lattice parameters are almost identical. Here, we propose a convenient method to assess the presence of magnetite-maghemite mixture and to further quantify its phase composition using the conventional peak deconvolution technique. A careful step scan around the high-angle peaks as (511) and (440) revealed the clear doublets indicative of the mixture phases. The quantitative analysis of the mixture phase was carried out by constructing a calibration curve using the pure magnetite and maghemite powders commercially available. The correlation coefficients, R(2), for magnetite-maghemite mixture was 0.9941. According to the method, the iron oxide nanoparticles prepared by the wire explosion in this study was calculated to contain 55.8 wt.% maghemite and 44.2 wt.% magnetite. We believe that the proposed method would be a convenient tool for the study of the magnetite-maghemite mixture which otherwise requires highly sophisticated equipments and techniques.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Electricity
  • Explosions
  • Ferric Compounds / analysis*
  • Ferric Compounds / chemistry
  • Ferrosoferric Oxide / analysis*
  • Ferrosoferric Oxide / chemistry
  • Iron / chemistry*
  • Nanoparticles / analysis*
  • Nanoparticles / chemistry
  • Particle Size
  • Powders
  • X-Ray Diffraction

Substances

  • Ferric Compounds
  • Powders
  • ferric oxide
  • Iron
  • Ferrosoferric Oxide