A recently discovered high temperature (22G-2800C) reaction between glycerol and the oxides and hydrous oxides of iron produces a green, well-crystalline complex glycerato-iron, whereas hydrous nickel oxides an) reduced by the glycerol to metallic nickel. When nickel isomorphously substitutes for iron within the goethite lattice this high temperature glyceration allows a separation of the two metals whereby the nickel can be extracted by solution techniques.