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Using X-ray photoelectron spectroscopy, the oxidation/alteration of massive coexisting pentlandite [(Fe,Ni) 9 S] and pyrrhotite (Fe 1-x S) from Voiseys Bay has been studied in aqueous solution at pH 9.3. The Fe 2p, Ni 2p, S 2p, and O1s spectra were obtained for each mineral from polished surfaces, and from surfaces reacted with the solutions for up to 180 minutes. Both minerals oxidize rapidly to give mostly a relatively thin layer (tens of angstroms) of Fe(III) oxyhydroxide (probably FeOOH). In addition, violarite (FeNi 2 S 4 ), Ni(OH) 2 , and NiSO 4  are found in the pentlandite oxidized overlayer, and Fe(III)-S and polysulfide species are found in the overlayers of both minerals. A protocol was developed to fit quantitatively all spectra in a consistent fashion. Fe 2p 3/2  spectra were fitted with two Fe(II)-S peaks depending upon Fe coordination (four and six) in pentlandite, pyrrhotite, and violarite. An Fe(III)-S multiplet, an Fe(III) oxyhydroxide multiplet, as well as Ni Auger peaks, were also required to fit the Fe 2p spectra. The Ni 2p 3/2  spectra for pentlandite were fit with two Ni(II)-S peaks from the original pentlandite or violarite (four and six coordination), as well as Ni(OH) 2  and NiSO 4  peaks. The S 2p spectra for both minerals were fit with four and five coordinate S peaks from the original minerals and violarite, as well as polysulfides and sulfate. Finally, the O 1s spectra of both minerals were fit with peaks from oxide, hydroxide, and adsorbed water.

Oxidation/alteration of pentlandite and pyrrhotite surfaces at pH 9.3: Part 1. Assignment of XPS spectra and chemical trends