Structure and reactivity of oxalate surface complexes on lepidocrocite derived from infrared spectroscopy, DFT-calculations, adsorption, dissolution and photochemical experiments

Author(s)
Susan Borowski, Jagannath Biswakarma, Kyounglim Kang, Walter Schenkeveld, Janet Hering, James Kubicki, Stephan Krämer, Stephan Hug
Abstract

Oxalate, together with other ligands, plays an important role in the dissolution of iron(hdyr)oxides and the bio-availability of iron. The formation and properties of oxalate surface complexes on lepidocrocite were studied with a combination of infrared spectroscopy (IR), density functional theory (DFT) calculations, dissolution, and photochemical experiments. IR spectra measured as a function of time, concentration, and pH (50–200 µM oxalate, pH 3–7) showed that several surface complexes are formed at different rates and in different proportions. Measured spectra could be separated into three contributions described by Gaussian line shapes, with frequencies that agreed well with the theoretical frequencies of three different surface complexes: an outer-sphere complex (OS), an inner-sphere monodentate mononuclear complex (MM), and a bidentate mononuclear complex (BM) involving one O atom from each carboxylate group. At pH 6, OS was formed at the highest rate. The contribution of BM increased with decreasing pH. In dissolution experiments, lepidocrocite was dissolved at rates proportional to the surface concentration of BM, rather than to the total adsorbed concentration. Under UV-light (365 nm), BM was photolyzed at a higher rate than MM and OS. Although the comparison of measured spectra with calculated frequencies cannot exclude additional possible structures, the combined results allowed the assignment of three main structures with different reactivities consistent with experiments. The results illustrate the importance of the surface speciation of adsorbed ligands in dissolution and photochemical reactions.

Organisation(s)
External organisation(s)
Eidgenössische Anstalt für Wasserversorgung, Abwasserreinigung und Gewässerschutz, Eidgenössische Technische Hochschule Zürich, École polytechnique fédérale de Lausanne, University of Texas at El Paso
Journal
Geochimica et Cosmochimica Acta
Volume
226
Pages
244-262
No. of pages
19
ISSN
0016-7037
DOI
https://doi.org/10.1016/j.gca.2018.01.024
Publication date
04-2018
Peer reviewed
Yes
Austrian Fields of Science 2012
104014 Surface chemistry, 105906 Environmental geosciences
Keywords
ASJC Scopus subject areas
Geochemistry and Petrology
Portal url
https://ucrisportal.univie.ac.at/en/publications/d2d0ce8e-3f46-46ef-8e8c-98b9e0f52a6c