Water determination of precursor solutions with oxidant cations by the Karl Fischer method: the YBCO-TFA case

A. CALLEJA; S. RICART; X. PALMER; R. F. LUCCAS; T. PUIG; X. OBRADORS

JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY

SPRINGER

Año: 2010 vol. 53 p. 347 - 352

0928-0707

Uncontrolled water content in non-aqueous precursor solutions can be a source of irreproducibility in thin film performance through changes in the gel network. Towards gaining control on the solution properties, water determination in metalorganic solutions of YBCO-TFA has been studied by the Karl Fischer titration in a volumetric-type unit. However, oxidizing cations usually present when preparing functional oxides by chemical solution routes severely interfere in the Karl Fischer analysis. In the case of YBCO-TFA, cupric ions in the initial solution oxidize the iodide produced in the Karl Fischer reaction back to iodine, which in turn feeds the titration reaction and consumes more water, causing a negative error in the analysis, which can be as large as 70%. However, such chemical interference of cupric salts can be modelled and quantified. A corrected Karl Fischer methodology is proposed for accurately measuring water content in YBCO-TFA solutions, which could be potentially extended to other precursor solutions containing oxidant cations.