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Journal of Structural Chemistry

2011 year, number 1

A STUDY OF THE HYDROLYSIS OF AND THE STRUCTURE OF INTERMEDIATE HYDROLYSIS PRODUCTS BY 19F AND 91Zr NMR IN THE 9.4 T FIELD

M. A. Fedotov1, A. V. Belyaev2
1
2
Keywords: Zr(IV), fluorides, fluoride complexes, hydrolysis, polycondensation, 19F and 91Zr NMR
Pages: 74-79

Abstract

The high-field 19F and 91Zr NMR method is used to study the hydrolysis and polycondensation of hexafluorozirconate in aqueous and water-peroxide solutions. During hydrolysis in aqueous solutions only and F- ions were observed by NMR, however, in the water-peroxide medium, an intermediate product of hydrolysis ( [F5Zr-OO-ZrF5]4- dimer) was detected. The dimer structure is confirmed by 19F and 91Zr NMR. In high fields (19F NMR frequency > 200 MHz), the fluorine exchange between and F- is slow in the 19F NMR scale and has a multisite character.