Synthesis of Uranium Fluorosulfates and the Group VI B Difluorophosphates

Author

Larry McCain Emme, Portland State University

Sponsor

Portland State University. Department of Chemistry

Date of Publication

1973

Document Type

Thesis

Degree Name

Master of Science (M.S.) in Chemistry

Department

Chemistry

Language

English

Subjects

Uranium fluorosulfates

DOI

10.15760/etd.1593

Physical Description

1 online resource (53 pages)

Abstract

Some reactions leading to several anhydrous Uranium fluorosulfates through the use of fluorosulfonic acid or peroxydisulfuryl di-fluoride have been studied. It was found that HS0F can oxidize uranium 3metal to the +4 state or the +2 state depending on the reaction conditions. The synthesis of the tan solid; U(S0₃F)₄ and the pale green solid thought to be U(S0₃F)₂ were prepared in this manner. It was found that S₂0₆F₂ can also oxidize uranium to yield the green solid U(S0₃F)₃. S₂0₆F₂ was also found to be a convenient reagent for placing a fluorosulfonate group on uranium tetrahalides to form addition or displacement products; the yellow solid UF₄(S0₃F)₂ and the tan solid U(S0₃F)₄ were prepared in this manner. Other reactions involving the fluorosulfate, U(S0₃F)₄ as a reactant are also discussed. Analytical data and infrared spectra are reported for the compounds and x-ray powder data and magnetic susceptibility data are presented for U(S0₃F)₂ and U(S0₃F)₄. The reaction of the fluorinated anhydride µ -oxo-bis (phosphoryl difluoride), P₂0₃F₄ with some group VI B metal oxide salts has found to form the corresponding difluorophosphates. Five new compounds were prepared; KCr0₂(P0₂F₂)₃·P₂0₃F_4, Cs₂Cr0₂(P0₂F₂)_4, Na₂MO0₂ (P0₂F₂)_4, Na₂W0₂(P0₂F₂)₄. Physical constants, analytical data and infrared spectra are presented supporting the proposed structures for these compounds. A method for the preparation of K₂Cr0₂(CF₃S0₃)₄ from K₂Cr0₄ and (CF₃S0₂)₂0 is also presented. Analytical data, infrared spectra and the x-ray powder spectra for this compound are given.

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Persistent Identifier

http://archives.pdx.edu/ds/psu/10879

Recommended Citation

Emme, Larry McCain, "Synthesis of Uranium Fluorosulfates and the Group VI B Difluorophosphates" (1973). Dissertations and Theses. Paper 1593.
https://doi.org/10.15760/etd.1593