Portland State University. Department of Chemistry
Date of Award
Master of Science (M.S.) in Chemistry
1 online resource (53 pages)
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·P203F4, 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.
Emme, Larry McCain, "Synthesis of Uranium Fluorosulfates and the Group VI B Difluorophosphates" (1973). Dissertations and Theses. Paper 1593.