HEXAFLUORIDES OF MOLYBDENUM, TUNGSTEN AND URANIUM. II. REACTIONS WITH LIQUID AND GASEOUS DINITROGEN TETROXIDE Page: 4 of 11
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2
INTRODUCTION
The reactions of molybdenum, tungsten and uranium hexafluorides with liquid and gaseous
dinitrogen tetroxide were studied to determine whether nitrylium salts analogous to the
nitrosylium salts described previously5 would be formed. .Other workers have prepared
nitryl complex fluorides of vanadium, niobium, tantalum,6 gold,. phosphorus, germanium,
and tin by the action of the metal fluoride or oxide either directly with nitryl fluoride or
with dinitrogen tetroxide in bromine trifluoride. Also,. Robinson and. Westland8 made
nitrylium hexafluoroiridate (IV) by reacting gaseous dinitrogen tetroxide with iridium
hexafluoride. These same workers obtained a heterogeneous product by the reaction of
iridium hexafluoride with liquid dinitrogen tetroxide.
EXPERIMENTAL
EQUIPMENT, MATERIALS AND PROCEDURE - A metal vacuum system was used for
storage and manipulation of reactants. Flanged nickel vessels with Teflon gaskets were
employed for reactors. All equipment was exposed to fluorine before use to minimize
reaction with the hexafluorides. The reactors were heated in a thermostatically con-
trolled oven. Purification of the hexafluorides has been described previously.5 Dinitrogen
tetroxide obtained from the Matheson Company was purified by low temperature distillation.
For reactions with liquid dinitrogen tetroxide, the desired amounts of reactarts were
added to a tared evacuated reactor by cold trapping,. using a liquid nitrogen bath. The
reactor was then brought to temperature in the oven.. After reaction, the gases and liquids
remaining in the reactor were analyzed and then removed by evacuation.. Solid products
were removed,, sampled and stored in a dry box.. Reactions with gaseous dinitrogen
tetroxide were performed and ,studied in an infrared gas cell by a technique already
described.5
5. Geichman,, J. R., et al.: Hexafluorides of Molybdenum, Tungsten and Uranium.
I.. Reactions with Nitrous and Nitric Oxides. Goodyear Atomic Corp.,, Jan. 10, 1962.
12p. (GAT-T-969) Submitted toInorg. Chem.
6. Clark,. H. C. andEmeleus, H.. J. J. Chem. Soc., 190 (1958)
7. Woolf, A. A. and Emeleus,. H. J. J. Chem.. Soc., 1050 (1950)
8. Robinson, P. L. and Westland, G. J. J. Chem. Soc., 4481 (1956)
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Geichman, J. R.; Smith, E. A.; Swaney, L. R. & Ogle, P. R. HEXAFLUORIDES OF MOLYBDENUM, TUNGSTEN AND URANIUM. II. REACTIONS WITH LIQUID AND GASEOUS DINITROGEN TETROXIDE, report, January 29, 1962; United States. (https://digital.library.unt.edu/ark:/67531/metadc1061497/m1/4/: accessed April 24, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.