Surprising coordination for plutonium in the first plutonium(III) borate

Inorganic Chemistry

Volumn 50, Issue 6, 2011, Pages 2079-2081

  Wang, Shuao ^a   Alekseev, Evgeny V ^b   Depmeier, Wulf ^b   Albrecht Schmitt, Thomas E ^a  

^a University of Notre Dame   (United States)

^b UNIVERSITY OF KIEL   (Germany)

Author keywords

[No Author keywords available]

Indexed keywords

BORIC ACID; PLUTONIUM;

ARTICLE; CHEMICAL STRUCTURE; CHEMISTRY;

BORATES; MODELS, MOLECULAR; PLUTONIUM;

EID: 79954428603     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic200064n     Document Type: Article

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22. 3 for 5 days at 200 °C (in an autoclave). The solution was ozonated for 1 h and reduced to a moist residue and redissolved in water forming a plutonium (VI) nitrate solution. UV-vis-near-IR spectroscopy indicates that only plutonium-(VI) is present. An aliquot containing 5 mg of plutonium was taken from this solution and reduced to a residue. A total of 50 μL of concentrated HBr was added to this residue, resulting in the immediate formation of bromine gas and a red solution [the red color is from the dissolved bromine, which masks the color of plutonium (III)]. The red solution was reduced to a purple-black residue at 130 °C and then transferred into an argon-filled glovebox. The residue was redissolved in 30 μ L of argonsparged water, producing a navy blue/purple solution characteristic of plutonium (III). The droplet of plutonium (III) was then transferred to a poly (tetrafluoroethylene) (PTFE) autoclave liner that had been previously heated in the glovebox for 2 days at 200 °C to drive the oxygen out of the PTFE. The catalyst for the glovebox was then regenerated. A large excess of boric acid (63 mg) was then added directly to the droplet containing plutonium (III). The mixture was then sealed in an autoclave and heated at 240 °C for 7 days, followed by slow cooling to room temperature over a 2 day period. The furnace for heating the autoclave was also inside the glovebox to prevent oxygen from reentering the autoclave because oxygen is not excluded by PTFE. The autoclave was opened, and cold water was added to dissolve the excess boric acid, revealing navy blue/purple crystals with a platelike habit.
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