Hydrothermal synthesis of a novel uranium oxalate/glycolate via in-situ ligand formation

Inorganic Chemistry

Volumn 46, Issue 16, 2007, Pages 6607-6612

  Knope, Karah E ^a   Cahill, Christopher L ^a,b  

^a GEORGE WASHINGTON UNIVERSITY   (United States)

^b GEOPHYSICAL LABORATORY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 34548025608     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic700700e     Document Type: Article

References (80)

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79. Synthesis of 1 using glycolic acid. Uranium oxynitrate hexahydrate (0.141 g, 0.28 mmol), tetraethylammonium hydroxide, 20 wt % solution in water (0.164 g, 0.22 mmol), glycolic acid (0.043g, 0.57 mmol), and distilled water (5 g, 278 mmol) were placed into a 23 mL Teflon-lined Parr bomb in the molar ratio of 1.0:0.8:2.0:992, pH 2.0. The reaction vessel was sealed and heated statically at 120 °C for 7 days. Upon cooling to room temperature, a clear yellow solution (pH 2.0) was decanted and yellow-orange plates were obtained. The crystals were washed with distilled water followed by ethanol and then allowed to air dry at room temperature. Yield: 52% (based on uranium). Product was characterized by single-crystal x-ray diffraction, and phase purity was confirmed by powder x-ray diffraction.
80. Synthesis of 1 from ethylene glycol. Uranium oxynitrate hexahydrate (0.141 g, 0.28 mmol), tetraethylammonium hydroxide, 20 wt % solution in water (0.164 g, 0.22 mmol), ethylene glycol (330 uL, 2.5 mmol), and distilled water (5 g, 278 mmol) were placed into a 23 mL Teflon-lined Parr bomb in the molar ratio of 1.0:0.8:9.0: 992, pH 3.15. The reaction vessel was sealed and heated statically at 120 °C for 14 days. Upon cooling to room temperature, a clear yellow solution (pH 2.4) was decanted and yellow-orange plates were obtained. The crystals were washed with distilled water followed by ethanol and then allowed to air dry at room temperature. Yield: 81% (based on uranium). Product was characterized by single-crystal x-ray diffraction, and phase purity was confirmed by powder x-ray diffraction.