PREPARATION OF METALLIC PROMETHIUM

Journal Article · Sat Jun 01 04:00:00 EDT 1963 · Angew. Chem., Intern. Ed. Engl.

DOI:https://doi.org/10.1002/anie.196303261· OSTI ID:4160083

Weigel, F

A method is described for purification of Pm by reduction of PmF/sub 3/ in vacuo. Processed Pm from the Isotopes Division of Oak Ridge National Laboratory, used as starting material, contained approximates 50 C (60 mg) of Pm/ sup 147/together with about 50 mg Sm, 40 mg Nd, and about 7 mg Am /sup 241/. The lanthanides were separted on Dowex 50 x 12 by elution with 0.5M ammonium alpha - hydroxyisobutyrate at pH 3.5 and 87 deg C. The Am was separated by absorption on Dowex 1 x 10 and elution of the Pm with SM ammonium thiocyanate. After this separation, the purplish pink solution of Pma in HNO/sub 3/ still contained about 17 C of Pm/sup 147/, and aliquot portions, each of 100 mu l, were removed from it. The purplish pink PmF/sub 3/ was precipitated with HF, washed several times with distilled water, centrifuged, and the supernatant solution pipetted off. After drying for two days over P/sub 2/O/sub 5/, the PmF/sub 3/ had shrunk to a compact pellet. The pellet was transferred to the inner basket of a tantalum crucible system, and approximates 10 times its wt of pure Li was placed in the outer crucible; the whole unit was then closed with a tantalum stopper and suspended in the container vessel of a vacuum manifold. At 2.7 x 10/sup -6/ mm Hg pressure the system was heated by means of an induction heater. At 750 deg C, excess Li effused from the crucible system. The crucible was then maintained for periods of 2 min each at 800 deg , 980 deg , and 1090 deg C, and then cooled to room temperature over 1 hr and examined under the microscope. Promethium metal had separated as a solid bead which had fused onto the tantalum wires of the inner container and which had the appearance of a Nd bead obtained under similar conditions. lts mp was 1080 plus or minus 10 deg C. Because of its high radioactivity (940 mC/mg), a glovebox was used for high vacuum operations involving Pm. (BBB)

• Research Organization: Universitat, Munich
• NSA Number: NSA-18-001627
• OSTI ID: 4160083
• Journal Information: Angew. Chem., Intern. Ed. Engl., Journal Name: Angew. Chem., Intern. Ed. Engl. Vol. Vol: 2
• Country of Publication: Country unknown/Code not available
• Language: English

Related Subjects

ACIDITY
AMERICIUM 241
AMMONIUM COMPOUNDS
BUTYRIC ACID
CHEMISTRY
COMPACTING
COPPER ALLOYS
CRUCIBLES
CRYSTALS
CYANIDES
DIFFRACTION
DISTILLATION
DTA
EVAPORATION
EXPANSION
GLOVEBOXES
GOLD
GOLD ALLOYS
HARDNESS
HIGH TEMPERATURE
HYDROFLUORIC ACID
IMPURITIES
ION EXCHANGE MATERIALS
LEACHING
LITHIUM
MICROSCOPY
NEODYMIUM
NITRIC ACID
ORGANIC ACIDS
ORGANIC SULFUR COMPOUNDS
PHASE DIAGRAMS
PHOSPHORUS OXIDES
PRECIPITATION
PREPARATION
PRESSURE
PROMETHIUM
PROMETHIUM 147
PROMETHIUM FLUORIDES
RADIATION PROTECTION
REDUCTION
REFINING
REMOTE HANDLING
SAMARIUM
SEPARATION PROCESSES
SILVER ALLOYS
SOLUTIONS
TANTALUM
TEMPERATURE
THOR