DOE Test Method CHEM-TP-A.20


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PDF IconView Actual DOE Method CHEM-TP-A.20 (PDF File)


Source:
DOE

Method Name:
Actinide Separations for Alpha Spectrometry Using Neodymium Fluoride Coprecipitation. Official Name: Actinide Separations for Alpha Spectrometry using Neodymium Fluoride Coprecipitation

Description:
Note: This procedure supersedes RESL ACB-TP-A.20 (Rev 1).Air filters, 10-g soil, 500-mL water, and 5-g vegetation-ash samples are fused in potassium fluoride followed by a pyrosulfate fusion. The flux is dissolved in dilute hydrochloric acid and thorium, uranium, plutonium, and americium are coprecipitated on barium sulfate. These actinides can be directly coprecipitated from water samples on Barium sulfate, if total decomposition is not necessary. The barium sulfate is dissolved and reprecipitated in the presence of diethylenetriamine-pentaacetic acid (DPTA) to separate the actinides from barium sulfate. The filtrate is wet ashed, fused in a pyrosulfate flux, and fusion cake dissolved in dilute nitric acid. Thorium is separated from the other actinides by coprecipitation on ceric iodate. Uranium, plutonium, and americium are separated sequentially, one from the other, by oxidizing them to their highest oxidation states followed by a series of coprecipitations of the nuclides. The isolated nuclides are coprecipitated on neodymium fluoride, filtered and determined by alpha spectrometry.

Scope:
The prcoedure prepares air filters, soil, water, and vegetation samples for determination of thorium (Th), uranium (U), plutonium (Pu), and americium (Am).

Citation:
Dept. of Energy RESL Technical Procedure

Interferences:
(A) Neptunium presence: Procedure will not work in the presence of neptunium because neptunium is incompletely separated from the other nuclides. (B) Cross contamination: To prevent cross contamination of samples and contamination of personnel, equipment, laboratory work area, and alpha spectrometry systems apply procedure to only low-level samples (see applicable conc. range).

QC Requirements:
QC procedures based on internal laboratory requirements for radiochemical analysis.

Maximum Holding Time:
None given.

Media:
WATER

Subcategory:
Radiochemical

Concentration:
Low-level samples: 5-20 dpm of alpha tracer and a comparable or lesser activity of analyte nuclide(s)

Precision:
The accuracy range in the method is 85-95% recovery. The resolution for full width at half maximum (fwhm) is between 40 and 70 kilo-electron volts (keV).

Detection:
Decontamination factors range between 103 and 104.

Revision Number:
May-99

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Analytical testing dots