DOE Test Method CHEM-TP-FE.1


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Analytical testing dots

Source:
DOE

Method Name:
Fe-55 in Water by Liquid Scintillation Counting. Official Name: Fe-55 in Water

Description:
Iron (Fe) is first precipitated as the hydroxide is dissolved in 10 M HCl. The solution is passed through an anion exchange column that has been equilibrated with 12 M HCl. The Fe-55 is selectively eluted with 0.1 M HCl after eluting and discarding interfering nuclides with 6 M and 4 M HCl. Concentrated H3PO4 is added to the eluant containing the Fe and the solution boiled down to a colorless solution of H3PO4. Water and scintillator are added and the mixture is shaken prior to counting.

Scope:
This procedure is applicable to the liquid-scintillation measurement of Fe-55 after its chemical separation from environmental waters and various liquids collected at nuclear reactor facilities.

Citation:
Dept. of Energy RESL Technical Procedure

Interferences:
(A) Higher Fe-59 energies: Many samples contain Fe-59, thus a correction for the overlap of much higher energy Fe-59 beta spectrum into the low energy Fe-55 spectral region is necessary.(B) Sample volumes: The volume of sample used depends on activity level as well as on the amount of stable iron present. Low activity samples can be concentrated by evaporation, and high activity samples can be analyzed by taking small aliquots. The iron in eluent taken plus the 10 mg of iron carrier added should not exceed 20 mg.

QC Requirements:
A reagent blank must be included with each set of samples analyzed. A Fe-55 std must also be prepared and counted to determine of the counting efficiency of each set of samples. An occasional Fe-59 control sample should be carried through the procedure to check chemical yield and spectral overlap. Correct performance of the liquid scintillation counter must be verified by an Instrument Performance Analysis (IPA) at the end of counting each sample set.

Maximum Holding Time:
None given.

Media:
WATER

Subcategory:
Radiochemical

Concentration:
None given.

Precision:
-

Detection:
Results in an average counting efficiency of 40 plus/minus 1% for Fe-55.

Revision Number:
Apr-99

Analytical testing dots

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Analytical testing dots