DOE Test Method 3H-04-RC

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View Actual DOE Method 3H-04-RC (PDF File)


Source:
DOE

Method Name:
Tritium in Water - Liquid Scintillation Counting. Official Name: Tritium in Water - Liquid Scintillation Counting

Description:
The 3H spectral range or window setting is first defined. The counting efficiencies are then determined by using efficiency curves (quench curves). The efficiency curve is a plot of the counting efficiency as a function of the quench index parameter (QIP). The QIP is also known as the automatic external standardization (AES) number or the transformed spectral index of the external standard (tSIE). A sample aliquot is prepared with a measured volume of a scintillation cocktail that is then placed in a programmed LS counter for spectrum analysis.

Scope:
The procedure is used for the rapid determination of tritium by liquid scintillation (LS) spectrometry. It applies to all clear liquid samples and it can be completed in a short period (1 to 2 h) once efficiency curves have been established. The procedure is designed for a Tri-Carb 2250CA LS counter using Insta-Gel XF cocktail and it requires distillation of the samples so that they are free of salts and other interfering radionuclides.

Citation:
DOE EML Procedures Manual HASL-300, Volume 1, 28th Ed.(1997)

Interferences:
(A) 3H Distillation: Perform a 3H distillation if information more accurate than gross tritium is needed.(B) High Count Rates: Reanalyze samples with excessively high count rates (e.g., > 1,000,000 counts min-1) using less sample material. (Note: When using this procedure, the calculated 3H concentration may be higher than the actual concentration because of possible interferences from other low-energy beta emitters and the beta continuum of high energy beta particles.)(C) Efficiency Drops - Add several drops of 30% H2O2 to the vial to bleach the sample if quenching causes the efficiency to drop to one fourth of the highest efficiency. (Note: Deep color in the samples may cause severe quenching that will lower the counting efficiency.)(D) Cross contamination: High-level and low-level samples should be processed in independent batches to minimize possibility of cross contamination.

QC Requirements:
QC samples should be analyzed to ensure required limits of precision and accuracy are being met. QC samples include instrument calibration standards, blank samples, control samples, an "spiked" samples.

Maximum Holding Time:
None given.

Media:
WATER

Subcategory:
Radiochemical

Concentration:
None given.

Precision:
-

Detection:
-

Revision Number:
EML Procedures Manual HASL-300, Volume 1, 28th Ed.(1997)



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