ASTM C1473-00

Standard Test Method for Radiochemical Determination of Uranium Isotopes in Urine by Alpha Spectrometry

SCOPE
1.1 This test method is applicable to the determination of uranium in urine at levels of detection dependent on sample size, count time, detector efficiency, background, and tracer yield. It is designed as a screening tool for detection of possible exposure of occupational workers.
1.2 This test method is designed for 50 mL of urine. This test method does not address the sampling protocol or sample preservation methods associated with its use.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Jun-2000
• ICS: 11.100 - Laboratory medicine
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaced By: ASTM C1473-05 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Urine by Alpha Spectrometry
• Effective Date: 01-Jun-2005

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:C1473–00
Standard Test Method for
Radiochemical Determination of Uranium Isotopes in Urine
by Alpha Spectrometry
This standard is issued under the fixed designation C 1473; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This test method is applicable to the determination of 4.1 This test method is used to detect possible exposures to
uranium in urine at levels of detection dependent on sample uranium isotopes from occupational operations.
size, count time, detector efficiency, background, and tracer
5. Interferences
yield.Itisdesignedasascreeningtoolfordetectionofpossible
5.1 Thepresenceof Uintheurinesamplewillbemasked
exposure of occupational workers.
233 234
1.2 This test method is designed for 50 mL of urine. This by the tracer addition. The alpha energies of U and U
cannot be fully resolved by alpha spectrometric measurement.
test method does not address the sampling protocol or sample
preservation methods associated with its use. Atable of uranium isotope alpha energies is given inAppendix
X1.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
6. Apparatus
responsibility of the user of this standard to establish appro-
6.1 Alpha Spectrometry System—Refer to Test Methods
priate safety and health practices and determine the applica-
C 1000 and C 1163 for guidance.
bility of regulatory limitations prior to use.
6.2 Electrodeposition Apparatus—Refer to Test Method
2. Referenced Documents
C 1000 for guidance.
6.3 Neodymium Fluoride Precipitation—Refer to Test
2.1 ASTM Standards:
C 1000 Test Method for Radiochemical Determination of Method C 1163 for guidance.
Uranium Isotopes in Soil by Alpha Spectrometry 6.4 Borosilicate Beakers or Flasks, 250 mL.
6.5 Borosilicate Beakers, 150 and 250 mL.
C 1163 Test Method for Mounting Actinides for Alpha
Spectrometry Using Neodymium Fluoride 6.6 Borosilicate Graduated Glass Cylinders, 5, 25, 100, and
1000 mL.
D 1193 Specification for Reagent Water
D 3648 Practices for Measurement of Radioactivity 6.7 Ion Exchange Columns, disposable polypropylene, with
polyethylene frit,$5-mL capacity.
3. Summary of Test Method
6.8 Ion Exchange Column Reservoir, funnel, polypropy-
3.1 A urine sample with U tracer solution added is lene, 100-mL capacity.
wet-ashed with nitric acid and hydrogen peroxide to destroy
NOTE 1—See Fig. 1 for a typical ion exchange column-reservoir setup.
organic material. The uranium-bearing solution is converted to
a hydrochloric acid medium. Uranium is absorbed on an anion
7. Reagents
exchange column from a 9 M hydrochloric acid solution and
7.1 Purity of Reagents—Reagent grade chemicals shall be
eluted with 0.1 M hydrochloric acid solution. The separated
used in all tests. Unless otherwise indicated, it is intended that
uranium is prepared for alpha spectrometric measurement
the reagents conform to the specifications of the Committee on
either by electrodeposition onto a metal disk or coprecipitation
Analytical Reagents of theAmerican Chemical Society, where
with neodymium fluoride and filtration onto a membrane filter. 6
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
the determination.
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Test
Methods.
Various column configurations are available from Bio-Rad Laboratories, Life
Current edition approved June 10, 2000. Published August 2000.
Science Group, Hercules, CA;Whatman LabSales, Hillsboro, OR; and Isolabs, Inc.,
Annual Book of ASTM Standards, Vol 12.01.
Akron, OH.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 11.02.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
C1473
9. Sampling
9.1 Collect the urine sample in accordance with the site-
specific protocol.
9.2 Preserve the urine sample in accordance with the site-
specific protocol.
10. Calibration and Standardization
10.1 If a standard U solution is not available for use as a
tracer, standardize a freshly prepared sample of U; for
guidancerefertoPracticeD 3648.A Ustandardmayalsobe
used to determine the detection efficiency of the
a-spectrometry system which, in turn, can be used to calculate
the chemical yield of each sample and the lower limit of
detection (LLD) of this test method.
FIG. 1 Typical Ion Exchange Column Arrangement
11. Procedure
11.1 Sample Preparation:
11.1.1 Measure 50 mL of preserved urine in a 100-mL
7.2 Purity of Water—Unless otherwise indicated, references
graduated cylinder.
to water shall be understood to mean reagent water as defined
11.1.2 Transfer the urine to a 250-mL beaker or flask.
by Type III of Specification D 1193.
11.1.3 Rinsethecylindertwicewith5mLof8 MHNO and
7.3 Reagent purity shall be such that the measured radioac-
add the rinsings to the beaker or flask.
tivity of blank samples is minimized.
11.1.4 Add an appropriate amount of U tracer solution to
7.4 Anion Exchange Resin—Analytical grade, AG1-x8,
the sample (ca. 0.02 Bq or as prescribed in the site-specific
100-200 mesh, chloride form.
protocol) and swirl the vessel to mix.
7.5 Electrolyte Solution—Refer to Test Method C 1000 for
11.1.5 Evaporate the contents of the vessel to near dryness
reagents.
on a medium hot plate.
7.6 Hydrochloric Acid (9 M)—Mix 750 mLof concentrated
11.1.6 Remove the vessel from the hot plate and cool for 1
HCl with water and dilute to 1 L.
min.
7.7 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
11.1.7 Add 10 mL of concentrated HNO to the vessel.
chloric acid (HCl). 3
Swirl to mix.
7.8 Hydrochloric Acid (0.1 M)—Mix 8.3 mL of concen-
11.1.8 Return the vessel to the hot plate and evaporate the
trated HCl with water and dilute to 1 L.
solution to near dryness.
7.9 Hydrogen Peroxide (30 %).
11.1.9 Remove the vessel from the hot plate and allow to
7.10 Neodymium Fluoride Precipitation—Refer to Test
cool for 1 min.
Method C 1163 for reagents.
11.1.10 Slowly add 10 to 15 mLof 30 % hydrogen peroxide
7.11 Nitric Acid (8 M)—Mix 500 mL of concentrated nitric
to the vessel to cover the residue. Swirl the vessel to mix.
acid with water and dilute to 1 L.
11.1.11 Return the vessel to the hot plate and evaporate the
7.12 Nitric Acid (sp gr 1.4)—Concentrated nitric acid
solution to near dryness.
(HNO ).
11.1.12 Repeat 11.1.9 and 11.1.10.
7.13 Uranium-232, standard solution.
11.1.13 Return the vessel to the hot plate and evaporate the
solution to obtain a white sample residue.
8. Hazards
11.1.14 Remove the vessel from the hot plate and allow to
8.1 Warning—Adequate laboratory facilities, such as fume
cool for 1 min.
hoods and controlled ventilation, along with safe techniques
11.1.15 Add 10 to 15 mL of concentrated HCl to the vessel
must be used in this p
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