ASTM C1539-08(2014)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:C1539 −08 (Reapproved 2014)
Standard Test Method for
Determination of Technetium-99 in Uranium Hexafluoride by
Liquid Scintillation Counting
This standard is issued under the fixed designation C1539; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope isotope in a given cocktail and vial combination is developed
by counting a series of standards containing the same activity
1.1 This test method is a quantitative method used to
99 of that isotope, but each with different quench. Sample quench
determine technetium-99 ( Tc) in uranium hexafluoride (UF )
is typically quantified by a variety of parameters.
by liquid scintillation counting.
1.2 The values stated in SI units are to be regarded as 4. Summary of Test Method
standard. No other units of measurement are included in this
4.1 Ameasuredportionofhydrolyzeduraniumhexafluoride
standard.
(UF ) containing approximately 0.8 to 1.2 g of uranium or a
1.3 This standard does not purport to address all of the
volume of sample less than or equal to 30 mLis transferred to
safety concerns, if any, associated with its use. It is the
a centrifuge tube. The uranium is precipitated using ammo-
responsibility of the user of this standard to establish appro-
niumhydroxide.Aftercentrifuging,thedecantedsupernatantis
priate safety and health practices and determine the applica-
acidified with sulfuric acid and extracted with tributyl phos-
bility of regulatory limitations prior to use.
phate.An aliquot of the extract is transferred to a scintillation
vial, where stannous chloride in hydrochloric acid and liquid
2. Referenced Documents
scintillation cocktail are added. The Tc beta activity is then
determined by liquid scintillation counting.
2.1 ASTM Standards:
C787Specification for Uranium Hexafluoride for Enrich-
5. Significance and Use
ment
C996Specification for Uranium Hexafluoride Enriched to
5.1 Uraniumhexafluorideisabasicmaterialusedtoprepare
Less Than 5 % U nuclear reactor fuel. To be suitable for this purpose, the
C1215Guide for Preparing and Interpreting Precision and material must meet the criteria for technetium composition.
Bias Statements in Test Method Standards Used in the Thistestmethodisdesignedtodeterminewhetherthematerial
Nuclear Industry meets the requirements described in Specifications C787 and
C996.
2.2 Other Document:
USEC-651 Uranium Hexafluoride: A Manual of Good
5.2 Usingthespecifiedinstrumentationandparameters,this
Handling Practices
method has a lower detection limit of 0.0004 µgTc/gU.
NOTE 1—Different instrumentation or parameters may provide varying
3. Terminology
detection limits, as calculated in 11.4.
3.1 Definitions:
6. Apparatus
3.1.1 quench standard curve—a relationship between
6.1 Liquid Scintillation Counter, with alpha/beta discrimi-
sample quench and detection efficiency.Aquench curve for an
nation and enhanced low level discrimination over the entire
energy range of 0 to 2000 keV.
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
6.2 Centrifuge.
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
6.3 Analytical Balance, 1 mg sensitivity.
Current edition approved June 1, 2014. Published June 2014. Originally
6.4 Separatory Funnel, 125 mL volume.
approved in 2002. Last previous edition approved in 2008 as C1539–08. DOI:
10.1520/C1539-08R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime
Standards volume information, refer to the standard’s Document Summary page on is Packard Tri-Carb Model 1905AB/LA. If you are aware of alternative suppliers,
the ASTM website. please provide this information to ASTM International Headquarters. Your com-
Available from U.S. Enrichment Corporation, 6903 Rockledge Drive, ments will receive careful consideration at a meeting of the responsible technical
Bethesda, MD 20817. committee, which you may attend.
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C1539−08 (2014)
6.5 Liquid Scintillation Vials, 20 mL. 9. Procedure
6.6 Centrifuge Tubes with Caps, 50 mL.
9.1 Transfer an aliquot up to 30 mLof one of the following
solutions, as applicable, to a 50 mL centrifuge tube:
6.7 Laboratory Wipes, lint free disposable.
9.1.1 Hydrolyzed UF Sample—Unknown UF sample hy-
6 6
7. Reagents and Materials
drolyzed in water.
7.1 Purity of Reagents—Reagent grade chemicals shall be
9.1.2 Standard—Laboratory control sample with a known
used in all tests. Unless otherwise indicated, it is intended that Tc concentration.
all reagents conform to the specifications of the Committee of
9.1.3 Spike Solution—UF sample spiked with a known
Analytical Reagents of theAmerican Chemical Society where
concentration of Tc (approximately ten times the sample
specifications are available.
activity).
7.2 Purity of Water—Unless otherwise indicated, references
9.2 Add 2 drops of potassium permanganate solution (1%
to water shall be understood to mean laboratory accepted
W/V) and swirl to mix.
deionized water.
9.3 Dilute with water to approximately 35 mL and swirl to
7.3 Ammonium Hydroxide(NH OH),concentrated(14.5M).
mix.
7.4 Hydrochloric Acid (HCl), concentrated (12M).
9.4 Add 5 mL concentrated ammonium hydroxide to pre-
7.5 Hydrochloric Acid (HCl), (1M).Add 82 mL of concen- cipitate uranium.
trated (12 M) HCl to 900 mLof water, dilute to a final volume
9.5 Dilute with deionized water to 50 mL.
of 1000 mL, and mix.
9.6 Cap and shake vigorously to break up large particles of
7.6 Liquid Scintillation Cocktail.
ammonium diuranate.
7.7 Potassium Permanganate (KMnO ), 1%W/Vin water.
9.7 Centrifuge for approximately 10 min at approximately
Dissolve1gof KMnO in 100 mL of water, and mix.
1500 rpm.
7.8 Stannous Chloride (SnCl ), 20% (W/V) SnCl in con-
2 2
9.8 Add 25 mL 9M H SO to a clean 125-mL separatory
2 4
centratedhydrochloricacid.Dissolve20gofSnCl in100mL
funnel.
of concentrated hydrochloric acid, and mix.
9.9 Decant the supernatant containing the technetium into
7.9 Sulfuric Acid (H SO ), concentrated 18M.
2 4
the 125-mL separatory funnel.
7.10 Sulfuric Acid (H SO ), 9M.Add 500 mL concentrated
2 4
NOTE 2—The precipitated uranium remains in the centrifuge tube.
H SO (18 M) to 400 mL water, dilute to a final volume of
2 4
9.10 Add 5 mL of TBP solution to the separatory funnel.
1000 mL, and mix.
9.11 Stopper or cap the funnel and shake for approximately
7.11 Sulfuric Acid (H SO ), 3M. Add 168 mL of concen-
2 4
60 s.
trated H SO (18M) to 800 mL of water, dilute to a final
2 4
volume of 1000 mL, and mix.
9.12 Allow phases to separate a minimum of 5 min.
7.12 SulfuricAcid(H SO ),1M.Add56mLofconcentrated
2 4
9.13 Drain off aqueous (lower) phase into a waste beaker.
H SO (18M) to 900 mL of water, dilute to a final volume of
2 4
9.14 Add 20 mL of 3M H SO .
2 4
1000 mL, and mix.
9.15 Stopper or cap the funnel and shake for approximately
7.13 Technetium Standard(s) in a Basic Aqueous Solution.
30 to 45 s.
7.14 Tributyl Phosphate (TBP C H O P), saturated solu-
12 27 4
tion. Equilibrate 500 mLTBPwith 500 mL3M H SO . Shake 9.16 Allow phases to separate for a minimum of 5 min.
2 4
for approximately 2 min. Allow to separate and discard
9.17 Drain off aqueous (lower) phase into a waste beaker.
aqueous layer.
9.18 Pipette up to 4 mL of the extract from the funnel into
8. Hazards
a 20 mL scintillation vial.
8.1 Since UF is radioactive, toxic, and highly reactive,
9.19 Pipette0.2mLstannouschloridesolutionintothevial.
especially when reducing substances and moisture are present
9.20 Pipette 12 mLliquid scintillation cocktail into the vial.
(see USEC-651), appropriate facilities and practices must be
NOTE 3—This test method has proven acceptable for 12 mL of liquid
provided.
scintillation cocktail, but up to 16 mL can be added depending on the
user’s instrumentation.
Reagent Chemicals, American Chemical Society Specifications, American
9.21 Cap the vial and shake vigorously for approximately 5
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
to 10 s.
Chemicals,BDHLtd.,Poole,Dorset,U.K.andthe United States Pharmacopeia and
9.22 Wipe the outside of the vial with a damp laboratory
National Formulary,U.S.PharmacopeialConvention,Inc.(USPC),Rockville,MD,
or equivalent.
wipe to remove static electricity, if necessary.
Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime
i
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