ASTM C1508-01

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:C1508–01
Standard Test Method for
Determination of Bromine and Chlorine in UF and Uranyl
Nitrate by X-Ray Fluorescence (XRF) Spectroscopy
This standard is issued under the fixed designation C 1508; 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 halides. The halides are collected on filter paper and are
analyzed by X-ray fluorescence using two different crystal/
1.1 This method covers the determination of bromine (Br)
detector systems.
and chlorine (Cl) in uranium hexafluoride (UF ) and uranyl
nitrate solution. The method as written covers the determina-
4. Significance and Use
tion of bromine in UF over the concentration range of 0.2 to
4.1 The method is designed to show whether or not the
8 µg/g, uranium basis. The chlorine in UF can be determined
tested materials meet the specifications as given in C 787 and
over the range of 4 to 160 µg/g, uranium basis. Higher
C 788.
concentrations may be covered by appropriate dilutions. The
detection limit for Br is 0.2 µg/g uranium basis and for Cl is 4
5. Interferences
µg/g uranium basis.
5.1 Plastic equipment must be used throughout the method
1.2 This standard may involve hazardous materials, opera-
for uranyl fluoride as the hydrofluoric acid in the uranyl
tions and equipment. This standard does not purport to address
fluoride leaches chloride from glassware causing a high bias.
all of the safety concerns, if any, associated with its use. It is
5.2 Low recoveries may occur as the precipitate can be
the responsibility of the user of this standard to establish
difficult to transfer quantitatively to the filter paper. A surfac-
appropriate safety and health practices and determine the
tant can be added (optional step) to minimize the adhesion of
applicability of regulatory limitations prior to use.
the precipitate to the walls of the beakers and the funnel.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
6.1 X-Ray Spectrometer, see Guide C 1118 for the selection
C 761 Test Methods for Chemical, Mass Spectrometric,
of the X-ray Spectrometer.
Spectrochemical, Nuclear and Radiochemical Analysis of
2 6.2 Plastic Vacuum Filtration Apparatus, for 47 mm diam-
Uranium Hexafluoride
eter filter paper.
C 787 Specification for Uranium Hexafluoride for Enrich-
6.3 Filter Paper, 0.45 micron, 47 mm diameter.
ment
2 6.4 Beakers, polypropylene, 250 mL.
C 788 Specification for Uranyl Nitrate
6.5 Stirring Rods, plastic or Teflon.
C 1118 Guide for Selecting Components for Wavelength
2 6.6 X-ray Sample Support, Rings. Inner diameter approxi-
Dispersive X-Ray Fluorescence (XRF) Systems
mately 40 mm.
D 1193 Specification for Reagent Water
7. Reagents
3. Summary of Test Method
7.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 Asample of hydrolyzed UF (uranyl fluoride) or uranyl
used in all tests. Unless otherwise indicated, it is intended that
nitratesolutionistreatedwithsodiumnitritetoreduceoxidized
all reagents conform to the specifications of the Committee on
formsofbromineandchlorine(bromatesandchlorates)totheir
Analytical Reagents of theAmerican Chemical Society, where
respectivehalideions.Additionofsilvernitrateprecipitatesthe
such specifications are available. Other grades may be used,
silver halides. Spike recoveries can be improved by the
provided it is first ascertained that the reagent is of sufficiently
addition of potassium iodide causing coprecipitation of the
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 Methods of The filter must be Cl and Br free. Millipore membrane filter type HABP
Test. (www.millipore.com) has been successfully used. An alternate is 15A from S.C.B,
Current edition approved August 10, 2001. Published September 2001. BP6, RN86, 07130 Soyons France. Any other equivalent is acceptable.
2 5
Annual Book of ASTM Standards, Vol 12.01. Reagent Chemicals, American Society Specifications, American Chemical
Annual Book of ASTM Standards, Vol 11.01. Society, Washington, DC.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1508–01
NOTE 1—Recommend cleaning all laboratory equipment with ammo-
7.2 Purity of Water—Unless otherwise indicated, references
nium hydroxide solution (7.4) prior to use.
to water shall be understood to mean reagent water conforming
to Specification D 1193, Type I.
9.2 Follow laboratory QA practices and run the necessary
7.3 Ammonium Hydroxide,NH OH, concentrated, specific
duplicates, spikes and controls with the samples. Use the
gravity 0.90.
solution prepared in 7.17 for the spikes.
7.4 Ammonium Hydroxide Solution, 1 + 3 (3.7 M). Dilute 1
NOTE 2—2 mL and 4 mL spike aliquots were found to be reasonable
part NH OH with 3 parts water.
volumes.
7.5 Surfactant, bromine and chlorine free. (Optional).
9.3 Add0.5mLofpotassiumiodidesolutiontoeachsample
7.6 Surfactant Solution, 1 + 999.Add 1 mL of surfactant to
and standard. (Optional step).
approximately 1 litre of water. (Optional).
9.4 Add 4 mL of surfactant solution 7.6. (Optional step).
7.7 Nitric Acid, HNO , concentrated, specific gravity 1.42.
9.5 Add 10 mL of sodium nitrite solution to each sample
7.8 Nitric Acid Solution, 1 + 999 (0.016 M). Add 1 mL of
andstandard.Stireachsolutionwithadedicatedplasticstirring
concentrated HNO to approximately 200 mL of water. Add 1
rod and allow to stand for a minimum of 2 minutes.
mL of the surfactant (7.6). (Optional). Dilute to 1 litre.
9.6 Slowly and with stirring add 25 mL of the silver nitrate
7.9 Sodium Nitrite, NaNO .
solution. Remove the plastic stirring rods. Heat the solution in
7.10 Sodium Nitrite Solution, 2 g/L. Dissolve1gof sodium
a water bath at approximately 80°C 6 10°C for 1 ⁄2 hours.
nitrite in water and dilute to 500 mL. Prepare fresh immedi-
9.7 Remove from the bath. Allow the halides to precipitate
ately before use.
overnight. A 2 hour precipitation time has been found to be
7.11 Silver Nitrate, AgNO .
successful, but the user must establish precision and bias based
7.12 Silver Nitrate Solution, 2 g/L. Dissolve2gof silver
on the shorter time.The precision and bias data in this standard
nitrateinwateranddiluteto1litre.Keepawayfromlightinan
were generated using an overnight precipitation.
opaque bottle. The solution should be made fresh weekly.
9.8 Filter using 0.45 micron filter paper. Use a plastic
Silver is an RCRA listed hazardous waste. Make up only as
vacuum filtration assembly. Use a plastic rod with a rubber
much of this solution as required to minimize e
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