ASTM C1508-01(2006)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:C1508–01(Reapproved2006)
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 C1508; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Summary of Test Method
1.1 This method covers the determination of bromine (Br) 3.1 Asample of hydrolyzed UF (uranyl fluoride) or uranyl
and chlorine (Cl) in uranium hexafluoride (UF ) and uranyl nitratesolutionistreatedwithsodiumnitritetoreduceoxidized
nitrate solution. The method as written covers the determina- formsofbromineandchlorine(bromatesandchlorates)totheir
tion of bromine in UF over the concentration range of 0.2 to respectivehalideions.Additionofsilvernitrateprecipitatesthe
8 µg/g, uranium basis. The chlorine in UF can be determined silver halides. Spike recoveries can be improved by the
over the range of 4 to 160 µg/g, uranium basis. Higher addition of potassium iodide causing coprecipitation of the
concentrations may be covered by appropriate dilutions. The halides. The halides are collected on filter paper and are
detection limit for Br is 0.2 µg/g uranium basis and for Cl is 4 analyzed by X-ray fluorescence using two different crystal/
µg/g uranium basis. detector systems.
1.2 This standard may involve hazardous materials, opera-
4. Significance and Use
tions and equipment. This standard does not purport to address
4.1 The method is designed to show whether or not the
all of the safety concerns, if any, associated with its use. It is
the responsibility of the user of this standard to establish tested materials meet the specifications as given in Specifica-
tions C787 and C788.
appropriate safety and health practices and determine the
applicability of regulatory limitations prior to use.
5. Interferences
2. Referenced Documents
5.1 Plastic equipment must be used throughout the method
2.1 ASTM Standards: for uranyl fluoride as the hydrofluoric acid in the uranyl
C761 Test Methods for Chemical, Mass Spectrometric, fluoride leaches chloride from glassware causing a high bias.
5.2 Low recoveries may occur as the precipitate can be
Spectrochemical, Nuclear, and Radiochemical Analysis of
Uranium Hexafluoride difficult to transfer quantitatively to the filter paper. A surfac-
tant can be added (optional step) to minimize the adhesion of
C787 Specification for Uranium Hexafluoride for Enrich-
ment the precipitate to the walls of the beakers and the funnel.
C788 Specification for Nuclear-Grade Uranyl Nitrate Solu-
6. Apparatus
tion or Crystals
6.1 X-Ray Spectrometer, see Guide C1118 for the selection
C1118 Guide for Selecting Components for Wavelength-
of the X-ray Spectrometer.
Dispersive X-Ray Fluorescence (XRF) Systems
6.2 Plastic Vacuum Filtration Apparatus, for 47 mm diam-
D1193 Specification for Reagent Water
eter filter paper.
6.3 Filter Paper, 0.45 micron, 47 mm diameter.
6.4 Beakers, polypropylene, 250 mL.
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
6.5 Stirring Rods, plastic or Teflon.
Test.
6.6 X-ray Sample Support, Rings. Inner diameter approxi-
Current edition approved July 1, 2006. Published September 2006. Originally
mately 40 mm.
approved in 2001. Last previous edition approved in 2001 as C1508 – 01. DOI:
10.1520/C1508-01R06.
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 The filter must be Cl and Br free. Millipore membrane filter type HABP
Standards volume information, refer to the standard’s Document Summary page on (www.millipore.com) has been successfully used. An alternate is 15A from S.C.B,
the ASTM website. BP6, RN86, 07130 Soyons France. Any other equivalent is acceptable.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1508–01 (2006)
7. Reagents 8. Standard Preparation
7.1 Purity of Reagents—Reagent grade chemicals shall be 8.1 Pipette the following aliquots of spike solution (from
used in all tests. Unless otherwise indicated, it is intended that
7.17) into polypropylene beakers. 0 mL, 1 mL, 2 mL, 5 mL, 10
all reagents conform to the specifications of the Committee on mL. The aliquots represent 0µg Br, 5µg Br, 10µg Br, 25µg Br,
Analytical Reagents of theAmerican Chemical Society, where
50µgBrand0µgCl,100µgCl,200µgCl,500µgCl,1000µgCl.
such specifications are available. Other grades may be used,
8.2 Add 70 mL water to each beaker.
provided it is first ascertained that the reagent is of sufficiently
8.3 Follow steps 9.3-9.8 at the same time as the samples.
high purity to permit its use without lessening the accuracy of
the determination.
9. Procedure
7.2 Purity of Water—Unless otherwise indicated, references
9.1 Transfer a known aliquot of uranyl fluoride solution
to water shall be understood to mean reagent water conforming
(prepared following Test Methods C761) or uranyl nitrate that
to Specification D1193, Type I.
contains a known amount of uranium, approximately 5 g, with
7.3 Ammonium Hydroxide,NH OH, concentrated, specific
a plastic graduated cylinder into a polypropylene beaker
gravity 0.90.
containing 70 mL water.
7.4 Ammonium Hydroxide Solution, 1 + 3 (3.7 M). Dilute 1
part NH OH with 3 parts water.
NOTE 1—Recommend cleaning all laboratory equipment with ammo-
nium hydroxide solution (7.4) prior to use.
7.5 Surfactant, bromine and chlorine free. (Optional).
7.6 Surfactant Solution, 1 + 999.Add 1 mL of surfactant to
9.2 Follow laboratory QA practices and run the necessary
approximately 1 litre of water. (Optional).
duplicates, spikes and controls with the samples. Use the
7.7 Nitric Acid, HNO , concentrated, specific gravity 1.42.
solution prepared in 7.17 for the spikes.
7.8 Nitric Acid Solution, 1 + 999 (0.016 M). Add 1 mL of
NOTE 2—2 mL and 4 mL spike aliquots were found to be reasonable
concentrated HNO to approximately 200 mL of water. Add 1
volumes.
mL of the surfactant (7.6). (Optional). Dilute to 1 litre.
7.9 Sodium Nitrite, NaNO . 9.3 Add0.5mLofpotassiumiodidesolutiontoeachsample
and standard. (Optional step).
7.10 Sodium Nitrite Solution, 2 g/L. Dissolve1gof sodium
nitrite in water and dilute to 500 mL. Prepare fresh immedi-
9.4 Add 4 mL of surfactant solution 7.6. (Optional step).
ately before use.
9.5 Add 10 mL of sodium nitrite solution to each sample
7.11 Silver Nitrate, AgNO .
andstandard.Stireachsolutionwithadedicatedplasticstirring
7.12 Silver Nitrate Solution, 2 g/L. Dissolve2gof silver
rod and allow to stand for a minimum of 2 minutes.
nitrateinwateranddiluteto1litre.Keepawayfromlightinan
9.6 Slowly and with stirring add 25 mL of the silver nitrate
opaque bottle. The solution should be made fresh weekly.
solution. Remove the plastic stirring rods. Heat the solution in
Silver is an RCRA listed hazardous waste. Make up only as
a water bath at approximately 80°C 6 1
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