ASTM C1508-01(2011)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: C1508 − 01 (Reapproved 2011)
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.Anumber 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
all of the safety concerns, if any, associated with its use. It is 4.1 The method is designed to show whether or not the
the responsibility of the user of this standard to establish tested materials meet the specifications as given in Specifica-
appropriate safety and health practices and determine the tions C787 and C788.
applicability of regulatory limitations prior to use.
5. Interferences
2. Referenced Documents
5.1 Plastic equipment must be used throughout the method
for uranyl fluoride as the hydrofluoric acid in the uranyl
2.1 ASTM Standards:
C761Test Methods for Chemical, Mass Spectrometric, fluoride leaches chloride from glassware causing a high bias.
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
5.2 Low recoveries may occur as the precipitate can be
Uranium Hexafluoride
difficult to transfer quantitatively to the filter paper. A surfac-
C787Specification for Uranium Hexafluoride for Enrich-
tant can be added (optional step) to minimize the adhesion of
ment
the precipitate to the walls of the beakers and the funnel.
C788Specification for Nuclear-Grade Uranyl Nitrate Solu-
tion or Crystals
6. Apparatus
C1118Guide for Selecting Components for Wavelength-
6.1 X-Ray Spectrometer, see Guide C1118 for the selection
Dispersive X-Ray Fluorescence (XRF) Systems (With-
3 of the X-ray Spectrometer.
drawn 2011)
6.2 Plastic Vacuum Filtration Apparatus, for 47 mm diam-
D1193Specification for Reagent Water
eter filter paper.
6.3 Filter Paper, 0.45 micron, 47 mm diameter.
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
6.4 Beakers, polypropylene, 250 mL.
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
6.5 Stirring Rods, plastic or Teflon.
Current edition approved June 1, 2011. Published June 2011. Originally
6.6 X-ray Sample Support, Rings. Inner diameter approxi-
approved in 2001. Last previous edition approved in 2006 as C1508–01(2006).
DOI: 10.1520/C1508-01R1.
mately 40 mm.
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
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. The filter must be Cl and Br free. Millipore membrane filter type HABP
The last approved version of this historical standard is referenced on (www.millipore.com) has been successfully used. An alternate is 15A from S.C.B,
www.astm.org. 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 (Reapproved 2011)
7. Reagents 7.18 Potassium Iodide, KI. (Optional).
7.1 Purity of Reagents—Reagent grade chemicals shall be 7.19 Potassium Iodide Solution, (Optional), 1g I/L. Dis-
used in all tests. Unless otherwise indicated, it is intended that solve 0.131 g potassium iodide in water and dilute to 100 mL.
all reagents conform to the specifications of the Committee on The solution should be prepared weekly.
Analytical Reagents of theAmerican Chemical Society, where
8. Standard Preparation
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
8.1 Pipette the following aliquots of spike solution (from
high purity to permit its use without lessening the accuracy of
7.17)intopolypropylenebeakers.0mL,1mL,2mL,5mL,10
the determination.
mL. The aliquots represent 0µg Br, 5µg Br, 10µg Br, 25µg Br,
50µgBrand0µgCl,100µgCl,200µgCl,500µgCl,1000µgCl.
7.2 Purity of Water—Unless otherwise indicated, references
towatershallbeunderstoodtomeanreagentwaterconforming
8.2 Add 70 mL water to each beaker.
to Specification D1193, Type I.
8.3 Follow steps 9.3-9.8 at the same time as the samples.
7.3 Ammonium Hydroxide, NH OH, concentrated, specific
9. Procedure
gravity 0.90.
9.1 Transfer a known aliquot of uranyl fluoride solution
7.4 Ammonium Hydroxide Solution, 1 + 3 (3.7 M). Dilute 1
(prepared following Test Methods C761) or uranyl nitrate that
part NH OH with 3 parts water.
contains a known amount of uranium, approximately 5 g, with
7.5 Surfactant, bromine and chlorine free. (Optional).
a plastic graduated cylinder into a polypropylene beaker
7.6 Surfactant Solution, 1 + 999.Add 1 mLof surfactant to
containing 70 mL water.
approximately 1 litre of water. (Optional).
NOTE 1—Recommend cleaning all laboratory equipment with ammo-
7.7 Nitric Acid, HNO , concentrated, specific gravity 1.42.
nium hydroxide solution (7.4) prior to use.
9.2 Follow laboratory QA practices and run the necessary
7.8 Nitric Acid Solution, 1 + 999 (0.016 M). Add 1 mL of
concentrated HNO to approximately 200 mL of water.Add 1 duplicates, spikes and controls with the samples. Use the
solution prepared in 7.17 for the spikes.
mL of the surfactant (7.6). (Optional). Dilute to 1 litre.
7.9 Sodium Nitrite, NaNO . NOTE 2—2 mL and 4 mL spike aliquots were found to be reasonable
volumes.
7.10 Sodium Nitrite Solution, 2 g/L. Dissolve1gof sodium
9.3 Add0.5mLofpotassiumiodidesolutiontoeachsample
nitrite in water and dilute to 500 mL. Prepare fresh immedi-
and standard. (Optional step).
ately before use.
9.4 Add 4 mL of surfactant solution 7.6. (Optional step).
7.11 Silver Nitrate, AgNO .
9.5 Add 10 mL of sodium nitrite solution to each sample
7.12 Silver Nitrate Solution, 2 g/L. Dissolve2gof silver
andstandard.Stireachsolutionwithadedicatedplasticstirring
nitrateinwateranddiluteto1litre.Keepawayfromlightinan
rod and allow to stand for a minimum of 2 minutes.
opaque bottl
...