ASTM C1219-05

Standard Test Methods for Arsenic in Uranium Hexafluoride

SIGNIFICANCE AND USE
Arsenic compounds are suspected to cause corrosion in some materials used in UF6 handling equipment. Arsenic originates as a contaminant in fluorspar (CaF2) used to produce anhydrous hydrogen fluoride which is used subsequently in the production of UF 6.
These test methods are used to measure the arsenic content in UO2F2 solutions prepared from the hydrolysis of UF6 for determination of conformance to Specification C 787.
SCOPE
1.1 These test methods are applicable to the determination of total arsenic in uranium hexafluoride (UF6) by atomic absorption spectrometry. Two test methods are given: Test Method A-Arsine Generation-Atomic Absorption (Sections ), and Test Method B-Graphite Furnace Atomic Absorption ().
1.2 The test methods are equivalent. The limit of detection for each test method is 0.1 g As/g U when using a sample containing 0.5 to 1.0 g U. Test Method B does not have the complete collection details for precision and bias data thus the method appears as an appendix.
1.3 Test Method A covers the measurement of arsenic in uranyl fluoride (UO2F2) solutions by converting arsenic to arsine and measuring the arsine vapor by flame atomic absorption spectrometry.
1.4 Test Method B utilizes a solvent extraction to remove the uranium from the UO2F2 solution prior to measurement of the arsenic by graphite furnace atomic absorption spectrometry.
1.5 Both insoluble and soluble arsenic are measured when UF6 is prepared according to Test Method C 761.
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: 31-Jul-2005
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1219-92(1997) - Standard Test Methods for Arsenic in Uranium Hexafluoride
• Effective Date: 01-Aug-2005
• Replaced By: ASTM C1219-05(2009) - Standard Test Methods for Arsenic in Uranium Hexafluoride (Withdrawn 2015)
• Effective Date: 01-Jul-2009
• Referred By: ASTM C1022-17(2022) - Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
• Effective Date: 01-Aug-2005
• Referred By: ASTM C761-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
• Effective Date: 01-Aug-2005
• Referred By: ASTM C799-19 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions
• Effective Date: 01-Aug-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: C 1219 – 05
Standard Test Methods for
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Arsenic in Uranium Hexafluoride
This standard is issued under the fixed designation C 1219; 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 D 1193 Specification for Reagent Water
1.1 These test methods are applicable to the determination
3. Summary of Test Methods
of total arsenic in uranium hexafluoride (UF ) by atomic
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3.1 Arsine Generation-Atomic Absorption Spectromety
absorption spectrometry. Two test methods are given: Test
Method—The sample of UF is hydrolyzed and the UO F
6 2 2
Method A—Arsine Generation-Atomic Absorption (Sections
solution is fumed with sulfuric acid in the presence of boric
5-10), and Test Method B—Graphite FurnaceAtomicAbsorp-
acid to complex the fluoride. Potassium iodide is used to
tion (Appendix X1).
reduce arsenic(V) to arsenic(III). Sodium borohydride is used
1.2 The test methods are equivalent. The limit of detection
togeneratearsinevaporinahydridegeneratorwithsubsequent
for each test method is 0.1 µg As/g U when using a sample
measurement by flame atomic absorption spectrometry.
containing 0.5 to 1.0 g U. Test Method B does not have the
3.2 Graphite Furnace Atomic Absorption Spectrometry
complete collection details for precision and bias data thus the
Method—ThesampleofUF ishydrolyzed,andtheuraniumin
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method appears as an appendix.
the UO F solution is removed by extraction with tri(2-ethyl-
2 2
1.3 Test Method A covers the measurement of arsenic in
hexyl)phosphate/heptane. The aqueous phase containing the
uranyl fluoride (UO F ) solutions by converting arsenic to
2 2
arsenic is analyzed by graphite furnace atomic absorption.
arsine and measuring the arsine vapor by flame atomic absorp-
tion spectrometry.
4. Significance and Use
1.4 Test Method B utilizes a solvent extraction to remove
4.1 Arsenic compounds are suspected to cause corrosion in
the uranium from the UO F solution prior to measurement of
2 2
some materials used in UF handling equipment. Arsenic
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the arsenic by graphite furnace atomic absorption spectrom-
originatesasacontaminantinfluorspar(CaF )usedtoproduce
2
etry.
anhydrous hydrogen fluoride which is used subsequently in the
1.5 Both insoluble and soluble arsenic are measured when
production of UF .
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UF is prepared according to Test Method C 761.
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4.2 These test methods are used to measure the arsenic
1.6 This standard does not purport to address all of the
content in UO F solutions prepared from the hydrolysis of
2 2
safety concerns, if any, associated with its use. It is the
UF for determination of conformance to Specification C 787.
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responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
TEST METHOD A—ARSINE GENERATION-ATOMIC
bility of regulatory limitations prior to use.
ABSORPTION SPECTROMETRY
2. Referenced Documents
5. Interferences
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2.1 ASTM Standards:
5.1 The presence of hydrofluoric acid in the sample sup-
C 761 Test Methods for Chemical, Mass Spectrometric,
presses arsine generation when using sodium borohydride.
Spectrochemical, Nuclear, and Radiochemical Analysis of
Boric acid is added to complex the fluoride present at a molar
Uranium Hexafluoride 3
excess of 250 %.
C 787 Specification for Uranium Hexafluoride for Enrich-
5.2 Arsenic(V) must be reduced to arsenic(III) otherwise
ment
arsine will not be generated using sodium borohydride and
hydrochloric acid.
5.3 The reduction of arsenic(V) by potassium iodide is time
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dependentatroomtemperaturerequiringstrictadherencetothe
This test methods are under the jurisdiction of ASTM Committee C26 on
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
procedure.
Methods of Tests.
Current edition approvedAugust 1, 2005. Published September 2005. Originally
approved in 1992. Last previous edition approved in 1997 as C 1219 – 92 (1997).
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Petrik, K., and Krivan, V., “Radiotracer Investigation of the Interference of
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Hydrofluoric Acid in the Determination of Arsenic and Antimony by Hydride
Standards volume information, refer to the standard’s Document Summary page on GenerationAtomicAbsorption Spectroscopy,”AnalyticalChemistry,Vol 59, No. 20
the ASTM website. (1987), pp. 2426–2427.
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C1219–05
TABLE 1 Atomic Absorption Operating Parameter
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