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ASTM C1457-00(2005)

(Test Method)

Standard Test Method for the Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction

Standard Test Method for the Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction

SIGNIFICANCE AND USE
Uranium dioxide is used as a nuclear-reactor fuel. Gadolinium oxide is used as an additive to uranium dioxide. In order to be suitable for this purpose, these materials must meet certain criteria for impurity content. This test method is designed to determine whether the hydrogen content meets Specifications C 753, C 776, C 888, and C 922.
SCOPE
1.1 This test method applies to the determination of hydrogen in nuclear-grade uranium oxide powders and pellets to determine compliance with specifications. Gadolinium oxide (Gd2O3) and gadolinium oxide-uranium oxide powders and pellets may also be analyzed using this test method.
1.2 This standard describes a procedure for measuring the total hydrogen content of uranium oxides. The total hydrogen content results from absorbed water, water of crystallization, hydro-carbides and other hydrogenated compounds which may exist as fuel's impurities.
1.3 This test method covers the determination of 0.05 to 200 g of residual hydrogen.
1.4 This test method describes an electrode furnace carrier gas combustion system equipped with a thermal conductivity detector.
1.5 The preferred system of units is micrograms hydrogen per gram of sample (g/g sample) or micrograms hydrogen per gram of uranium (g/g U).
1.6 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-May-2005
ICS
27.120.30 - Fissile materials and nuclear fuel technology
Technical Committee
C26 - Nuclear Fuel Cycle
Drafting Committee
C26.05 - Methods of Test
Current Stage
Ref Project

Relations

Replaces
ASTM C1457-00 - Standard Test Method for the Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction
Effective Date
01-Jun-2005
Replaced By
ASTM C1457-00(2010)e1 - Standard Test Method for the Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction
Effective Date
01-Jun-2010
Referred By
ASTM C696-19 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets
Effective Date
01-Jun-2005
Referred By
ASTM C968-19 - Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide Pellets
Effective Date
01-Jun-2005

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ASTM C1457-00(2005) - Standard Test Method for the Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas ExtractionASTM C1457-00(2005) - Standard Test Method for the Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction
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ASTM C1457-00(2005) - Standard Test Method for the Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction
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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:C1457–00 (Reapproved 2005)
Standard Test Method for
Determination of Total Hydrogen Content of Uranium Oxide
1
Powders and Pellets by Carrier Gas Extraction
This standard is issued under the fixed designation C1457; 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 C888 Specification for Nuclear-Grade Gadolinium Oxide
(Gd O ) Powder
1.1 This test method applies to the determination of hydro- 2 3
C922 Specification for Sintered Gadolinium Oxide-
gen in nuclear-grade uranium oxide powders and pellets to
Uranium Dioxide Pellets
determine compliance with specifications. Gadolinium oxide
(Gd O ) and gadolinium oxide-uranium oxide powders and
2 3
3. Summary of Test Method
pellets may also be analyzed using this test method.
3.1 The total hydrogen content is determined using a hy-
1.2 This standard describes a procedure for measuring the
drogen analyzer. The hydrogen analyzer is based on the carrier
total hydrogen content of uranium oxides. The total hydrogen
gas method using argon or nitrogen as carrier gas. The actual
content results from absorbed water, water of crystallization,
configuration of the system may vary with vendor and model.
hydro-carbides and other hydrogenated compounds which may
3.2 Thesamplestobeanalyzedaredroppedintoapreheated
exist as fuel’s impurities.
graphite crucible, and then, heated up to a temperature of more
1.3 Thistestmethodcoversthedeterminationof0.05to200
than 1700°C in a graphite crucible. At that temperature
µg of residual hydrogen.
hydrogen, oxygen, nitrogen, and carbon monoxide (oxygen is
1.4 This test method describes an electrode furnace carrier
converted to CO when it reacts with the crucible) are released.
gas combustion system equipped with a thermal conductivity
The release gas is purified in the carrier gas stream by
detector.
oxidation and absorption columns. The hydrogen is separated
1.5 The preferred system of units is micrograms hydrogen
by chromatographic means and analyzed in a thermal conduc-
per gram of sample (µg/g sample) or micrograms hydrogen per
tivity detector.
gram of uranium (µg/g U).
1.6 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 Uranium dioxide is used as a nuclear-reactor fuel.
responsibility of the user of this standard to establish appro-
Gadolinium oxide is used as an additive to uranium dioxide. In
priate safety and health practices and determine the applica-
order to be suitable for this purpose, these materials must meet
bility of regulatory limitations prior to use.
certain criteria for impurity content. This test method is
2. Referenced Documents designed to determine whether the hydrogen content meets
2 Specifications C753, C776, C888, and C922.
2.1 ASTM Standards:
C753 Specification for Nuclear-Grade, Sinterable Uranium
5. Interferences
Dioxide Powder
5.1 Contamination of carrier gas, crucibles, or samples with
C776 Specification for Sintered Uranium Dioxide Pellets
extraneous sources of hydrogen may cause a positive bias. A
blankcorrectionwillhelptominimizethebiasfromcarriergas
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
and crucibles. Interference from adsorbed hydrogen on
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
samples may be eliminated by keeping the sample in an inert
Test.
atmosphere or vacuum.
Current edition approved June 1, 2005. Published December 2005. Originally
5.2 The purification system typically associated with the
approved in 2000. Last previous edition approved in 2000 as C1457–00. DOI:
10.1520/C1457-00R05.
recommended combustion and detection equipment is de-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
signed to minimize other expected sources of interferences,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
suchassulfur,halogens,carbonmonoxide,carbondioxide,and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. water.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C1457–00 (2005)
5.2.1 The nitrogen and hydrogen peaks are close together 7.8 Tin Flux, if Zr or Ti hydride standards are to be used.
and must be well-separated to prevent falsely high result from 7.9 Graphite Crucibles.
the nitrogen. The molecular sieve must be sufficiently long to 7.10 Tin Capsules.
separate the peaks and must be changed when th
...

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Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis

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5.1 Plutonium and uranium mixtures are used as nuclear reactor fuels. For use as a nuclear reactor fuel, the material must meet certain criteria for combined uranium and plutonium content, effective fissile content, and impurity content as described in Specifications C757 and C833. After dissolution using one of the procedures described in this practice, the material is assayed for plutonium and uranium to determine if the content is correct as specified by the purchaser.  
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1.3 One or more of the procedures in this practice may be applicable to unique plutonium materials, such as alloys, compounds, and scrap materials. The user must determine the applicability of this practice to such materials.  
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Procedure Number  
Procedure Title  
Section  
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2  
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14  
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15  
8  
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Powder  
16  
9  
Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder  
17  
10  
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Pellets  
18  
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ABSTRACT
This specification covers finished sintered and ground (uranium-plutonium) dioxide pellets for use in thermal reactors. It applies to uranium-plutonium dioxide pellets containing plutonium additions up to 15 % weight. The diversity of manufacturing methods shall be recognized by which uranium-plutonium dioxide pellets are produced and the many special requirements for chemical and physical characterization that may be imposed by the operating conditions to which the pellets will be subjected in specific reactor systems. The following are different chemical requirements that shall be determined: uranium content, plutonium content, impurity content, stoichiometry, moisture content, gas content, and americium-241 content. Nuclear requirements such as isotopic content, plutonium equivalent at a given date, equivalent boron content, and reactivity shall also be determined. Physical properties of the pellets like dimensions, density, grain size, pore morphology, plutonium-oxide homogeneity, plutonium-oxide particle size, plutonium-oxide particle distribution, integrity, and surface cracks shall be determined as well. The surfaces of finished pellets shall be visually free of loose chips, oil, macroscopic inclusions, and foreign materials. An estimate of the fuel pellet irradiation stability shall be obtained unless adequate allowance for such effects are factored into the fuel rod design. The estimate of the stability shall consist of either conformance to the thermal stability test as specified in the or by adequate correlation of manufacturing process or microstructure to in-reactor behavior, or both.
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4.1 Materials handling equipment operability and long-term integrity are concerns that originate during the design and fabrication sequences. Such concerns are most efficiently addressed during one or the other of these stages. Equipment operability and integrity can be compromised during handling and installation sequences. For this reason, the subject equipment should be handled and installed under closely controlled and supervised conditions.  
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4.5.2 Materials handling equipment should be capable of withstanding rigorous chemical cleaning and decontamination procedures.  
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4.1 The materials covered that must meet ASTM specifications are uranium metal and uranium oxide.  
4.2 Uranium materials are used as nuclear reactor fuel. For this use, these materials must meet certain criteria for uranium content, uranium-235 enrichment, and impurity content, as described in Specifications C753 and C776. The material is assayed for uranium to determine whether the content is as specified.  
4.3 Uranium alloys, refractory uranium materials, and uranium containing scrap and ash are unique uranium materials for which the user must determine the applicability of this practice. In general, these unique uranium materials are dissolved with various acid mixtures or by fusion with various fluxes.
SCOPE
1.1 This practice covers dissolution treatments for uranium materials that are applicable to the test methods used for characterizing these materials for uranium elemental, isotopic, and impurities determinations. Dissolution treatments for the major uranium materials assayed for uranium or analyzed for other components are listed.  
1.2 The treatments, in order of presentation, are as follows:    
Procedure Title  
Section  
Dissolution of Uranium Metal and Oxide with Nitric Acid  
8.1  
Dissolution of Uranium Oxides with Nitric Acid and Residue
Treatment  
8.2  
Dissolution of Uranium-Aluminum Alloys in Hydrochloric Acid
with Residue Treatment  
8.3  
Dissolution of Uranium Scrap and Ash by Leaching with Nitric
Acid and Treatment of Residue by Carbonate Fusion  
8.4  
Dissolution of Refractory Uranium-Containing Material by
Carbonate Fusion  
8.5  
Dissolution of Uranium—Aluminum Alloys
Uranium Scrap and Ash, and Refractory
Uranium-Containing Materials by
Microwave Treatment  
8.6  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM C1165-23(Test Method)
Standard Test Method for Determining Plutonium by Controlled-Potential Coulometry in H2SO4 at a Platinum Working Electrode

SIGNIFICANCE AND USE
5.1 This test method is used to ascertain whether or not materials meet specifications for plutonium concentration or plutonium mass fraction.  
5.1.1 The materials (nuclear grade plutonium nitrate solutions, plutonium metal, plutonium oxide powder, and mixed oxide and carbide powders and pellets) to which this test method applies are subject to nuclear safeguards regulations governing their possession and use. However, adherence to this test method does not automatically guarantee regulatory acceptance of the resulting safeguards measurements. It remains the sole responsibility of the user of this test method to ensure that its application to safeguards has the approval of the proper regulatory authorities.  
5.1.2 When used in conjunction with appropriate certified reference materials (CRMs), this test method can demonstrate traceability to the international measurements system (SI).  
5.2 Fitness for Purpose of Safeguards and Nuclear Safety Application—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.  
5.3 A chemical calibration of the coulometer is necessary for accurate results.
FIG. 1 Example of a Cell Design Used at Los Alamos National Laboratory (LANL)
SCOPE
1.1 This test method covers the determination of milligram quantities of plutonium in unirradiated uranium-plutonium mixed oxide having a U/Pu ratio range of 0.1 to 10. This test method is also applicable to plutonium metal, plutonium oxide, uranium-plutonium mixed carbide, various plutonium compounds including fluoride and chloride salts, and plutonium solutions.  
1.2 The recommended amount of plutonium for each aliquant in the coulometric analysis is 5 mg to 10 mg. Precision worsens for lower amounts of plutonium, and elapsed time of electrolysis becomes impractical for higher amounts of plutonium.  
1.3 The quantity values stated in SI units are to be regarded as standard. The quantity values with non-SI units are given in parentheses for information only.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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    sale 15% off