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ASTM C1477-06

(Test Method)

Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry

Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry

SIGNIFICANCE AND USE
The test method is capable of measuring uranium isotopic abundances of 234U, 235U, 236U and 238U as required by Specifications C 787 and C 996.
SCOPE
1.1 This test method covers the isotopic abundance analysis of 234U, 235U, 236U and 238U in samples of hydrolysed uranium hexafluoride (UF6) by inductively coupled plasma source, multi-collector, mass spectrometry (ICP-MC-MS). The method applies to material with  235U abundance in the range of 0.2 to 6 % mass. This test method is also described in ASTM STP 1344.
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
30-Jun-2006
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 C1477-00 - Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafloride by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry
Effective Date
01-Jul-2006
Replaced By
ASTM C1477-08 - Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry
Effective Date
01-Jun-2008
Referred By
ASTM C761-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
Effective Date
01-Jul-2006
Referred By
ASTM C1636-22 - Standard Guide for Determination of Uranium-232 in Uranium Hexafluoride
Effective Date
01-Jul-2006
Referred By
ASTM C1880-19 - Standard Practice for Sampling Gaseous Uranium Hexafluoride using Alumina Pellets
Effective Date
01-Jul-2006
Referred By
ASTM C1913-21 - Standard Practice for Sampling Gaseous Uranium Hexafluoride Using Zeolite in Single-Use Destructive Assay Sampler
Effective Date
01-Jul-2006

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ASTM C1477-06 - Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass SpectrometryASTM C1477-06 - Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry
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ASTM C1477-06 - Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry
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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: C 1477 – 06
Standard Test Method for
Isotopic Abundance Analysis of Uranium Hexafluoride and
Uranyl Nitrate Solutions by Multi-Collector, Inductively
1
Coupled Plasma-Mass Spectrometry
This standard is issued under the fixed designation C 1477; 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 samples are hydrolysed, diluted and acidified with nitric acid.
Uranic solution samples are diluted and acidified with nitric
1.1 This test method covers the isotopic abundance analysis
234 235 236 238
acid. Subsequently, an internal reference of thorium isotopes is
of U, U, Uand Uinsamplesofhydrolyseduranium
added to each diluted sample.
hexafluoride (UF ) by inductively coupled plasma source,
6
3.2 The samples are contained in polypropylene tubes that
multi-collector,massspectrometry(ICP-MC-MS).Themethod
235
are inserted into the auto-sampler rack of the mass spectrom-
applies to material with U abundance in the range of 0.2 to
eter. Sample details are input to the computer and the instru-
6 % mass. This test method is also described in ASTM
ment is prepared for measurement. The automatic measuring
STP 1344.
sequence is initiated.
1.2 This standard does not purport to address all of the
3.3 Uranium Isotopic Reference Materials (UIRMs) are
safety concerns, if any, associated with its use. It is the
used to calibrate the instrument. Each UIRM is prepared in
responsibility of the user of this standard to establish appro-
aqueoussolution(acidifiedwithnitricacid)andspikedwiththe
priate safety and health practices and determine the applica-
same internal reference as the samples. This calibration solu-
bility of regulatory limitations prior to use.
tion is measured and a mass bias parameter is calculated that is
2. Referenced Documents
stored and subsequently imported into each of the sample
4
2
measurements to correct the measured uranium isotopic ra-
2.1 ASTM Standards:
tios.
C 761 Test Methods for Chemical, Mass Spectrometric,
3.4 Measurements of isotopic ratios in the calibration solu-
Spectrochemical, Nuclear, and Radiochemical Analysis of
tion and the subsequent samples are initiated by customised
Uranium Hexafluoride
230 232
software. Using the Th / Th ratios (that are acquired
C 787 Specification for Uranium Hexafluoride for Enrich-
234 238 235 238 236 238
simultaneously to the U/ U, U/ U and U/ U
ment
ratios) and the mass bias parameter imported from the calibra-
C 996 Specification for Uranium Hexafluoride Enriched to
235
tion, the mass bias factor is computed. The mass bias factor is
Less Than 5 % U
234 238 235 238
then used to correct the measured U/ U, U/ U
D 1193 Specification for Reagent Water
236 238
and U/ U ratios in “real time.” The abundances are
2.2 Other Document:
expressed as % atomic. Details of the mass bias correction are
STP 1344 Applications of Inductively Coupled Plasma-
presented in Appendix X1.
Mass Spectrometry (ICP-MS) to Radionuclide Determi-
3
nations
4. Significance and Use
3. Summary of Test Method 4.1 The test method is capable of measuring uranium
234 235 236 238
isotopic abundances of U, U, U and U as required
3.1 Samples are received either in the form of uranium
by Specifications C 787 and C 996.
hexafluoride (UF ) or aqueous uranic solution. The UF
6 6
5. Interferences
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
5.1 Mass Bias—Electrostatic repulsion between uranium
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
ions causes a so-called “mass bias” effect. Mass bias is
Test .
Current edition approved July 1, 2006. Published August 2006. Originally
observed as an enhancement in the number of ions detected at
approved in 2000. Last previous edition approved in 2000 as C 1477 – 00.
the collectors from the heavier uranium isotopes relative to the
2
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
4
the ASTM website. Theuraniumisotopicmeasurementprecision,limitofdetectionanduncertainty
3
Available from ASTM Headquarters. of measurement are listed in Section 15, Section 16 andAppendix X1 respectively.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C1477–06
lighter uranium isotopes. A calibration procedure is used to 7. Reagents
correct the mass spectrometer for mass bias.
7.1 Purity of Water—Demineralised
...

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SIGNIFICANCE AND USE
5.1 This test method allows the determination of 241Am in a plutonium solution without separation of the americium from the plutonium. It is generally applicable to any solution containing 241Am.  
5.2 The 241Am in solid plutonium materials may be determined when these materials are dissolved (see Practice C1168).  
5.3 When the plutonium solution contains unacceptable levels of fission products or other materials, this method may be used following a tri-n-octylphosphine oxide (TOPO) extraction, ion exchange or other similar separation techniques (see Test Methods C758 and C759).  
5.4 This test method is less subject to interferences from plutonium than alpha counting since the energy of the gamma ray used for the analysis is better resolved from other gamma rays than the alpha particle energies used for alpha counting.  
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1.1 This test method covers the quantitative determination of 241Am by gamma-ray spectrometry in plutonium nitrate solution samples that do not contain significant amounts of radioactive fission products or other high specific activity gamma-ray emitters.  
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1.3 The values stated in SI units are to be regarded as standard. Additionally, the non-SI units of electron volts, kiloelectron volts, and liters are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM C1168-23(Practice)
Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis

SIGNIFICANCE AND USE
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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1.1 This practice is a compilation of dissolution techniques for plutonium materials that are applicable to the test methods used for characterizing these materials. Dissolution treatments for the major plutonium materials assayed for plutonium or analyzed for other components are listed. Aliquots of the dissolved materials are dispensed on a mass basis when one of the analyses must be of high precision, such as plutonium assay; otherwise they are dispensed on a volume basis.  
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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.  
1.4 The treatments, in order of presentation, are as follows:    
Procedure Number  
Procedure Title  
Section  
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Dissolution of Plutonium Metal with Hydrochloric Acid at Room Temperature  
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2  
Dissolution of Plutonium Metal with Hydrochloric Acid and Heating  
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Dissolution of Plutonium Metal with Sulfuric Acid  
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Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxides by Sodium Bisulfate Fusion  
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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  
1.5 The values stated in SI units are to be regarded as standard. The non-SI unit of molarity (M) is also to be regarded as standard. Values in parentheses (non-SI units), where provided, are for information only and are not considered standard.  
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5.1 Uranium hexafluoride is a basic material used to produce nuclear reactor fuel. To be suitable for this purpose, the material must meet criteria for isotopic composition. This test method is designed to determine whether the material meets the requirements described in Specifications C787 and C996.
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ASTM C833-23(Specification)
Standard Specification for Sintered (Uranium-Plutonium) Dioxide Pellets for Light Water Reactors

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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4.5.1 Boots and similar protective covers should not restrict movement of the equipment, should be properly sealed to the equipment and should withstand the radiation, cell atmosphere, dust, cell temperatures, chemical exposures, and cleaning and decontamination reagents, and also resist snags and tearing.  
4.5.2 Materials handling equipment should be capable of withstanding rigorous chemical cleaning and decontamination procedures.  
4.5.3 Materials handling equipment should be designed and fabricated to remain dimensionally stable throughout its life cycle.  
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SCOPE
1.1 Intent:  
1.1.1 This guide covers materials handling equipment used in hot cells (shielded cells) for the processing and handling of nuclear and radioactive materials. The intent of this guide is to aid in the selection and design of materials handling equipment for hot cells in order to minimize equipment failures and maximize the equipment utility.  
1.1.2 It is intended that this guide record the principles and caveats that experience has shown to be essential to the design, fabrication, installation, maintenance, repair, replacement, and decontamination and decommissioning of materials handling equipment capable of meeting the stringent demands of operating, dependably and safely, in a hot cell environment where operator visibility is limited due to the radiation exposure hazards.  
1.1.3 This guide may apply to materials handling equipment in other radioactive remotely operated facilities such as suited entry repair areas and canyons, but does not apply to materials handling equipment used in commercial power reactors.  
1.1.4 This guide covers mechanical master-slave manipulators and electro-mechanical manipulators, but does not cover electro-hydraulic manipulators.  
1.2 Applicability:  
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Standard Practice for Sampling of Gaseous Uranium Hexafluoride for Enrichment

SIGNIFICANCE AND USE
5.1 Uranium hexafluoride is normally produced and handled in large (typically 1 to 14-ton) quantities and must, therefore, be characterized by reference to representative samples (see ISO 7195). The samples are used to determine compliance with the applicable commercial specification C787. The quantities involved, physical properties, chemical reactivity, and hazardous nature of UF6 are such that for representative sampling, specially designed equipment must be used and operated in accordance with the most carefully controlled and stringent procedures. This practice can be used by UF6 converters to review the effectiveness of existing procedures or as a guide to the design of equipment and procedures for future use.  
5.2 The intention of this practice is to avoid liquid UF6 sampling once the cylinder has been filled. For safety reasons, manipulation of large quantities of liquid UF6 should be avoided when possible.  
5.3 It is emphasized that this practice is not meant to address conventional or nuclear criticality safety issues.
SCOPE
1.1 This practice covers methods for withdrawing representative sample(s) of uranium hexafluoride (UF6) during a transfer occurring in the gas phase. Such transfer in the gas phase can take place during the filling of a cylinder during a continuous production process, for example the distillation column in a conversion facility. Such sample(s) may be used for determining compliance with the applicable commercial specification, for example Specification C787.  
1.2 Since UF6 sampling is taken during the filling process, this practice does not address any special additional arrangements that may be agreed upon between the buyer and the seller when the sampled bulk material is being added to residues already present in a container (“heels recycle”). Such arrangements will be based on QA procedures such as traceability of cylinder origin (to prevent for example contamination with irradiated material).  
1.3 If the receiving cylinder is purged after filling and sampling, special verifications must be performed by the user to verify the representativity of the sample(s). It is then expected that the results found on volatile impurities with gas phase sampling may be conservative.  
1.4 This practice is only applicable when the transfer occurs in the gas phase. When the transfer is performed in the liquid phase, Practice C1052 should apply. This practice does not apply to gas sampling after the cylinder has been filled since the sample taken will not be representative of the cylinder.  
1.5 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.  
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ASTM C1347-08(2023)(Practice)
Standard Practice for Preparation and Dissolution of Uranium Materials for Analysis

SIGNIFICANCE AND USE
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