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ASTM C1832-16

(Test Method)

Standard Test Method for Determination of Uranium Isotopic Composition by the Modified Total Evaporation (MTE) Method Using a Thermal Ionization Mass Spectrometer

Standard Test Method for Determination of Uranium Isotopic Composition by the Modified Total Evaporation (MTE) Method Using a Thermal Ionization Mass Spectrometer

SIGNIFICANCE AND USE
5.1 Uranium material is used as a fuel in certain types of nuclear reactors. To be suitable for use as nuclear fuel, the starting material shall meet certain specifications such as those described in Specifications C753, C776, C787, C833, C967, C996, and C1008, or as specified by the purchaser. The isotope amount ratios of uranium material can be measured by mass spectrometry following this test method to ensure that they meet the specification.  
5.2 The MTE method can be used for a wide range of sample sizes even in samples containing as low as 50 μg of uranium. If the uranium sample is in the form of uranium hexafluoride, it can be converted into a uranium nitrate solution for measurement by the MTE method. The concentration of the loading solution for MTE has to be in the range of 1 to 6 mg/g to allow a sample loading of 2 to 6 μg of uranium. A minimum loading of 3 μg uranium per filament is recommended. This is needed to have a suitable ion signal especially for the two minor isotopes (234U and 236U) thus enabling the internal calibration of SEM versus the Faraday cups during the measurement.  
5.3 Until now, the instrument capabilities for the MTE method have only been implemented on the TRITON™ TIMS instrument.5 Therefore all recommendations for measurement parameters in this test method are specified for the TRITON™ TIMS instrument. The manufacturers of other TIMS instruments (for example, IsotopX and Nu Instruments) have plans to implement the modifications needed in their instruments to use the MTE method.  
5.4 The MTE method described here can also be extended to measurement of elements other than uranium. Note that the MTE method has already been implemented for plutonium and calcium.
SCOPE
1.1 This test method describes the determination of the isotope amount ratios of uranium material as nitrate solutions by the modified total evaporation (MTE) method using a thermal ionization mass spectrometer (TIMS) instrument.  
1.2 The analytical performance in the determination of the 235U/238U major isotope amount ratio by MTE is similar to the (“classical”) total evaporation (TE) method as described in Test Method C1672. However, in the MTE method, the evaporation process is interrupted on a regular basis to allow measurements and subsequent corrections for background form peak tailing, perform internal calibration of a secondary electron multiplier (SEM) detector versus the Faraday cups, peak centering, and ion source refocusing. Performing these calibrations and corrections on a regular basis during the measurement, improves precision, and significantly reduces uncertainties for the minor isotope amount ratios 234U/238U and 236U/238U as compared to the TE method.  
1.3 In principle, the MTE method yields major isotope amount ratios without the need for mass fractionation correction. However, depending on the measurement conditions, small variations are seen among sample turrets; therefore, a small correction based on measurements of a certified reference material is recommended to improve consistency. The uncertainty around the mass fractionation correction factor usually includes unity.  
1.4 Units—The values stated in SI units are to be regarded as the standard. When non-SI units are provided, they are for information only.  
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
14-Jan-2016
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

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ASTM C1832-16 - Standard Test Method for Determination of Uranium Isotopic Composition by the Modified Total Evaporation (MTE) Method Using a Thermal Ionization Mass SpectrometerASTM C1832-16 - Standard Test Method for Determination of Uranium Isotopic Composition by the Modified Total Evaporation (MTE) Method Using a Thermal Ionization Mass Spectrometer
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ASTM C1832-16 - Standard Test Method for Determination of Uranium Isotopic Composition by the Modified Total Evaporation (MTE) Method Using a Thermal Ionization Mass Spectrometer
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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:C1832 −16
Standard Test Method for
Determination of Uranium Isotopic Composition by the
Modified Total Evaporation (MTE) Method Using a Thermal
1
Ionization Mass Spectrometer
This standard is issued under the fixed designation C1832; 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 2. Referenced Documents
2
1.1 This test method describes the determination of the 2.1 ASTM Standards:
isotope amount ratios of uranium material as nitrate solutions C753Specification for Nuclear-Grade, Sinterable Uranium
by the modified total evaporation (MTE) method using a Dioxide Powder
thermal ionization mass spectrometer (TIMS) instrument. C776Specification for Sintered Uranium Dioxide Pellets
C787Specification for Uranium Hexafluoride for Enrich-
1.2 The analytical performance in the determination of the
235 238 ment
U/ U major isotope amount ratio by MTE is similar to the
C833Specification for Sintered (Uranium-Plutonium) Diox-
(“classical”)totalevaporation(TE)methodasdescribedinTest
ide Pellets
MethodC1672.However,intheMTEmethod,theevaporation
C859Terminology Relating to Nuclear Materials
processisinterruptedonaregularbasistoallowmeasurements
C967Specification for Uranium Ore Concentrate
and subsequent corrections for background form peak tailing,
C996Specification for Uranium Hexafluoride Enriched to
perform internal calibration of a secondary electron multiplier
235
Less Than 5% U
(SEM) detector versus the Faraday cups, peak centering, and
C1008 Specification for Sintered (Uranium-Plutonium)
ion source refocusing. Performing these calibrations and cor-
3
DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
rections on a regular basis during the measurement, improves
C1068Guide for Qualification of Measurement Methods by
precision, and significantly reduces uncertainties for the minor
234 238 236 238
a Laboratory Within the Nuclear Industry
isotope amount ratios U/ U and U/ U as compared to
C1128Guide for Preparation of Working Reference Materi-
the TE method.
als for Use in Analysis of Nuclear Fuel Cycle Materials
1.3 In principle, the MTE method yields major isotope
C1156Guide for Establishing Calibration for a Measure-
amount ratios without the need for mass fractionation correc-
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
tion. However, depending on the measurement conditions,
rials
small variations are seen among sample turrets; therefore, a
C1347Practice for Preparation and Dissolution of Uranium
small correction based on measurements of a certified refer-
Materials for Analysis
ence material is recommended to improve consistency. The
C1411Practice for The Ion Exchange Separation of Ura-
uncertainty around the mass fractionation correction factor
nium and Plutonium Prior to Isotopic Analysis
usually includes unity.
C1625Test Method for Uranium and Plutonium Concentra-
1.4 Units—The values stated in SI units are to be regarded tions and Isotopic Abundances by Thermal Ionization
Mass Spectrometry
as the standard. When non-SI units are provided, they are for
information only. C1672Test Method for Determination of Uranium or Pluto-
nium Isotopic Composition or Concentration by the Total
1.5 This standard does not purport to address all of the
Evaporation Method Using a Thermal Ionization Mass
safety concerns, if any, associated with its use. It is the
Spectrometer
responsibility of the user of this standard to establish appro-
D1193Specification for Reagent Water
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Standards volume information, refer to the standard’s Document Summary page on
Test. the ASTM website.
3
Current edition approved Jan. 15, 2016. Published January 2016. DOI: 10.1520/ The last approved version of this historical standard is referenced on
C1832-16. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1832−16
E2655Guide for Reporting Uncertainty of Test Results and 3.3.18 RSD—relative standard deviation—SD (see below)
Use of the Term Measurement Uncertainty inASTM Test divided by the mean value of the observations in repeated
Methods sampling
E2586Practice for Calculating and Using Basic Statistics
...

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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.  
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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).  
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5.6 This test method is applicable only to homogeneous solutions. This test method is not suitable for solutions containing solids.  
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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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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.  
5.2 Unique plutonium materials, such as alloys, compounds, and scrap metals, are typically dissolved with various acid mixtures or by fusion with various fluxes. Many plutonium salts are soluble in hydrochloric acid. One or more of the procedures included in this practice may be effective for some of these materials; however their applicability to a particular plutonium material shall be verified by the user.
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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  
1  
Dissolution of Plutonium Metal with Hydrochloric Acid at Room Temperature  
9  
2  
Dissolution of Plutonium Metal with Hydrochloric Acid and Heating  
10  
3  
Dissolution of Plutonium Metal with Sulfuric Acid  
11  
4  
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed
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12  
5  
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxides by Sodium Bisulfate Fusion  
13  
6  
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired Plutonium Oxide in Beakers  
14  
7  
Open-Vessel (with Reflux Condenser) Dissolution of Plutonium Oxide Powder  
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  
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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ASTM C833-23(Specification)
Standard Specification for Sintered (Uranium-Plutonium) Dioxide Pellets for Light Water Reactors

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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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1.1 This specification covers finished sintered and ground (U, Pu)O2 pellets for use in light water reactors. It applies to (U, Pu)O2 pellets containing a plutonium mass fraction up to 15 % (that is, mass of Pu divided by the sum of masses U, Pu, and Am yielding 0.15 or less).  
1.2 Pellets produced under this specification are available in four grades.  
1.2.1 Grade R—240Pu / (Pu + Am) isotope mass fraction is at least 19 %.  
1.2.2 Grade F—240Pu / (Pu + Am) isotope mass fraction is at least 7 % and less than 19 %.  
1.2.3 Grade N1—240Pu / (Pu + Am) isotope mass fraction is less than 7 %.  
1.2.4 Grade N2—240Pu /239Pu isotope mass fraction does not exceed 0.10 (10 %).  
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1.1 This terminology standard contains terms, definitions, descriptions of terms, nomenclature, and explanations of acronyms and symbols specifically associated with standards under the jurisdiction of Committee C26 on Nuclear Fuel Cycle. The content of this terminology standard may also be applicable to documents not under the jurisdiction of Committee C26, in which case this terminology standard may be referenced in those documents.  
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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.  
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1.2.1.2 The equipment will generally be used over a long-term life cycle (for example, in excess of two years), but equipment intended for use over a shorter life cycle is not excluded.
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SCOPE
1.1 This test method describes the determination of dissolved plutonium from unirradiated nuclear-grade (that is, high-purity) materials by controlled-potential coulometry. Controlled-potential coulometry may be performed in a choice of supporting electrolytes, such as 0.9 mol/L (0.9 M) HNO3, 1 mol/L (1 M) HClO4, 1 mol/L (1 M) HCl, 5 mol/L (5 M) HCl, and 0.5 mol/L (0.5 M) H2SO4. Limitations on the use of selected supporting electrolytes are discussed in Section 6. Optimum quantities of plutonium for this procedure are 5 mg to 20 mg.  
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1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are 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.  
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ASTM
ASTM C1204-14(2023)(Test Method)
Standard Test Method for Uranium in Presence of Plutonium by Iron(II) Reduction in Phosphoric Acid Followed by Chromium(VI) Titration

SIGNIFICANCE AND USE
4.1 Factors governing selection of a method for the determination of uranium include available quantity of sample, sample purity, desired level of reliability, and equipment availability.  
4.2 This test method is suitable for samples between 20 mg to 300 mg of uranium, is applicable to fast breeder reactor (FBR)-mixed oxides having a uranium to plutonium ratio of 2.5 and greater, is tolerant towards most metallic impurity elements usually specified for FBR-mixed oxide fuel, and uses no special equipment.  
4.3 The ruggedness of the titration method has been studied for both the volumetric (6) and the weight (7) titration of uranium with dichromate.
SCOPE
1.1 This test method covers unirradiated uranium-plutonium mixed oxide having a uranium to plutonium ratio of 2.5 and greater. The presence of larger amounts of plutonium (Pu) that give lower uranium to plutonium ratios may give low analysis results for uranium (U) (1)2, if the amount of plutonium together with the uranium is sufficient to slow the reduction step and prevent complete reduction of the uranium in the allotted time. Use of this test method for lower uranium to plutonium ratios may be possible, especially when 20 mg to 50 mg quantities of uranium are being titrated rather than the 100 mg to 300 mg in the study cited in Ref (1). Confirmation of that information should be obtained before this test method is used for ratios of uranium to plutonium less than 2.5.  
1.2 The amount of uranium determined in the data presented in Section 12 was 20 mg to 50 mg. However, this test method, as stated, contains iron in excess of that needed to reduce the combined quantities of uranium and plutonium in a solution containing 300 mg of uranium with uranium to plutonium ratios greater than or equal to 2.5. Solutions containing up to 300 mg uranium with uranium to plutonium ratios greater than or equal to 2.5 have been analyzed (1) using the reagent volumes and conditions as described in Section 10.  
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. For specific hazard statements, see Section 8.  
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 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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