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ASTM C1845-16

(Practice)

Standard Practice for The Separation of Lanthanide Elements from Uranium Matrices Using High Pressure Ion Chromatography (HPIC) for Isotopic Analyses by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

Standard Practice for The Separation of Lanthanide Elements from Uranium Matrices Using High Pressure Ion Chromatography (HPIC) for Isotopic Analyses by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

SIGNIFICANCE AND USE
5.1 The measurement of isotopic distributions for the lanthanide series elements is of important to all phases of the nuclear fuels cycle. Examples include the purification of the Nd isotopes from Ce and Sm isotopes for the determination of atom percent fission through the production of 148Nd in irradiated nuclear fuels using Practice C1769, determination of rare earth content and isotopic distribution in Uranium Ore Concentrates (UOC) for source term and production of lanthanide fission products in irradiated nuclear fuels for determination of performance, improvements of depletion codes, and analysis of burnup indicators.3
SCOPE
1.1 This practice provides instructions for the rapid separation of lanthanide elements using high pressure ion chromatography (HPIC) from dissolved uranium materials such as: nuclear fuels, uranium ores, hydrolyzed UF6, and depleted, natural, or enriched oxides/powders, or metals. When optimized, this technique will produce purified elemental fractions of the lanthanide elements isolated from the bulk uranium matrix allowing for isotopic assay using inductively coupled plasma mass spectrometry (ICP-MS).  
1.2 This practice is most applicable for analyte concentrations of nanograms per gram uranium or higher. For ICP-MS detection and measurement of analyte concentrations lower than this, it would be necessary to perform additional pre-cleanup or concentration techniques, or both, which are not addressed in this practice.  
1.3 When combined with isotope dilution, this practice can also be used for improved precision assays of the lanthanide elements using the principle of isotope dilution mass spectrometry (IDMS).  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this practice.  
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
Published
Publication Date
31-May-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

Relations

Refers
ASTM C1168-15 - Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
Effective Date
01-Sep-2015
Refers
ASTM C1052-20 - Standard Practice for Bulk Sampling of Liquid Uranium Hexafluoride
Effective Date
01-Jul-2020
Refers
ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
Effective Date
15-Jun-2014
Referred By
ASTM E321-20 - Standard Test Method for Atom Percent Fission in Uranium and Plutonium Fuel (Neodymium-148 Method)
Effective Date
01-Jun-2016

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ASTM C1845-16 - Standard Practice for The Separation of Lanthanide Elements from Uranium Matrices Using High Pressure Ion Chromatography (HPIC) for Isotopic Analyses by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)ASTM C1845-16 - Standard Practice for The Separation of Lanthanide Elements from Uranium Matrices Using High Pressure Ion Chromatography (HPIC) for Isotopic Analyses by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
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ASTM C1845-16 - Standard Practice for The Separation of Lanthanide Elements from Uranium Matrices Using High Pressure Ion Chromatography (HPIC) for Isotopic Analyses by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
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Standards Content (Sample)

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.
Designation: C1845 − 16
Standard Practice for
The Separation of Lanthanide Elements from Uranium
Matrices Using High Pressure Ion Chromatography (HPIC)
for Isotopic Analyses by Inductively Coupled Plasma Mass
1
Spectrometry (ICP-MS)
This standard is issued under the fixed designation C1845; 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 practice provides instructions for the rapid separa- 2.1 ASTM Standards:
tion of lanthanide elements using high pressure ion chroma- C859Terminology Relating to Nuclear Materials
tography (HPIC) from dissolved uranium materials such as: C1052Practice for Bulk Sampling of Liquid Uranium
nuclear fuels, uranium ores, hydrolyzed UF , and depleted, Hexafluoride
6
natural, or enriched oxides/powders, or metals. When C1075Practices for Sampling Uranium-Ore Concentrate
optimized, this technique will produce purified elemental C1168PracticeforPreparationandDissolutionofPlutonium
fractions of the lanthanide elements isolated from the bulk Materials for Analysis
uranium matrix allowing for isotopic assay using inductively C1347Practice for Preparation and Dissolution of Uranium
coupled plasma mass spectrometry (ICP-MS). Materials for Analysis
C1689Practice for Subsampling of Uranium Hexafluoride
1.2 This practice is most applicable for analyte concentra-
C1769Practice for Analysis of Spent Nuclear Fuel to De-
tions of nanograms per gram uranium or higher. For ICP-MS
termine Selected Isotopes and Estimate Fuel Burnup
detection and measurement of analyte concentrations lower
D1193Specification for Reagent Water
than this, it would be necessary to perform additional pre-
E105Practice for Probability Sampling of Materials
cleanup or concentration techniques, or both, which are not
addressed in this practice.
3. Terminology
1.3 When combined with isotope dilution, this practice can
3.1 Definitions—For definitions of terms used in this
also be used for improved precision assays of the lanthanide
practice, refer to Terminology C859.
elementsusingtheprincipleofisotopedilutionmassspectrom-
etry (IDMS). 4. Summary of Practice
1.4 The values stated in SI units are to be regarded as
4.1 Solid samples are dissolved according to Practices
standard. No other units of measurement are included in this C1168, C1347, or other appropriate methods. Uranium
practice.
hexafluoride can be sampled in accordance with Practices
C1052 and C1689. The resulting dissolver solution is pro-
1.5 This standard does not purport to address all of the
cessed to produce solutions of isolated lanthanide elements for
safety concerns, if any, associated with its use. It is the
mass spectrometric isotopic analysis. The elements are selec-
responsibility of the user of this standard to establish appro-
tivelyseparatedfromthedissolversolutionandcollectedusing
priate safety and health practices and determine the applica-
HPIC instrumentation equipped with automated fraction col-
bility of regulatory limitations prior to use.
lection. Appropriate aliquots of the unseparated dissolutions
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
2
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Test. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved June 1, 2016. Published June 2016. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
C1845-16. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1845 − 16
are taken to provide up to 100 ng/mL of a lanthanide element compartment should be employed to maintain consistency
on the analytical column to be separated from 3.5 mg/mL or between sample analyses.
less of uranium. In a strong nitric acid matrix, no pre-
7. Apparatus
separation valence adjustments are necessary.
7.1 High pressure ion chromatograph equipped with a
NOTE 1—This practice has been verified to separate 0.7 mg of total
singlevariablespeedgradientpumpcapableofdeliveringflow
uraniumfromthelanthanideanalytes.20ngtotalofeachanalytehasbeen
rates of 0.001 to 10 mL/min.The system requires eluent degas
shown to have efficient resolution on the column to yield purified
capabilityandalow
...

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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).  
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1.2.4 Grade N2—240Pu /239Pu isotope mass fraction does not exceed 0.10 (10 %).  
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4.1 The purpose of this guide is to provide information that will help to ensure that nuclear fuel dissolution facilities are conceived, designed, fabricated, constructed, and installed in an economic and efficient manner. This guide will help facilities meet the intended performance functions, eliminate or minimize the possibility of nuclear criticality and provide for the protection of both the operator personnel and the public at large under normal and abnormal (emergency) operating conditions as well as under credible failure or accident conditions.
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1.2.1.1 Dissolution Procedures—Fuel compositions, fuel element geometry, and fuel manufacturing methods are subject to continuous change in response to the demands of new reactor designs and requirements. These changes preclude the inclusion of design considerations for dissolvers suitable for the processing of all possible fuel types. This guide will only address equipment associated with dissolution cycles for those fuels that have been used most extensively in reactors as of the time of issue (or revision) of this guide. (See Appendix X1.)  
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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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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.  
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Section  
Dissolution of Uranium Metal and Oxide with Nitric Acid  
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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

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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.
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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.  
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ASTM C1455-14(2023)(Test Method)
Standard Test Method for Nondestructive Assay of Special Nuclear Material Holdup Using Gamma-Ray Spectroscopic Methods

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5.1 Measurement results from this test method assists in demonstrating regulatory compliance in such areas as safeguards SNM inventory control, criticality control, waste disposal, and decontamination and decommissioning (D&D). This test method can apply to the measurement of holdup in process equipment or discrete items whose gamma-ray absorption properties may be measured or estimated. This method may be adequate to accurately measure items with complex distributions of radioactive and attenuating material, however, the results are subject to larger measurement uncertainties than measurements of less complex distributions of radioactive material.  
5.2 Scan—A scan is used to provide a qualitative indication of the extent, location, and the relative quantity of holdup. It can be used to plan or supplement the quantitative measurements.  
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5.1 Factors governing selection of a method for the determination of plutonium include available quantity of sample, sample purity, desired level of reliability, and equipment.  
5.1.1 This test method determines 5 mg to 20 mg of plutonium with prior dissolution using Practice C1168.  
5.1.2 This test method calculates plutonium mass fraction in solutions and solids using an electrical calibration based upon Ohm’s Law and the Faraday Constant.  
5.1.3 Chemical standards are used for quality control. When prior chemical separation of plutonium is necessary to remove interferences, the quality control standards should be included with each chemical separation batch (9).  
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.
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.  
1.2 Plutonium-bearing materials are radioactive and toxic. Adequate laboratory facilities, such as gloved boxes, fume hoods, controlled ventilation, etc., along with safe techniques must be used in handling specimens containing these materials.  
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.  
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 C1128-23(Guide)
Standard Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle Materials

SIGNIFICANCE AND USE
5.1 Certified reference materials (CRMs) prepared from nuclear materials are well characterized, traceable, and sufficiently homogenous and stable for their intended use. Usually they are certified using the most unbiased and precise measurement methods available, often with more than one laboratory being used on a national or international level. CRMs are at the top of the metrological hierarchy of reference materials. A graphical representation of a typical national nuclear measurement system is shown in Fig. 3.
FIG. 3 Typical National Nuclear Measurement System  
5.2 Working reference materials (WRMs) need to have quality characteristics that are similar to CRMs, although the rigor used to achieve those characteristics is not usually as stringent as for CRMs. Similarly, production of WRMs should be in accordance with applicable requirements of ISO 17034. Where possible, CRMs are typically used to calibrate the methods used for establishing reference values assigned to WRMs, thus providing traceability to CRMs as required by ISO/IEC 17025. A WRM is normally prepared for a specific application.  
5.3 Because of the importance of having highly reliable measurement data from nuclear material analysis, particularly for material control and accountability purposes, CRMs are used for calibration when available. However, CRMs prepared from nuclear materials are not always available for specific applications. Thus, there may be a need for a laboratory to prepare nuclear material WRMs to meet specific needs; for example, to match the matrix in process samples. In such cases, a WRM can be tailored to meet specific needs of a process or laboratory. Also, CRM supply may be too limited for use in the quantities needed for long-term, routine use. When properly prepared, WRMs will serve equally well as CRMs for most applications, and using WRMs will help preserve supplies of CRMs.  
5.4 Difficulties may be encountered in the preparation of RMs from nuclear materials becaus...
SCOPE
1.1 This guide covers the preparation and characterization of working reference materials (WRM) that are produced by a laboratory for its own use in the analysis of nuclear fuel cycle materials. Guidance is provided for proper planning, preparation, packaging, and storage; requirements for characterization; homogeneity and stability considerations; and value assignment. When traceability to SI is desired for a WRM, it will be achieved by a defined, statistically sound characterization process that is traceable to a certified value on a certified reference materials. While the guidance provided is generic for nuclear fuel cycle materials, detailed examples for some materials are provided in the appendixes.  
1.2 This guide does not apply to the production and characterization of certified reference materials (CRM). Refer to ISO 17034 and ISO Guide 35 for guidance on reference material production, characterization, certification, sale, and distribution requirements.  
1.3 The information provided by this guide is found in the following sections:    
Section  
Perform WRM Planning  
6  
Prepare and Process Materials  
7  
Packaging and Storage of Materials  
8  
Perform Homogeneity Study  
9  
Perform Stability Studies  
10  
Characterize Materials  
11  
Perform Uncertainty Analysis  
12  
Produce Documentation  
13  
Carry Out WRM Utilization and Monitoring  
14  
1.4 The values stated in SI units are to be regarded as standard. The non-SI units of molar, M, and normal, N, are also regarded as standard. Any non-SI units of measurement shown in parentheses 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6...

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