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ASTM C1853-17

(Test Method)

Standard Test Method for The Determination of Carbon (Total) Content in Mixed Oxide ((U, Pu)O2) Sintered Pellets by Direct Combustion-Infrared Detection Method

Standard Test Method for The Determination of Carbon (Total) Content in Mixed Oxide ((U, Pu)O<inf>2</inf>) Sintered Pellets by Direct Combustion-Infrared Detection Method

SIGNIFICANCE AND USE
5.1 MOX is used as a nuclear-reactor fuel. This test method is designed to determine whether the carbon content of the pellets meet the requirements of the fuel specification. Examples of these requirements are given in Specification C833.  
5.2 This method is suitable for all sintered MOX pellets containing up to 12 weight % PuO2 when the UO2 and PuO2 meet the requirements of Specifications C753 and C757. The method uncertainty is related to the concentration of the carbon in the sample. At lower concentrations, the relative uncertainty increases. At carbon contents close to the typical carbon content specification limit (100 μg carbon/g U + Pu metal) the method uncertainty is on the order of 5 %, but exact method performance is difficult to determine due to the lack of matrix matched certified reference material.
SCOPE
1.1 This test method is an alternative to Test Method C698 for the determination of carbon in nuclear grade sintered mixed oxide (MOX) fuel pellets. The method for the determination of carbon presented in Test Method C698 consists of combusting carbon contained in MOX pellets with oxygen in a high-frequency induction furnace and detecting the resulting carbon dioxide using a thermal conductivity cell. The method for the determination of carbon presented in this test method consists of combusting carbon contained in MOX pellets with oxygen in a high-frequency induction furnace and subsequent detection of the resulting carbon dioxide (CO2) using a non-dispersive infrared detector (NDIR). Sulfur oxide is stripped from the carrier gas stream by a cellulose filter prior to the detection of CO2.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard may involve hazardous material, operations, and equipment. 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 consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

General Information

Status
Published
Publication Date
31-May-2017
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 C753-16 - Standard Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
Effective Date
01-Feb-2016
Refers
ASTM C1408-16 - Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
Effective Date
01-Mar-2016
Refers
ASTM C757-16 - Standard Specification for Nuclear-Grade Plutonium Dioxide Powder for Light Water Reactors
Effective Date
01-Apr-2016
Refers
ASTM C698-16 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O<inf>2</inf>)
Effective Date
01-Jun-2016
Refers
ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
Effective Date
15-Jun-2014
Referred By
ASTM C1865-18 - Standard Test Method for The Determination of Carbon and Sulfur Content in Plutonium Oxide Powder by the Direct Combustion-Infrared Spectrophotometer
Effective Date
01-Jun-2017

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ASTM C1853-17 - Standard Test Method for The Determination of Carbon (Total) Content in Mixed Oxide ((U, Pu)O<inf>2</inf>) Sintered Pellets by Direct Combustion-Infrared Detection MethodASTM C1853-17 - Standard Test Method for The Determination of Carbon (Total) Content in Mixed Oxide ((U, Pu)O<inf>2</inf>) Sintered Pellets by Direct Combustion-Infrared Detection Method
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ASTM C1853-17 - Standard Test Method for The Determination of Carbon (Total) Content in Mixed Oxide ((U, Pu)O<inf>2</inf>) Sintered Pellets by Direct Combustion-Infrared Detection Method
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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: C1853 − 17
Standard Test Method for
The Determination of Carbon (Total) Content in Mixed Oxide
((U, Pu)O ) Sintered Pellets by Direct Combustion-Infrared
2
1
Detection Method
This standard is issued under the fixed designation C1853; 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 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This test method is an alternative to Test Method C698
C698 Test Methods for Chemical, Mass Spectrometric, and
forthedeterminationofcarboninnucleargradesinteredmixed
Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
oxide (MOX) fuel pellets.The method for the determination of
ides ((U, Pu)O )
carbon presented in Test Method C698 consists of combusting
2
C753 Specification for Nuclear-Grade, Sinterable Uranium
carbon contained in MOX pellets with oxygen in a high-
Dioxide Powder
frequency induction furnace and detecting the resulting carbon
C757 Specification for Nuclear-Grade Plutonium Dioxide
dioxide using a thermal conductivity cell. The method for the
Powder for Light Water Reactors
determination of carbon presented in this test method consists
C833 Specification for Sintered (Uranium-Plutonium) Diox-
of combusting carbon contained in MOX pellets with oxygen
inahigh-frequencyinductionfurnaceandsubsequentdetection ide Pellets for Light Water Reactors
C859 Terminology Relating to Nuclear Materials
of the resulting carbon dioxide (CO ) using a non-dispersive
2
infrared detector (NDIR). Sulfur oxide is stripped from the C1068 Guide for Qualification of Measurement Methods by
a Laboratory Within the Nuclear Industry
carrier gas stream by a cellulose filter prior to the detection of
CO . C1408 Test Method for Carbon (Total) in Uranium Oxide
2
Powders and Pellets By Direct Combustion-Infrared De-
1.2 The values stated in SI units are to be regarded as
tection Method
standard. No other units of measurement are included in this
3
2.2 ISO Standards:
standard.
ISO 21614 Nuclear Fuel Technology – Determination of
1.3 This standard may involve hazardous material,
Carbon Content of UO , (U,Gd)O and (U, Pu)O Pow-
2 2 2
operations, and equipment. This standard does not purport to
ders and Sintered Pellets – Combustion in a High-
address all of the safety concerns, if any, associated with its
Frequency Induction Furnace – InfraredAbsorption Spec-
use. It is the responsibility of the user of this standard to
trometry
consult and establish appropriate safety and health practices
3. Terminology
and determine the applicability of regulatory limitations prior
to use.
3.1 For definitions of terms used in this test method but not
1.4 This international standard was developed in accor-
defined herein, refer to terminology relating to nuclear mate-
dance with internationally recognized principles on standard-
rials in Terminology C859.
ization established in the Decision on Principles for the
3.2 Definitions of Terms Specific to This Standard:
Development of International Standards, Guides and Recom-
3.2.1 MOX—nuclearfuelcomposedofamixtureofuranium
mendations issued by the World Trade Organization Technical
and plutonium oxides ((U, Pu)O ).
2
Barriers to Trade (TBT) Committee.
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
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear Standards volume information, refer to the standard’s Document Summary page on
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of the ASTM website.
3
Test. Available from International Organization for Standardization (ISO), ISO
Current edition approved June 1, 2017. Published June 2017. DOI: 10.1520/ Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
C1853-17. Geneva, Switzerland, http://www.iso.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1853 − 17
3.2.2 sintering—the process of forming a solid mass of increases. At carbon contents close to the typical carbon
material by heat or pressure, or both, without melting it to the content specification limit (100 µg carbon/gU+Pu metal) the
point of liquefaction. method uncertainty is on the order of 5 %, but exact method
performance is difficult to determine due to the lack of matrix
3.2.3 reference m
...

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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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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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1.1 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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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.  
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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.  
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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.  
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ASTM
ASTM C1108-23(Test Method)
Standard Test Method for Plutonium by Controlled-Potential Coulometry

SIGNIFICANCE AND USE
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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