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ASTM C968-06

(Test Method)

Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide Pellets

Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide Pellets

SIGNIFICANCE AND USE
The test methods in this method are designed to show whether a given material is in accordance with Specification C922.
SCOPE
1.1 These test methods cover procedures for the analysis of sintered gadolinium oxide-uranium dioxide pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order: Section Carbon (Total) by Direct CombustionThermal Conductivity Method  C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method  Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method  C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide  Gadolinia Content by Energy-Dispersive X-Ray Spectrometry  C1456 Test Method for Determination of Uranium or Gadolinium, or Both, in Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray Fluorescence (XRF)  Hydrogen by Inert Gas Fusion  C1457 Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction  Isotopic Uranium Composition by Multiple-Filament Surface-Ionization Mass Spectrometric Method  C1413 Test Method for Isotopic Analysis of Hydrolysed Uranium Hexafluoride And Uranyl Nitrate Solutions By Thermal Ionization Mass Spectrometry  C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis  Nitrogen by DistillationNessler Reagent (Photometric) Method6 to 16 Oxygen-to-Metal Ratio of Sintered Gadolinium Oxide-Uranium Dioxide Pellets  C1430 Test Method for Determination of Uranium, Oxygen to Uranium, and Oxygen to Metal (O/M) in Sintered Uranium Dioxide and Gadolinia-Uranium Dioxide Pellets by Atmospheric Equilibration  Spectrochemical Determination of Trace Impurity Elements  C1517 Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission Spectroscopy  Total Gas by Hot Vacuum Extraction  Ceramographic Determination of Free Gd2O3 and Free UO2 to Estimate the Homogeneity of (U,Gd)O2 Pellets17 to 24
1.3 The values stated in SI units are to be regarded as the 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 and health practices and determine the applicability of regulatory limitations prior to use.  
6.1 This test method describes the determination of nitrogen in gadolinium oxide-uranium dioxide pellets (Gd2O3/UO2). With a 2 to 5-g sample, concentrations from 5 to 100 μg of nitrogen are determined without interference.  
17.1 The homogeneity of Gd2O3 in UO2 has been cited in Specification C922 as an important requirement for this fuel form. The uniform distribution of gadolinia in urania will result in up to three components in the pellet: free Gd2O3, free UO2, and a Gd2O3-UO2 solid solution. There are a number of ways for assessing uniformity of which the ceramographic method described here may not be the most definitive. This technique has been used over the gadolinia concentration range from 1 to 10 weight %.

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 C968-99 - Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide Pellets
Effective Date
01-Jul-2006
Replaced By
ASTM C968-12 - Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide Pellets
Effective Date
01-Jan-2012
Referred By
ASTM C1430-18 - Standard Test Method for Determination of Uranium, Oxygen to Uranium (O/U), and Oxygen to Metal (O/M) in Sintered Uranium Dioxide and Gadolinia-Uranium Dioxide Pellets by Atmospheric Equilibration
Effective Date
01-Jul-2006
Referred By
ASTM C922-21 - Standard Specification for Sintered Gadolinium Oxide-Uranium Dioxide Pellets for Light Water Reactors
Effective Date
01-Jul-2006

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ASTM C968-06 - Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide PelletsASTM C968-06 - Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide Pellets
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ASTM C968-06 - Standard Test Methods for Analysis of Sintered Gadolinium Oxide-Uranium Dioxide Pellets
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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:C968–06
Standard Test Methods for
Analysis of Sintered Gadolinium Oxide-Uranium Dioxide
1
Pellets
This standard is issued under the fixed designation C968; 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 1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods cover procedures for the analysis of
responsibility of the user of this standard to establish appro-
sintered gadolinium oxide-uranium dioxide pellets to deter-
priate safety and health practices and determine the applica-
mine compliance with specifications.
bility of regulatory limitations prior to use.
1.2 The analytical procedures appear in the following order:
Section
2. Referenced Documents
2
Carbon (Total) by Direct Combustion—Thermal Conductivity Method
3 3
C1408 Test Method for Carbon (Total) in Uranium Oxide Powders
2.1 ASTM Standards:
and Pellets By Direct Combustion-Infrared Detection Method
C922 Specification for Sintered Gadolinium Oxide-
4
Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode
Uranium Dioxide Pellets
Method
3
C1502 Test Method for Determination of Total Chlorine and Fluorine
C1347 Practice for Preparation and Dissolution of Uranium
in Uranium Dioxide and Gadolinium Oxide
Materials for Analysis
4
Gadolinia Content by Energy-Dispersive X-Ray Spectrometry
3
C1408 Test Method for Carbon (Total) in Uranium Oxide
C1456 Test Method for Determination of Uranium or Gadolinium, or
Both, in Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray
Powders and Pellets By Direct Combustion-Infrared De-
Fluorescence (XRF)
tection Method
4
Hydrogen by Inert Gas Fusion
3
C1457 Test Method for Determination of Total Hydrogen Content of C1413 Test Method for Isotopic Analysis of Hydrolyzed
Uranium Oxide Powders and Pellets by Carrier Gas Extraction
Uranium Hexafluoride and Uranyl Nitrate Solutions by
2
Isotopic Uranium Composition by Multiple-Filament Surface-
Thermal Ionization Mass Spectrometry
Ionization Mass Spectrometric Method
3
C1413 Test Method for Isotopic Analysis of Hydrolysed Uranium C1430 Test Method for Determination of Uranium, Oxygen
Hexafluoride And Uranyl Nitrate Solutions By Thermal Ionization
to Uranium (O/U), and Oxygen to Metal (O/M) in Sintered
Mass Spectrometry
3 Uranium Dioxide and Gadolinia-Uranium Dioxide Pellets
C1347 Practice for Preparation and Dissolution of Uranium Materials
for Analysis by Atmospheric Equilibration
Nitrogen by Distillation—Nessler Reagent (Photometric) Method 6 to 16
C1456 TestMethodforDeterminationofUraniumorGado-
4
Oxygen-to-Metal Ratio of Sintered Gadolinium Oxide-Uranium Diox-
linium (or both) in Gadolinium Oxide-Uranium Oxide
ide Pellets
3
C1430 Test Method for Determination of Uranium, Oxygen to Ura-
Pellets or by X-Ray Fluorescence (XRF)
nium, and Oxygen to Metal (O/M) in Sintered Uranium Dioxide
C1457 Test Method for Determination of Total Hydrogen
and Gadolinia-Uranium Dioxide Pellets by Atmospheric Equilibra-
Content of Uranium Oxide Powders and Pellets by Carrier
tion
4
Spectrochemical Determination of Trace Impurity Elements
Gas Extraction
3
C1517 Test Method for Determination of Metallic Impurities in Ura-
C1502 Test Method for Determination of Total Chlorine
nium Metal or Compounds by DC-Arc Emission Spectroscopy
2
and Fluorine in Uranium Dioxide and Gadolinium Oxide
Total Gas by Hot Vacuum Extraction
Ceramographic Determination of Free Gd O and Free UO to Esti- 17 to 24
2 3 2 C1517 Test Method for Determination of Metallic Impuri-
mate the Homogeneity of (U,Gd)O Pellets
2
tiesinUraniumMetalorCompoundsbyDC-ArcEmission
1.3 The values stated in SI units are to be regarded as the Spectroscopy
standard. D1193 Specification for Reagent Water
1
These test methods are under the jurisdiction of ASTM C26 on Nuclear Fuel
3
Cycle and are the direct responsibility of C26.05 on Methods of Test. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2006. Published August 2006. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1981. Last previous edition approved in 1999 as C968 – 99. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C0968-06. the ASTM website.
2 4
Discontinued 1999. See C968 – 94. Discontinued 2005. See C968 – 99.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C968–06
E146 Methods of Chemical Analy
...

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10  
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18  
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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.  
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1.1 Intent:  
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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 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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