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ASTM C889-06

(Test Method)

Standard Test Methods for Chemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd2O3) Powder

Standard Test Methods for Chemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd<sub>2</sub>O<sub>3</sub>) Powder

SIGNIFICANCE AND USE
Gadolinium oxide powder is used, with subsequent processing, in nuclear fuel applications, such as an addition to uranium dioxide. These test methods are designed to determine whether the material meets the requirements described in Specification C 888.
3.1.1 The material is analyzed to determine whether it contains the minimum gadolinium oxide content specified.
3.1.2 The loss on ignition and impurity content are determined to ensure that the weight loss and the maximum concentration limit of specified impurity elements are not exceeded.
SCOPE
1.1 These test methods cover procedures for the chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide powders to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
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. For specific hazard statements, see Section .
1.3 This test method covers the loss-on-ignition of volatile constituents from nuclear-grade gadolinium oxide (Gd2O 3) powder.
1.4 The percent gadolinium oxide content of powders, exclusive of volatiles, is determined by calculation after the material has been analyzed to determine the total impurities.

General Information

Status
Historical
Publication Date
31-Dec-2005
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 C889-99 - Standard Test Methods for Chemical and Mass Spectrographic Analysis of Nuclear-Grade Gadolinium Oxide (Gd<sub>2</sub>O<sub>3</sub>) Powder
Effective Date
01-Jan-2006
Replaced By
ASTM C889-11 - Standard Test Methods for Chemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd<sub>2</sub>O<sub>3</sub>) Powder
Effective Date
01-Jun-2011
Referred By
ASTM C888-18 - Standard Specification for Nuclear-Grade Gadolinium Oxide (Gd<inf>2</inf>O<inf>3</inf >) Powder
Effective Date
01-Jan-2006
Referred By
ASTM F2168-13(2019) - Standard Specification for Packing Material, Graphitic, Corrugated Ribbon or Textured Tape, and Die-Formed Ring
Effective Date
01-Jan-2006
Referred By
ASTM F2191/F2191M-13(2020)e1 - Standard Specification for Packing Material, Graphitic or Carbon Braided Yarn
Effective Date
01-Jan-2006

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ASTM C889-06 - Standard Test Methods for Chemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd<sub>2</sub>O<sub>3</sub>) PowderASTM C889-06 - Standard Test Methods for Chemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd<sub>2</sub>O<sub>3</sub>) Powder
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ASTM C889-06 - Standard Test Methods for Chemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd<sub>2</sub>O<sub>3</sub>) Powder
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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:C889–06
Standard Test Methods for
Chemical and Mass Spectrometric Analysis of Nuclear-
1
Grade Gadolinium Oxide (Gd O ) Powder
2 3
This standard is issued under the fixed designation C889; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope Spectrochemical, Nuclear, and Radiochemical Analysis of
Uranium Hexafluoride
1.1 These test methods cover procedures for the chemical
C888 Specification for Nuclear-Grade Gadolinium Oxide
and mass spectrometric analysis of nuclear-grade gadolinium
(Gd O ) Powder
oxide powders to determine compliance with specifications. 2 3
C1287 Test Method for Determination of Impurities in
1.2 The analytical procedures appear in the following order:
Nuclear Grade Uranium Compounds by Inductively
Sections
2
Coupled Plasma Mass Spectrometry
Carbon by Direct Combustion—Thermal Conductivity
3
C1408 Test Method for Carbon (Total) in Uranium Oxide
C1408 Test Method for Carbon (Total) in Uranium Oxide
Powders and Pel lets By Direct Combustion-Infrared Detec-
Powders and Pellets By Direct Combustion-Infrared De-
tion Method
tection Method
Total Chlorine and Fluorine by Pyrohydrolysis Ion— -
Selective Electrode
C1502 Test Method for Determination of Total Chlorine
Loss of Weight on Ignition 7-13
and Fluorine in Uranium Dioxide and Gadolinium Oxide
2
Sulfur by Combustion—Iodometric Titration
2
Impurity Elements by a Spark-Source Mass Spectrographic D1193 Specification for Reagent Water
3
C761 Test Methods for Chemical, Mass Spectrometric, Spec-
trochemical,Nuclear, and Radiochemical Analysis of Uranium
3. Significance and Use
Hexafluoride
3
C1287 Test Method for Determination of Impurities In Ura- 3.1 Gadolinium oxide powder is used, with subsequent
nium Dioxide By Inductively Coupled Plasma Mass Spec-
processing, in nuclear fuel applications, such as an addition to
trometry
uranium dioxide.These test methods are designed to determine
Gadolinium Content in Gadolinium Oxide by Impurity 14-17
Correction whether the material meets the requirements described in
4
C1502 Test Method for Determination of Total Chlorine and
Specification C888.
Fluorine in Uranium Dioxide and Gadolinium Oxide
3.1.1 The material is analyzed to determine whether it
1.3 This standard does not purport to address all of the
contains the minimum gadolinium oxide content specified.
safety concerns, if any, associated with its use. It is the
3.1.2 The loss on ignition and impurity content are deter-
responsibility of the user of this standard to establish appro-
mined to ensure that the weight loss and the maximum
priate safety and health practices and determine the applica-
concentration limit of specified impurity elements are not
bility of regulatory limitations prior to use. For specific hazard
exceeded.
statements, see Section 5.
4. Reagents
2. Referenced Documents
4.1 Purity of Reagents—Reagent grade chemicals shall be
3
2.1 ASTM Standards:
used in all tests. Unless otherwise indicated, it is intended that
C761 Test Methods for Chemical, Mass Spectrometric,
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
5
where such specifications are available. Other grades may be
1
These test methods are under the jurisdiction of ASTM Committee C26 on
used, provided it is first ascertained that the reagent is of
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
sufficiently high purity to permit its use without lessening the
Methods of Test.
accuracy of the determination.
Current edition approved Jan. 1, 2006. Published February 2006. Originally
approved in 1978. Last previous edition approved in 1999 as C889 – 99. DOI:
10.1520/C0889-06.
2 5
Discontinued January 1999. See C889–90. Reagent Chemicals, American Chemical Society Specifications, American
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC. For suggestions on the testing of reagents not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM listed by the American Chemical Society, see Analar Standards for Laboratory
Standards volume information, refer to the standard’s Document Summary page on Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
the ASTM website. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
4
Discontinued March 2005. See C889–90. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
...

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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.  
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Section  
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9  
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17  
10  
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Pellets  
18  
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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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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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4.5.2 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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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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