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ASTM C759-98

(Test Method)

Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions

Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions

SCOPE
1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:  Sections Plutonium by Controlled-Potential Coulometry 2 Plutonium by Amperometric Titration with Iron (II) 2 Free Acid by Titration in an Oxalate Solution 16 to 23 Free Acid by Iodate Precipitation- Potentiometric Titration Test Method 24 to 30 Uranium by Arsenazo I Spectrophotometric Test Method 31 to 41 Thorium by Thorin Spectrophotometric Test Method 42 to 50 Iron by 1,10-Phenanthroline Spectrophotometric Test Method 51 to 58 Chloride by Thiocyanate Spectrophotometric Test Method 59 to 66 Fluoride by Distillation-Spectrophotometric Test Method 67 to 74 Sulfate by Barium Sulfate Turbidimetric Test Method 75 to 82 Isotopic Composition by Mass Spectrometry 83 to 84 Americium-241 by Extraction and Gamma Counting 85 to 93 Americium-241 by Gamma Counting 94 to 102 Gamma-Emitting Fission Products, Uranium, and Thorium by Gamma-Ray Spectroscopy 103 to 110 Rare Earths by Copper Spark Spectrochemical Test Method 111 to 113 Tungsten, Niobium (Columbium), and Tantalum by Spectro-chemical Test Method 114 to 122 Sample Preparation for Spectrographic Analysis for General Impurities 123 to 126
1.3 This standard does not purport to address all of the safety problems, 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 safeguard and safety hazard statements, see Section 5.

General Information

Status
Historical
Publication Date
09-Feb-1998
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

Replaced By
ASTM C759-04 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions
Effective Date
01-Jan-2004
Referred By
ASTM C1307-21 - Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry
Effective Date
10-Feb-1998
Referred By
ASTM C758-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Metal
Effective Date
10-Feb-1998
Referred By
ASTM C1432-15 - Standard Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
Effective Date
10-Feb-1998
Referred By
ASTM C1268-15 - Standard Test Method for Quantitative Determination of <sup>241</sup>Am in Plutonium by Gamma-Ray Spectrometry
Effective Date
10-Feb-1998
Referred By
ASTM C1637-21 - Standard Test Method for Determination of Impurities in Plutonium Materials—Acid Digestion and Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS) Analysis
Effective Date
10-Feb-1998

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ASTM C759-98 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate SolutionsASTM C759-98 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions
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ASTM C759-98 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions
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Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: C 759 – 98
Standard Test Methods for
Chemical, Mass Spectrometric, Spectrochemical, Nuclear,
and Radiochemical Analysis of Nuclear-Grade Plutonium
1
Nitrate Solutions
This standard is issued under the fixed designation C 759; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope C 697 Test Methods for Chemical, Mass Spectrometric, and
Spectrochemical Analysis of Nuclear-Grade Plutonium
1.1 These test methods cover procedures for the chemical,
2
Dioxide Powders and Pellets
mass spectrometric, spectrochemical, nuclear, and radiochemi-
C 852 Guide for Design Criteria for Plutonium Glove-
cal analysis of nuclear-grade plutonium nitrate solutions to
3
boxes
determine compliance with specifications.
C 1009 Guide for Establishing a Quality Assurance Pro-
1.2 The analytical procedures appear in the following order:
gram for Analytical Chemistry Laboratories Within the
Sections
3
Nuclear Industry
2
Plutonium by Controlled-Potential Coulometry
C 1068 Guide for Qualification of Measurement Methods
2
Plutonium by Amperometric Titration with Iron(II)
3
by a Laboratory Within the Nuclear Industry
Plutonium by Diode Array Spectrophotometry 4
V 1108 Test Method for Plutonium by Controlled-Potential
Free Acid by Titration in an Oxalate Solution 8 to 15
3
Free Acid by Iodate Precipitation-Potentiometric Titration 16 to 22
Coulometry
Test Method
C 1128 Guide for Preparation of Working Reference Mate-
Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33
rials for Use in the Analysis of Nuclear Fuel Cycle
Thorium by Thorin Spectrophotometric Test Method 34 to 42
3
Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50
Materials
Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58
C 1156 Guide for Establishing Calibration for a Measure-
Fluoride by Distillation-Spectrophotometric Test Method 59 to 66
Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74 ment Method Used to Analyze Nuclear Fuel Cycle Mate-
3
Isotopic Composition by Mass Spectrometry 75 to 76
rials
Americium-241 by Extraction and Gamma Counting 77 to 85
C 1165 Test Method for Determining Plutonium by Con-
Americium-241 by Gamma Counting 86 to 94
Gamma-Emitting Fission Products, Uranium, and Thorium by 94 to 102 trolled Potential Coulometry in H SO at a Platinum
2 4
3
Gamma-Ray Spectroscopy
Working Electrode
Rare Earths by Copper Spark Spectrochemical Test Method 103 to 105
C 1206 Test Method for Plutonium by Iron (II)/Chromium
Tungsten, Niobium (Columbium), and Tantalum by Spectro 106 to 114
3
chemical Test Method (VI) Amperometric Titration
Sample Preparation for Spectrographic Analysis for General 123 to 126
C 1210 Guide for Establishing a Measurement System
Impurities
Quality Control Program for Analytical Chemistry Labo-
3
1.3 This standard does not purport to address all of the
ratories Within the Nuclear Industry
safety concerns, if any, associated with its use. It is the
C 1268 Test Method for Quantitative Determination of
responsibility of the user of this standard to establish appro-
Americium 241 in Plutonium by Gamma-Ray Spectrom-
3
priate safety and health practices and determine the applica-
etry
bility of regulatory limitations prior to use. For specific
C 1297 Guide for Qualification of Laboratory Analysts for
3
safeguard and safety hazard statements, see Section 6.
the Analysis of Nuclear Fuel Cycle Materials
C 1307 Test Method for Plutonium Assay by Plutonium(III)
2. Referenced Documents
3
Diode Array Spectrophotometry
4
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
E 50 Practices for Apparatus, Reagents, and Safety Precau-
5
tions for Chemical Analysis of Metals
1
These test methods are under the jurisdiction of ASTM Committee C-26 on
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
Methods of Test.
3
Current edition approved Feb. 10, 1998. Published May 1998. Originally Annual Book of ASTM Standards, Vol 12.01.
4
pub-lished as C 759 – 73. Last previous edition C 759 – 92. Annual Book of ASTM Standards, Vol 11.01.
2 5
Discontinued as of November 15, 1992. Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 759
E 115 Practice for Photographic Processing in Optical 6. Safety Hazards
5
Emission Spectrographic An
...

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ASTM C1268-23(Test Method)
Standard Test Method for Quantitative Determination of 241Am in Plutonium by Gamma-Ray Spectrometry

SIGNIFICANCE AND USE
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.  
5.2 The 241Am in solid plutonium materials may be determined when these materials are dissolved (see Practice C1168).  
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).  
5.4 This test method is less subject to interferences from plutonium than alpha counting since the energy of the gamma ray used for the analysis is better resolved from other gamma rays than the alpha particle energies used for alpha counting.  
5.5 The minimal sample preparation reduces the amount of sample handling and exposure to the analyst.  
5.6 This test method is applicable only to homogeneous solutions. This test method is not suitable for solutions containing solids.  
5.7 Solutions containing 241Am at concentrations as little as 1 × 10−5 g/L may be analyzed using this method. The lower limit depends on the detector used and the counting geometry. Solutions containing high concentrations may be analyzed following an appropriate dilution.
SCOPE
1.1 This test method covers the quantitative determination of 241Am by gamma-ray spectrometry in plutonium nitrate solution samples that do not contain significant amounts of radioactive fission products or other high specific activity gamma-ray emitters.  
1.2 This test method can be used to determine the 241Am in samples of plutonium metal, oxide and other solid forms, when the solid is appropriately sampled and dissolved.  
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.  
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 C1168-23(Practice)
Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis

SIGNIFICANCE AND USE
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.
SCOPE
1.1 This practice is a compilation of dissolution techniques for plutonium materials that are applicable to the test methods used for characterizing these materials. Dissolution treatments for the major plutonium materials assayed for plutonium or analyzed for other components are listed. Aliquots of the dissolved materials are dispensed on a mass basis when one of the analyses must be of high precision, such as plutonium assay; otherwise they are dispensed on a volume basis.  
1.2 Procedures in this practice are intended for the dissolution of plutonium metal, plutonium oxide, and uranium-plutonium mixed oxides. Aliquots of dissolved materials are analyzed using test methods, such as those developed by Subcommittee C26.05 on Methods of Test, to demonstrate compliance with applicable requirements. These may include product specifications such as Specifications C757 and C833.  
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.  
1.6 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 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).  
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 %).  
1.3 There is no discussion of or provision for preventing criticality incidents, nor are health and safety requirements, the avoidance of hazards, or shipping precautions and controls discussed. Observance of this specification does not relieve the user of the obligation to be aware of and conform to all applicable international, federal, state, and local regulations pertaining to possessing, processing, shipping, or using source or special nuclear material. Examples of U.S. government documents are Code of Federal Regulations Title 10, Part 50—Domestic Licensing of Production and Utilization Facilities; Code of Federal Regulations Title 10, Part 71—Packaging and Transportation of Radioactive Material; and Code of Federal Regulations Title 49, Part 173—General Requirements for Shipments and Packaging.  
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5.1 Uranium hexafluoride is a basic material used to produce nuclear reactor fuel. To be suitable for this purpose, the material must meet criteria for isotopic composition. This test method is designed to determine whether the material meets the requirements described in Specifications C787 and C996.
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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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ASTM C859-23(Terminology)
Standard Terminology Relating to Nuclear Materials

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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.  
1.2 While subcommittees within Committee C26 are free to only provide terms and definitions within individual standards, each subcommittee may request the addition of utilized terms and definitions to this terminology standard if it believes that such serves the broader interest of Committee C26 and the nuclear fuel cycle profession. Therefore, terms and definitions proposed for inclusion in Terminology C859 need not be used in more than one committee standard before being considered.  
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1.4 Subcommittee C26.10 (Nondestructive Assay) also has a terminology standard applicable to its standards: Terminology C1673.  
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ASTM C1554-18(2023)(Guide)
Standard Guide for Materials Handling Equipment for Hot Cells

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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.  
4.2 This guide is intended as a supplement to other standards (Section 2, Referenced Documents), and to federal and state regulations, codes, and criteria applicable to the design of equipment intended for this use.  
4.3 This guide is intended to be generic and to apply to a wide range of types and configurations of materials handling equipment.  
4.4 The term materials handling equipment is used herein in a generic sense. It includes manipulators, cranes, carts or bogies, and special equipment for handling tools and material in hot cells.  
4.5 This service imposes stringent requirements on the quality and the integrity of the equipment, as follows:  
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.  
4.5.4 Attention to fabrication tolerances is necessary to allow the proper fit-up between components for the proper installation and mounting of materials handling equipment in hot cells, for example, when parts or components are being replaced. Fabrication tolerances should be controlled to provide sufficie...
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.  
1.1.4 This guide covers mechanical master-slave manipulators and electro-mechanical manipulators, but does not cover electro-hydraulic manipulators.  
1.2 Applicability:  
1.2.1 This guide is intended to be applicable to equipment used under one or more of the following conditions:
1.2.1.1 The materials handled or processed constitute a significant radiation hazard to man or to the environment.
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.
1.2.1.3 The equipment can neither be accessed directly for purposes of operation or maintenance, nor can the equipment be viewed directly, for example, without shielded viewing windows, periscopes, or a video monitoring system.  
1.3 User Caveats:  
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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 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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