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ASTM C1022-02

(Test Method)

Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate

Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate

SCOPE
1.1 These test methods cover procedures for the chemical and atomic absorption analysis of uranium-ore concentrates to determine compliance with the requirements prescribed in Specification C 967.
1.2 The analytical procedures appear in the following order:SectionsUranium by Ferrous Sulfate Reduction-Potassium Dichromate Titrimetry9Nitric Acid-Insoluble Uranium10 to 18Extractable Organic Material19 to 26Arsenic by Diethyldithiocarbamate (Photometric Method)27 to 36Carbonate by CO2 Gravimetry37 to 43Fluoride by Ion-Selective Electrode44 to 51Halides by Volhard Titration52 to 59Moisture by Loss of Weight at 110°C60 to 66Phosphorus by Spectrophotometry67 to 75Silicon by Gravimetry76 to 82Thorium by the Thorin (Photometric) Method83 to 91Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-dium by Atomic Absorption Spectrophotometry92 to 101Potassium and Sodium by Atomic Absorption Spectrophotometry102 to 111Boron by Spectrophotometry112 to 121
1.3 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. Specific precautionary statements are given in Sections 7, 32, and Note 14.

General Information

Status
Historical
Publication Date
09-Jan-2002
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 C1022-93 - Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
Effective Date
10-Jan-2002
Replaced By
ASTM C1022-05 - Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
Effective Date
01-Jan-2005
Referred By
ASTM C1843-16(2022) - Standard Test Method for Determining Moisture Content in Uranium-Ore Concentrate
Effective Date
10-Jan-2002
Referred By
ASTM C967-20 - Standard Specification for Uranium Ore Concentrate
Effective Date
10-Jan-2002
Referred By
ASTM C1075-17(2022) - Standard Practices for Sampling Uranium-Ore Concentrate
Effective Date
10-Jan-2002
Referred By
ASTM C1295-15 - Standard Test Method for Gamma Energy Emission from Fission and Decay Products in Uranium Hexafluoride and Uranyl Nitrate Solution
Effective Date
10-Jan-2002

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ASTM C1022-02 - Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore ConcentrateASTM C1022-02 - Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
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ASTM C1022-02 - Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
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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:C1022–02
Standard Test Methods for
Chemical and Atomic Absorption Analysis of Uranium-Ore
1
Concentrate
This standard is issued under the fixed designation C 1022; 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.
2
1. Scope C 967 Specification for Uranium Ore Concentrate
C 1254 Test Method for Uranium in Mineral Acids by
1.1 These test methods cover procedures for the chemical
X-Ray Fluoresence
and atomic absorption analysis of uranium-ore concentrates to
C 1267 Test Method for Uranium by Iron (II) Reduction in
determine compliance with the requirements prescribed in
PhosphoricAcidFolloweedbyChromium(IV)Titrationin
Specification C 967.
2
the Presence of Vanadium
1.2 The analytical procedures appear in the following order:
C 1347 Practice for Preparation and Dissolution of Uranum
Sections
2
Materials for Analysis
Uranium by Ferrous Sulfate Reduction—Potassium Dichromate
3
Titrimetry 9 D 1193 Specification for Reagent Water
Nitric Acid-Insoluble Uranium 10 to 18
E 60 Practice for Photometric and Spectrophotometric
Extractable Organic Material 19 to 26
4
Methods for Chemical Analysis of Metals
Arsenic by Diethyldithiocarbamate (Photometric Method) 27 to 36
Carbonate by CO Gravimetry 37 to 43
2
3. Terminology
Fluoride by Ion-Selective Electrode 44 to 51
Halides by Volhard Titration 52 to 59
3.1 Definitions—For definitions of terms used in these test
Moisture by Loss of Weight at 110°C 60 to 66
methods, refer to Terminology C 859.
Phosphorus by Spectrophotometry 67 to 75
Silicon by Gravimetry 76 to 82
Thorium by the Thorin (Photometric) Method 83 to 91
4. Significance and Use
Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-
4.1 The test methods in this standard are designed to show
dium by Atomic Absorption Spectrophotometry 92 to 101
Potassium and Sodium by Atomic Absorption
whether a given material meets the specifications prescribed in
Spectrophotometry 102 to 111
Specification C 967.
Boron by Spectrophotometry 112 to 121
4.2 Because of the variability of matrices of uranium-ore
1.3 This standard does not purport to address all of the
concentrate and the lack of suitable reference or calibration
safety concerns, if any, associated with its use. It is the
materials, the precision and bias of these test methods should
responsibility of the user of this standard to establish appro-
be established by each individual laboratory that will use them.
priate safety and health practices and determine the applica-
The precision and bias statements given for each test method
bility of regulatory limitations prior to use. Specific precau-
are those reported by various laboratories and can be used as a
tionary statements are given in Sections 7, 32, and Note 14.
guideline.
4.3 Instrumental test methods such as X-ray fluorescence
2. Referenced Documents
andemissionspectroscopycanbeusedforthedeterminationof
2.1 ASTM Standards:
some impurities where such equipment is available.
C 761 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and Radiochemical Analysis of
5. Interferences
2
Uranium Hexafluoride
5.1 Interferences are identified in the individual test meth-
2
C 859 Terminology Relating to Nuclear Materials
ods.
5.2 Oreconcentratesareofaveryvariablenature;therefore,
all interferences are very difficult to predict. The individual
1
These test methods are under the jurisdiction of ASTM Committee C26 on
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
Methods of Test.
Current edition approved Jan. 10, 2002. Published April 2002. Originally
3
published as C 1022 – 84. Last previous edition C 1022 – 93. Annual Book of ASTM Standards, Vol 11.01.
2 4
Annual Book of ASTM Standards, Vol 12.01. 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 ----------------------
C1022
user should verify the applicability of each procedure for washed with 1 M nitric acid until the filtrate gives a negative
specific ore concentrates. test for uranium. The washed residue is then dried and ignited
at 1000 6 25°C for 1 h. The uranium content is determined on
6. Reagents
the ignited residue by spectrophotometry.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that 12. Interference
all reagents shall conform to the specifications of the Commit-
12.1 At the specification limit for nitric acid insoluble
tee onAnalytical Reagents of theAmerican Chemical Society,
uranium usually
...

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ASTM C1168-23(Practice)
Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis

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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.  
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.
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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  
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Section  
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2  
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16  
9  
Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder  
17  
10  
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Pellets  
18  
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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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Standard Specification for Sintered (Uranium-Plutonium) Dioxide Pellets for Light Water Reactors

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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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ASTM C1554-18(2023)(Guide)
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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 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.  
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1.1 Intent:  
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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.  
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1.3 User Caveats:  
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5.1 Uranium hexafluoride is normally produced and handled in large (typically 1 to 14-ton) quantities and must, therefore, be characterized by reference to representative samples (see ISO 7195). The samples are used to determine compliance with the applicable commercial specification C787. The quantities involved, physical properties, chemical reactivity, and hazardous nature of UF6 are such that for representative sampling, specially designed equipment must be used and operated in accordance with the most carefully controlled and stringent procedures. This practice can be used by UF6 converters to review the effectiveness of existing procedures or as a guide to the design of equipment and procedures for future use.  
5.2 The intention of this practice is to avoid liquid UF6 sampling once the cylinder has been filled. For safety reasons, manipulation of large quantities of liquid UF6 should be avoided when possible.  
5.3 It is emphasized that this practice is not meant to address conventional or nuclear criticality safety issues.
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1.3 If the receiving cylinder is purged after filling and sampling, special verifications must be performed by the user to verify the representativity of the sample(s). It is then expected that the results found on volatile impurities with gas phase sampling may be conservative.  
1.4 This practice is only applicable when the transfer occurs in the gas phase. When the transfer is performed in the liquid phase, Practice C1052 should apply. This practice does not apply to gas sampling after the cylinder has been filled since the sample taken will not be representative of the cylinder.  
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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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ASTM
ASTM C1165-23(Test Method)
Standard Test Method for Determining Plutonium by Controlled-Potential Coulometry in H2SO4 at a Platinum Working Electrode

SIGNIFICANCE AND USE
5.1 This test method is used to ascertain whether or not materials meet specifications for plutonium concentration or plutonium mass fraction.  
5.1.1 The materials (nuclear grade plutonium nitrate solutions, plutonium metal, plutonium oxide powder, and mixed oxide and carbide powders and pellets) to which this test method applies are subject to nuclear safeguards regulations governing their possession and use. However, adherence to this test method does not automatically guarantee regulatory acceptance of the resulting safeguards measurements. It remains the sole responsibility of the user of this test method to ensure that its application to safeguards has the approval of the proper regulatory authorities.  
5.1.2 When used in conjunction with appropriate certified reference materials (CRMs), this test method can demonstrate traceability to the international measurements system (SI).  
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.  
5.3 A chemical calibration of the coulometer is necessary for accurate results.
FIG. 1 Example of a Cell Design Used at Los Alamos National Laboratory (LANL)
SCOPE
1.1 This test method covers the determination of milligram quantities of plutonium in unirradiated uranium-plutonium mixed oxide having a U/Pu ratio range of 0.1 to 10. This test method is also applicable to plutonium metal, plutonium oxide, uranium-plutonium mixed carbide, various plutonium compounds including fluoride and chloride salts, and plutonium solutions.  
1.2 The recommended amount of plutonium for each aliquant in the coulometric analysis is 5 mg to 10 mg. Precision worsens for lower amounts of plutonium, and elapsed time of electrolysis becomes impractical for higher amounts of plutonium.  
1.3 The quantity values stated in SI units are to be regarded as standard. The quantity values with non-SI units are given in parentheses 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. Specific precautionary statements are given in Section 9.  
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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    6 pages
    English language
    sale 15% off