1、Designation: C757 06 (Reapproved 2011)1C757 16Standard Specification forNuclear-Grade Plutonium Dioxide Powder, SinterablePowderfor Light Water Reactors1This standard is issued under the fixed designation C757; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1 NOTESection 4.6 was changed editorially in June 2011.INTRODUCTIONThis specification is i
3、ntended to provide the nuclear industry with a general standard for sinterableplutonium dioxide (PuO2) powder. It recognizes the diversity of manufacturing methods by whichplutoniumPuO2 dioxide powders are produced,produced and the many special requirements forchemical and physical characterization
4、that may be applicable for a particular Mixed Oxide (MOX,that is (U, Pu)O2) fuel pellet manufacturing process or imposed by the end useuser of the powder ina specific reactor system.different light water reactors. It is, therefore, anticipated that the buyer maysupplement this specification with mor
5、e stringent or additional requirements for specific applications.1. Scope1.1 This specification covers nuclear grade plutoniumPuO2 dioxide, sinterable powder obtained by the oxalate precipitationroute, calcined above 500C, or any other equivalent process acceptable to thepowder. It applies to PuO2 b
6、uyer. Included isplutonium dioxide of various isotopic compositions as normally prepared by in-reactor neutron irradiation of natural or slightlyenriched uranium or by in-reactor neutron irradiation of recycled plutonium mixed with uranium.1.2 There is no discussion of or provision for preventing cr
7、iticality incidents, nor are health and safety requirements, theavoidance of hazards, or shipping precautions and controls discussed. Observance of this specification does not relieve the userof the obligation to be aware of and conform to all national applicable international, national, or federal,
8、 state, and local regulationson processing, shipping, pertaining to possessing, shipping, processing, or using source or special nuclear materials.material. Forexamples in the U.S. Government, relevant documents are Code of Federal Regulations, Title 10 Nuclear Safety Guide, U.S.Atomic Energy Commis
9、sion ReportTID-70162, and “Handbook of Nuclear Safety”, H. K. Clark, U.S.Atomic Energy CommissionReport, DP-5322.1.3 The PuO2 shall be produced by a qualified process and in accordance with a quality assurance program approved by the user.1.4 The values stated in SI units are to be regarded as the s
10、tandard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Refere
11、nced Documents2.1 ASTM Standards:3B243 Terminology of Powder MetallurgyC697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium DioxidePowders and Pellets1 This specification is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and
12、is the direct responsibility of Subcommittee C26.02 on Fuel and FertileMaterial Specifications.Current edition approved June 1, 2011April 1, 2016. Published July 2011April 2016. Originally approved in 1974. Last previous edition approved in 20062011 asC757 06.C757 06 (2011)1. DOI: 10.1520/C0757-06R1
13、1E01.10.1520/C0757-16.2 Available from Superintendent of Documents, U.S. Government Printing Office, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20402.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book o
14、f ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technical
15、ly possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C
16、700, West Conshohocken, PA 19428-2959. United States1C859 Terminology Relating to Nuclear MaterialsC1233 Practice for Determining Equivalent Boron Contents of Nuclear MaterialsC1274 Test Method for Advanced Ceramic Specific Surface Area by Physical AdsorptionC1295 Test Method for Gamma Energy Emissi
17、on from Fission and Decay Products in Uranium Hexafluoride and Uranyl NitrateSolutionC1770 Test Method for Determination of Loose and Tapped Bulk Density of Plutonium OxideE105 Practice for Probability Sampling of Materials2.2 ANSIASME Standard:ANSI/ASMEASME NQA-1 Quality Assurance Requirements for
18、Nuclear Facility Applications42.3 U.S. Government Documents:Code of Federal Regulations, Title 10, Nuclear Safety Guide, U.S. Atomic Energy Commission Report TID-70162“Handbook of Nuclear Safety,” Clark, H. K., U.S. Atomic Energy Commission Report, DP-53222.4 ISO Standard:ISO 8300 Determination of P
19、u Content in Plutonium Dioxide (PuO2) of Nuclear Grade Quality, Gravimetric Method4ISO 9161 Uranium Dioxide PowderDetermination of Apparent Density and Tap DensityISO 13463 Nuclear-grade Plutonium Dioxide Powder for Fabrication of Light Water Reactor MOX FuelGuidelines to Helpin the Definition of a
20、Product Specification3. Terminology3.1 DefinitionsDefinitions of terms are as given in Terminologies B243 and C859.4. Isotopic Content4.1 Concentrations and homogeneity ranges of the plutonium isotopes(Pu) shall be as specified by the buyer.4.2 The isotopic composition of the final product shall be
21、determined by mass spectrometry and a method to be agreed uponbetween the buyer and seller and shall be reported on a weight basis.Pu basis including the associated measurement uncertainties.The date of the determination will be indicated.5. Chemical Composition5.1 Plutonium ContentThe minimum Pu co
22、ntent shall be 86.0 weight % including measurement uncertainties as sampled onthe date of sampling and 87.5 weight % after heating 4 h to 950C.sampling.5.2 Uranium ContentThe uranium content of the plutoniumPuO2 dioxide shall be measured and reported on a plutoniumPubasis.5.3 Americium ContentThe am
23、ericium (Am) content shall be measured and reported on a plutoniumPu basis. The maximumacceptable americiumAm content shall be agreed upon between the buyer and the seller.5.4 The dates of analyses of U, Th and Am shall be recorded.5.5 Impurity ContentThe impurity content shall not exceed the indivi
24、dual element limit specified in Table 1. on a Pu basis.Total non-volatile oxide impurity content excluding Am shall not exceed 6000 g/g Pu. Some other elements such as those listedin Table 2 may also be of concern for the buyer and should be measured and reported if requested. If an element analysis
25、 is reportedas “less than” a given concentration, this “less than” value shall be used in the determination of total impurities. Impurity elementsmeasured and their associated limits may differ from what is listed in this specification as agreed upon between the buyer and seller.5.6 Moisture Content
26、The moisture content shall be measured and reported on a Pu basis. The maximum acceptable moisturecontent shall be agreed upon between the buyer and the seller.5.7 Equivalent Boron ContentFor thermal reactor use, the total equivalent boron content (EBC) shall not exceed 20.0 g/gon a plutonium weight
27、 basis. For the purpose of EBC calculation Eu, Dy, and Sm shall be included in addition to elements listedin Pu basis. Table 1. The method of performing the calculation shall be as indicated in Practice C1233. For fast reactor use, theabove limitation on EBC does not apply.5.8 Gamma ActivityThe gamm
28、a activity (Bq/g Pu) of the gamma emitting fission products whose isotopes have half lives of30 days or greater shall be measured. The gamma radiation from fission products shall be less than 105 MeVBq/g Pu.5.8.1 The list of nuclides and mean energies per disintegration found in Test Method C1295 ar
29、e to be used in the calculations.6. Physical Properties6.1 Cleanliness and WorkmanshipThe PuO2 powder shall be free of visible fragments of foreign matter.4 Available from American National Standards Institute, 11 W. 42nd St., 13th Floor, Society of Mechanical Engineers (ASME), ASME International He
30、adquarters, TwoPark Ave., New York, NY 10036.10016-5990, http:/www.asme.org.C757 1626.2 Particle SizePuO2 powder particle size limits and method of determination shall be agreed upon between the buyer andseller. As an example, in oxalic acid type precipitation processes, no particles should exist ab
31、ove 100 m and at least 95 % of theparticles are expected to be less than 50 m.6.3 Particle SizeTap DensityAll The measured tap density of the PuO2 powder shall be capable of passing a 100 m sieveandwill depend on the production process and measurement method. This measurement is often used in critic
32、ality calculations. Thetap density limit and method of determination (for example, Test Method C1770 95 % of the powder by weight shall be capableof passing a 44 m sieve.or ISO 9161) shall be agreed upon between the buyer and seller.TABLE 1 Impurity Elements and Maximum Concentration LimitsElementMa
33、ximum ConcentrationLimitof Uranium, g/gPuBoron 3Cadmium 3CarbonA 200Chlorine 300Chromium 200Fluorine 200Iron 300Gadolinium 3Nickel 100Nitride Nitrogen 200Thorium 200TABLE 1 Impurity Elements and Maximum Concentration LimitsElementCMaximum ConcentrationLimitof Plutonium, g/gPuAluminum (Al) 300Boron (
34、B) 3Cadmium (Cd) 3Carbon (C)A 500Chlorine (Cl) 300Chromium (Cr) 200Dysprosium (Dy) 0.5Europium (Eu) 0.5Fluorine (F) 200Iron (Fe) 500Gadolinium (Gd) 3Magnesium (Mg) 200Molybdenum (Mo) 100Nickel (Ni) 200Nitrogen (N) 300Samarium (Sm) 2Silicon (Si) 200Sodium (Na) 100Titanium (Ti) 100Thorium (Th)B 50Tung
35、sten (W) 100Zinc (Zn) 100A Sample may be heated prior to carbon analysis.BThorium is primarily of concern because of the reactor production of 233U.CAny additional potential impurities, added by the fabrication process for example,beyond those listed here shall be evaluated (for example, in terms of
36、 equivalentboron), and associated limits established and agreed upon between the buyer andseller.TABLE 2 Additional Impurity ElementsElementBeryllium (Be) Niobium (Nb)Bismuth (Bi) Phosphorous (P)Calcium (Ca) Potassium (K)Cobalt (Co) Silver (Ag)Copper (Cu) Sulfur (S)Indium (In) Tantalum (Ta)Lead (Pb)
37、 Tin (Sn)Lithium (Li) Vanadium (V)Manganese (Mn) Zirconium (Zr)Neptunium (Np)C757 1636.4 Specific SurfaceAreaThe specific surface area shall not be less than 5 mlimits and method of determination shall be agreedupon between the2/g and not greater than 30 buyer and seller.As an example, in oxalic aci
38、d type precipitation processes the specificsurface area of the purified PuO2 powder is expected to be between 2 m2/g based on a Brunauer, Emmett, Teller (BET) adsorptionmethod. Seethe Brunauer-Emmet-Teller, or BET, adsorption method (for Notes 1 and 2.example, in accordance with GuideC1274).NOTE 1A
39、Requirements relative to the physical properties of the PuO2 will depend on the particular MOX fuel pellet fabrication process employed.For example, the unique physical properties of all of the PuO2specific surface area as low as 2 m (for example, particle size, tap density, specific surfacearea, et
40、c.) entering into the MOX fuel pellet manufacturing process are essentially erased when the powder is milled in the case where this is a fuelmanufacturing step. Nevertheless, even when no pass-fail criteria on physical property measurements is applicable, typical measurement values can beprovided as
41、 an expected target and2/g has been demonstrated to be acceptable when subsequently blended with other powder(s) of greater specific surfacearea.Therefore, powder with measurements can be provided for information in order to detect process drift, for example. Consistency between as-receivedPuO2 a sp
42、ecific surface area as batches, reflecting a stable and controlled PuO2 low as 2 mpowder manufacturing process, is2/g may be acceptable ifagreed upon between the supplier and the user. desirable to minimize any potential impact on the MOX fuel pellet manufacturing process.NOTE 2Consideration For fue
43、l pellet manufacturing processes that involve blending of different powders, consideration should be given to thecompatibility of powders with widely different surface areasphysical properties within the intended process.7. Sampling7.1 PlutoniumPuO2 oxide is hygroscopic and can absorb sufficient wat
44、er during exposure to a moist atmosphere to causedetectable analytical errors. Sampling, weighing of the sample, and handling the sample shall be done under atmosphericconditions that do not alter the moisture or impurity content of the sample.7.2 The necessary chemical and physical analyses shall b
45、e performed on portions of a representative sample taken from eachlot.7.2.1 A lot is defined as the quantity of material that is uniform in isotopic, chemical, and physical characteristics.7.2.2 Lots may be formed by blending the powder to ensure homogeneity within each lot.7.2.3 The mixing of two o
46、r more lots shall require the establishment of a new lot.7.2.4 The identity of a lot shall be retained throughout its processing history.7.2.5 A powder lot shall form the basis for defining sampling plans used to establish conformance to this specification.7.3 Sampling plans and procedures, includin
47、g the frequency and time period for conducting analyses, shall be agreed uponbetween buyer and seller in accordance with quality assurance requirements.seller.Analytical confirmation of sampling plans shallbe documented as part of the manufacturers quality assurance and nuclear materials control and
48、 accountability program.7.4 All sample containers shall be clearly identified by lot number and container number.7.5 The sample material shall be packaged so that no foreign material is introduced into the powder during storage or shipment.7.6 Lot AcceptanceAcceptance testing may be performed by the
49、 buyer on either the sample provided by the seller or a sampletaken at the buyers plant by sampling one or more individual containers with a sample thief. Practice E105 is referenced as a guide.Acceptance shall be on a lot basis and shall be contingent upon the material properties meeting the requirements of Sections 4through 7.8. Methods of Chemical and Isotopic Analysis8.1 The analytical chemistry methods used shall be as described in Test Method C697 or other methods agreed upon betweenbuyer and seller. See, for example, ISO 8300 for dete
