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5.1 Uranium and plutonium are used in nuclear reactor fuel and must be analyzed to insure that they meet certain criteria for isotopic composition as described in Specifications C833 and C1008. This practice is used to chemically separate the same mass peak interferences from uranium and plutonium and from other impurities prior to isotopic abundance determination by thermal ionization mass spectrometry.5.2 In those facilities where perchloric acid use is tolerated, the separation in Test Method C698 may be used prior to isotopic abundance determination. Uranium and plutonium concentrations as well as isotopic abundances using thermal ionization mass spectrometry can be determined using this separation and following Test Method C1625.1.1 This practice is for the ion exchange separation of uranium and plutonium from each other and from other impurities for subsequent isotopic analysis by thermal ionization mass spectrometry. Plutonium-238 and uranium-238, and plutonium-241 and americium-241, will appear as the same mass peak and must be chemically separated prior to analysis. Only high purity solutions can be analyzed reliably using thermal ionization mass spectrometry.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.4 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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4.1 This  practice  is  applicable  when  small amounts of 241Am are present in plutonium samples (see Test Methods C758 and C759). An example is the determination of 241Am in a 238Pu sample. The high specific activity of 238Pu presents a safety hazard that precludes its presence in a counting facility. Therefore, it is necessary to remove the 238Pu prior to the determination of 241Am. 4.2 When a plutonium solution contains fission or activation products, this practice does not separate all radionuclides that interfere in the determination of 241Am, such as the rare earths. 1.1 This practice describes the use of an ion exchange technique to separate plutonium from solutions containing low concentrations  of americium  prior  to measurement of the 241Am by gamma counting. 1.2 This practice covers the removal of plutonium, but not all the other radioactive isotopes that may interfere in the determination of 241Am. 1.3 This practice can be used when 241Am is to be determined in samples in which the plutonium is in the form of metal, oxide, or other solid provided that the solid is appropriately sampled and dissolved (See Test Methods C758, C759, and C1168). 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.

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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)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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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.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 Section1 Dissolution of Plutonium Metal with Hydrochloric Acid at Room Temperature 92 Dissolution of Plutonium Metal with Hydrochloric Acid and Heating 103 Dissolution of Plutonium Metal with Sulfuric Acid 114 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxide by the Sealed-Reflux Technique 125 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxides by Sodium Bisulfate Fusion 136 Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired Plutonium Oxide in Beakers 147 Open-Vessel (with Reflux Condenser) Dissolution of Plutonium Oxide Powder 158 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Powder 169 Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder 1710 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Pellets 181.5 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.1.7 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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5.1 This test method can be used on plutonium matrices in nitrate solutions.5.2 This test method has been validated for all elements listed in Test Methods C757 except sulfur (S) and tantalum (Ta).5.3 This test method has been validated for all of the cation elements measured in Table 1. Phosphorus (P) requires a vacuum or an inert gas purged optical path instrument.1.1 This test method covers the determination of 25 elements in plutonium (Pu) materials. The Pu is dissolved in acid, the Pu matrix is separated from the target impurities by an ion exchange separation, and the concentrations of the impurities are determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES).1.2 This test method is specific for the determination of impurities in 8 M HNO3 solutions. Impurities in other plutonium materials, including plutonium oxide samples, may be determined if they are appropriately dissolved (see Practice C1168) and converted to 8 M HNO3 solutions.1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions that are provided for information only and are not considered standard. Additionally, the non-SI units of molarity and centimeters of mercury are to be regarded as 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. Some specific hazards statements are given in Section 9 on Hazards.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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5.1 The burnup of an irradiated nuclear fuel can be determined from the amount of a fission product formed during irradiation. Among the fission products, 148Nd has the following properties to recommend it as an ideal burnup indicator: 5.1.1 It is not volatile, does not migrate in solid fuels below their recrystallization temperature, and has no volatile precursors. 5.1.2 It is nonradioactive and requires no decay corrections. 5.1.3 It has a low destruction cross section and formation from adjacent mass chains can be corrected for. 5.1.4 It has good emission characteristics for mass analysis. 5.1.5 Its fission yield is nearly the same for 235U and 239Pu and is essentially independent of neutron energy (6). 5.1.6 It has a shielded isotope, 142Nd, which can be used for correcting natural Nd contamination. 5.1.7 It is not a normal constituent of unirradiated fuel. 5.2 The analysis of 148Nd in irradiated fuel does not depend on the availability of preirradiation sample data or irradiation history. Atom percent fission is directly proportional to the 148Nd-to-fuel ratio in irradiated fuel. However, the production of 148Nd from 147Nd by neutron capture will introduce a systematic error whose contribution must be corrected for. In power reactor fuels, this correction is relatively small. In test reactor irradiations where fluxes can be very high, this correction can be substantial (see Table 1). (A) Assuming continuous reactor operation and a 274 ± 91 barn 1 47Nd effective neutron absorption cross section for a thermal neutron power reactor. This cross section was obtained by adjusting the 440 ± 150 barn 147Nd cross section (7) measured at 20 °C to a Maxwellian spectrum at a neutron temperature of 300 °C. 5.3 The test method can be applied directly to U fuel containing less than 0.5 % initial Pu with 1 to 100 GW days/metric ton burnup. For fuel containing 5 to 50 % initial Pu, increase the Pu content by a factor of 10 to 100, respectively in both reagents 6.3 and 6.4. 1.1 This test method covers the determination of stable fission product 148Nd in irradiated uranium (U) fuel (with initial plutonium (Pu) content from 0 to 50 %) as a measure of fuel burnup (1-3).2 1.2 It is possible to obtain additional information about the uranium and plutonium concentrations and isotopic abundances on the same sample taken for burnup analysis. If this additional information is desired, it can be obtained by precisely measuring the spike and sample volumes and following the instructions in Test Method E267. 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. 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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