3.1 The purpose of this guide is to establish criteria for the design of gloveboxes as primary confinement systems to ensure the safety of the workers and the protection of the environment when storing, handling, processing, and disposing of both combustible and non-combustible forms of plutonium. The use of this guide will provide the user with guidance to design a successfully performing glovebox system.1.1 This guide defines criteria for the design of glovebox systems to be used for the handling of plutonium in any chemical or physical form or isotopic composition or when mixed with other elements or compounds. Not included in the criteria are systems auxiliary to the glovebox systems such as utilities, ventilation, alarm, and waste disposal. Also not addressed are hot cells or open-face hoods.1.2 The scope of this guide excludes specific license requirements relating to provisions for criticality prevention, hazards control, safeguards, packaging, and material handling. Observance of this guide does not relieve the user of the obligation to conform to all federal, state, and local regulations for design and construction of glovebox systems.1.3 Units—The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in nonconformance with the 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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5.1 This practice provides a means of collecting fluoride and chloride from plutonium test materials for analysis by ISE or IC. The results can be used to determine whether the material meets the requirements of Specifications C757 or C833, or other specification agreed by a supplier and customer, for fluoride or chloride content, or both.1.1 This practice provides a procedure for the preparation of samples of plutonium (Pu) materials, using pyrohydrolysis, for subsequent measurement of fluoride, chloride, or both, by ion chromatography (IC) or ion-selective electrode (ISE).1.2 This practice utilizes a sample size of 0.3 ± 0.1 g and is therefore suitable when the larger sample size used in Test Methods C697 and C698 is not available.1.3 Test materials within the scope of this practice include plutonium dioxide powder and mixed (U, Pu) oxide powder. Pellets of plutonium dioxide and mixed (U, Pu) oxide may also be treated after pulverization and with use of an accelerant. Samples of neptunium oxide may also be prepared using this practice.1.4 Full recovery may not be achieved for levels above 50 μg/g fluoride or 50 μg/g chloride (1).2 At higher levels precipitation may occur in the reaction vessel or condenser, or both. The user should validate suitability of the method above these levels.1.5 The procedure described in this practice may be applicable to other plutonium materials, such as plutonium compounds and scrap metals. The user must determine the safety and applicability of this practice to such materials.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7 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.1.8 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 is intended for use in quality control laboratories where a quantitative analysis of adsorbed moisture on a PuO2 sample is desired.5.2 The parameters described should be considered as guidelines. They may be altered to suit a particular analysis or type of analyzer, provided the changes are validated by the laboratory and noted in the report.5.3 The quantity of an adsorbed gas on a given PuO2 sample may indicate specific quality or end use performance characteristics. Specific limits on moisture content, for example, are required in cases where PuO2 will be packaged and stored for extended periods of time.1.1 This test method provides necessary information to determine the total amount of moisture (physisorbed and chemisorbed water molecules) in a plutonium dioxide (PuO2) sample using a combination of thermogravimetric and mass spectrometric analyses. This test method is useful when performing analysis in cases where a maximum amount of moisture content in PuO2 samples has been agreed upon by interested parties. For example this method can be used to determine the moisture content of some types of PuO2 packaged to meet the requirements of DOE-STD-3013 (1),2 “Stabilization, Packaging, and Storage of Plutonium-Bearing Materials,” when such PuO2 meets the specifications given in this test method (2).1.2 This test method is applicable to PuO2 samples having the following characteristics: Plutonium mass fraction ≥ 83 % (the plutonium in the sample should be close to stoichiometric PuO2 which is approximately 88 wt% plutonium depending on the isotopic composition of the plutonium, but can have several weight percent impurities), moisture ≤1 %.1.3 The temperature range of test is typically room temperature to greater than 1000 °C. Typically the PuO2 is heated to 1100 °C.1.4 This test method utilizes an inert gas environment (argon, nitrogen, or helium).1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 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.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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5.1 Uranium and plutonium oxides can be used as a nuclear-reactor fuel in the form of pellets. In order to be suitable for use as a nuclear fuel the starting material must meet certain specifications, such as found in Specifications C757, C833, C753, C776, C1008, or as specified by the purchaser. The uranium concentration, plutonium concentration, or both, and the isotopic abundances are measured by mass spectrometry following this test method.5.2 The separated heavy element fractions placed on mass spectrometric filaments must be very pure. The quantity required depends upon the sensitivity of the instrument detection system. If an electron multiplier detector is to be used, only a few nanograms are required. If a Faraday cup is used, a few micrograms are needed. Chemical purity of the sample becomes more important as the sample size decreases, because ion emission of the sample is suppressed by impurities.1.1 This test method covers the determination of the concentration and isotopic composition of uranium and plutonium in solutions. The purified uranium or plutonium from samples ranging from nuclear materials to environmental or bioassay matrices is loaded onto a mass spectrometric filament. The isotopic ratio is determined by thermal ionization mass spectrometry, the concentration is determined by isotope dilution.1.2 The values stated in SI units are to be regarded as the standard. Values in parentheses are for information only.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 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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5.1 This test method may be run together with Test Method C1432 to analyze for trace impurities in Pu metal. Using the technique described in this test method and the technique described in Test Method C1432 will provide the analyst with a more thorough verification of the impurity concentrations contained in the Pu metal sample. In addition, Test Method C1432 can be used to determine impurity concentrations for analytes such as Ca, Fe, Na, and Si, which have not been determined using this test method.5.2 This test method can be used on Pu matrices in nitrate solutions.5.3 This test method has been validated for use on materials that meet the specifications described in Specification C757 and Test Methods C758 and C759.5.4 This test method has been validated for all elements listed in Table 1.(A) Without outlying value.1.1 This test method covers the determination of trace elements in plutonium (Pu) materials such as Pu metal, Pu oxides, and Pu/uranium (U) mixed oxides. The Pu sample is dissolved in acid, and the concentration of the trace impurities are determined by Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS).1.2 This test method is specific for the determination of trace impurities where the samples are dissolved and the oxidation state is adjusted to the Pu(IV) and, if applicable, the U(VI) state. It may be applied to other matrices; however, it is the responsibility of the user to evaluate the performance of other matrices.1.3 The use of a quadrupole ICP-MS or a high resolution ICP-MS (HR-ICP-MS) can be employed in all applications relevant to this test method. HR-ICP-MS is a better option in many cases since it can reduce or potentially eliminate interferences encountered in the following complex sample matrices.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 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.1.6 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 practice can be used to separate uranium or plutonium, or both, prior to the impurity analysis by various techniques. The removal of uranium and plutonium prior to quantification can improve the detection limits by minimizing the signal suppression caused by uranium or plutonium when using ICP techniques. Detection limits of ~1–10 part-per-billion (PPB) may be obtainable by matrix removal. Also, removal of the uranium and plutonium may allow the impurities analysis to be performed on a non-glove box enclosed instrument.5.2 Other test methods exist to determine impurities in uranium or plutonium. Test Method C1517 is able to determine many impurities in uranium at detection levels of ~1–10 part-per-million (ppm) by DC-Arc Spectrometry. Test Method C1287 is able to determine impurities in uranium at detection levels of ~100 ppb by ICP-MS. Test Method C1432 provides an alternative technique to remove plutonium by ion exchange prior to analysis of the impurities by ICP-AES.5.3 This practice can be used to demonstrate compliance with nuclear fuel specifications, for example, Specifications C753, C757, C776, C787, C788, and C996.1.1 This practice covers instructions for using an extraction chromatography column method for the removal of plutonium or uranium, or both, from liquid or digested oxides or metals prior to impurity measurements. Quantification of impurities can be made by techniques such as inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES), or atomic absorption spectrometry (AAS.)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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5.1 The total evaporation method is used to measure the isotopic composition of uranium, plutonium, and americium materials, and may be used to measure the elemental concentrations of these elements when employing the IDMS technique.5.2 Uranium and plutonium compounds are used as nuclear reactor fuels. In order to be suitable for use as a nuclear fuel the starting material must meet certain criteria, such as found in Specifications C757, C833, C753, C776, C787, C967, C996, or as specified by the purchaser. The uranium concentration, plutonium concentration, or both, and isotope abundances are measured by TIMS following this method.5.3 Americium-241 is the decay product of 241Pu isotope. The abundance of the 241Am isotope together with the abundance of the 241Pu parent isotope can be used to estimate radio-chronometric age of the Pu material for nuclear forensic applications Ref (6). The americium concentration and isotope abundances are measured by TIMS following this method.5.4 The total evaporation method allows for a wide range of sample loading with no significant change in precision or accuracy. The method is also suitable for trace-level loadings with some loss of precision and accuracy. The total evaporation method and modern instrumentation allow for the measurement of minor isotopes using ion counting detectors, while the major isotope(s) is(are) simultaneously measured using Faraday cup detectors.5.5 The new generation of miniaturized ion counters allow extremely small samples, in the picogram range, to be measured via the total evaporation method. The method may be employed for measuring environmental or safeguards inspection samples containing nanogram quantities of uranium or plutonium. Very small loadings require special sample handling and careful evaluation of measurement uncertainties.5.6 Typical uranium analyses are conducted using sample loadings between 50 nanograms and 800 nanograms. For uranium isotope ratios the total evaporation method had been used in several recent NBL isotopic certified reference material (CRM) characterizations (for example (2, 3)). A detailed comparison of the total evaporation data on NBL uranium CRMs analyzed by the MAT 261 and TRITONTM instruments is provided in Ref (5). For total evaporation, plutonium analyses are generally conducted using sample loads in the range of 20 to 200 nanograms of plutonium.1.1 This method describes the determination of the isotopic composition, or the concentration, or both, of uranium, plutonium, and americium as nitrate solutions by the total evaporation method using a thermal ionization mass spectrometer (TIMS) instrument. Purified uranium, plutonium, or americium nitrate solutions are deposited onto a metal filament and placed in the mass spectrometer. Under computer control, ion currents are generated by heating of the filament(s). The ion currents are continually measured until the whole deposited solution sample is exhausted. The measured ion currents are integrated over the course of the measurement and normalized to a reference isotope ion current to yield isotope ratios.1.2 In principle, the total evaporation method should yield isotope ratios that do not require mass bias correction. In practice, samples may require this bias correction. Compared to the conventional TIMS method described in Test Method C1625, the total evaporation method is approximately two times faster, improves precision of the isotope ratio measurements by a factor of two to four, and utilizes smaller sample sizes. Compared to the C1625 method, the total evaporation method provides “major” isotope ratios 235U/238U, 240Pu/239Pu, and 241Am/243Am with improved accuracy.1.3 The total evaporation method is prone to biases in the “minor” isotope ratios (233U/238U, 234U/238U, and 236U/238U ratios for uranium materials and 238Pu/239Pu, 241Pu/239Pu, 242Pu/239Pu, and 244Pu/239Pu ratios for plutonium materials) due to peak tailing from adjacent major isotopes. The magnitude of the absolute bias is dependent on measurement and instrumental characteristics. The relative bias, however, depends on the relative isotopic abundances of the sample. The use of an electron multiplier equipped with an energy filter may eliminate or diminish peak tailing effects. Measurement of the abundance sensitivity of the instrument may be used to ensure that such biases are negligible, or may be used to bias correct the minor isotope ratios.1.4 The values stated in SI units are to be regarded as standard. When non-SI units are provided in parentheses, they are for information only.1.5 This standard may involve the use of hazardous materials and equipment. This standard does not purport to address all 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 to determine the applicability of regulatory limitations prior to use.1.6 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 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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4.1 Plutonium dioxide is used in mixtures with uranium dioxide as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for plutonium content, isotopic composition, and impurity content. These test methods are designed to show whether or not a given material meets the specifications for these items as described in Specification C757.4.1.1 An assay is performed to determine whether the material has the minimum plutonium content specified on a dry weight basis.4.1.2 Determination of the isotopic content of the plutonium in the plutonium dioxide powder is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.4.1.3 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC) as described in Practice C1233.4.2 Fitness for Purpose of Safeguards and Nuclear Safety Applications—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets to determine compliance with specifications.1.2 The analytical procedures appear in the following order:  SectionsPlutonium Sample Handling   8 to 10Plutonium by Controlled-Potential Coulometry 2Plutonium by Ceric Sulfate Titration 3Plutonium by Amperometric Titration with Iron(II) 2Plutonium by Diode Array Spectrophotometry 3Nitrogen by Distillation Spectrophotometry Using Nessler Reagent  11 to 18Carbon (Total) by Direct Combustion–Thermal Conductivity  19 to 29Total Chlorine and Fluorine by Pyrohydrolysis  30 to 37Sulfur by Distillation Spectrophotometry  38 to 46Plutonium Isotopic Analysis by Mass Spectrometry 4Rare Earth Elements by Spectroscopy  47 to 54Trace Elements by Carrier–Distillation Spectroscopy  55 to 62(Alternative: Impurities by ICP-AES or ICP-MS)  Impurity Elements by Spark-Source Mass Spectrography 63 to 69Moisture by the Coulometric Electrolytic Moisture Analyzer 70 to 77Total Gas in Reactor-Grade Plutonium Dioxide Pellets 5Plutonium-238 Isotopic Abundance by Alpha Spectrometry 3Americium-241 in Plutonium by Gamma-Ray Spectrometry 2Rare Earths By Copper Spark-Spectroscopy 78 to 87Plutonium Isotopic Analysis by Mass Spectrometry 88 to 96Oxygen-To-Metal Atom Ratio by Gravimetry 97 to 1041.3 The values stated in SI units are to be regarded as 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Sections 6, 16.2.5, 44.7, 51.9 and 92.5.1.

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