5.1 This test method is considered to be the most accurate NDA technique for the assay of many physical forms of Pu. Isotopic measurements by gamma-ray spectroscopy or destructive analysis techniques are part of this test method when it is applied to the assay of Pu.5.1.1 Calorimetry has been applied to a wide variety of Pu-bearing solids including metals, alloys, oxides, fluorides, mixed Pu-U oxides, mixed oxide fuel pins, waste, and scrap, for example, ash, ash heels, salts, crucibles, and graphite scarfings) (2, 3). This test method has been routinely used at U.S. and European facilities for Pu process measurements and nuclear material accountability since the mid 1960’s (2-9).5.1.2 Pu-bearing materials have been measured in calorimeter containers ranging in size from about 0.025 m to about 0.63 m in diameter and from about 0.076 m to about 1.38 m in height.5.1.3 Gamma-ray spectroscopy typically is used to determine the Pu isotopic composition and 241Am to Pu ratio (see Test Method C1030). However, isotopic information from mass spectrometry and alpha counting measurements may be used instead (see Test Method C697).5.2 This test method is considered to be the most accurate NDA method for the measurement of tritium. For many physical forms of tritium compounds calorimetry is currently the only practical measurement technique available.5.3 Physical standards representative of the materials being assayed are not required for the test method.5.3.1 This test method is largely independent of the elemental distribution of the nuclear materials in the matrix.5.3.2 The accuracy of the method can be degraded for materials with inhomogeneous isotopic composition.5.4 The thermal power measurement is traceable to national measurement systems through electrical standards used to directly calibrate the calorimeters or to calibrate secondary 238Pu heat standards.5.5 Heat-flow calorimetry has been used to prepare secondary standards for neutron and gamma-ray assay systems (7-12).5.6 Four parameters of the item and the item packaging affect measurement time. These four parameters are density, mass, thermal conductivity, and change in temperature. The measurement well of passive calorimeters will also affect measurement time because it too will need to come to the new equilibrium temperature. Calorimeters operated in power compensation mode maintain a constant measurement well temperature and have no additional effect on measurement time.5.6.1 Calorimeter measurement times range from 20 minutes (13) for smaller, temperature-conditioned containers up to 72 h (14) for larger containers and items with long thermal-time constants.5.6.2 Measurement times may be reduced by using equilibrium prediction techniques, by temperature preconditioning of the item to be measured, by operating the calorimeter using the power compensation technique, or by optimization of the item container (low thermal mass and high thermal conductivity) and packaging.1.1 This test method describes the nondestructive assay (NDA) of plutonium, tritium, and 241Am using heat flow calorimetry. For plutonium the typical range of applicability, depending on the isotopic composition, corresponds to ~0.1 g to ~5 g quantities while for tritium the typical range extends from ~0.001 g to ~400 g. This test method can be applied to materials in a wide range of container sizes up to 380 L. It has been used routinely to assay items whose thermal power ranges from 0.001 W to 135 W.1.2 This test method requires knowledge of the relative abundances of the plutonium isotopes and the 241Am/Pu mass ratio to determine the total plutonium mass.1.3 This test method provides a direct measure of tritium content.1.4 This test method provides a measure of  241Am either as a single isotope or mixed with plutonium.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 and health practices and determine the applicability of regulatory limitations prior to use.

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4.1 Factors governing selection of a method for the determination of uranium include available quantity of sample, sample purity, desired level of reliability, and equipment availability.4.2 This test method is suitable for samples between 20 mg to 300 mg of uranium, is applicable to fast breeder reactor (FBR)-mixed oxides having a uranium to plutonium ratio of 2.5 and greater, is tolerant towards most metallic impurity elements usually specified for FBR-mixed oxide fuel, and uses no special equipment.4.3 The ruggedness of the titration method has been studied for both the volumetric (6) and the weight (7) titration of uranium with dichromate.1.1 This test method covers unirradiated uranium-plutonium mixed oxide having a uranium to plutonium ratio of 2.5 and greater. The presence of larger amounts of plutonium (Pu) that give lower uranium to plutonium ratios may give low analysis results for uranium (U) (1)2, if the amount of plutonium together with the uranium is sufficient to slow the reduction step and prevent complete reduction of the uranium in the allotted time. Use of this test method for lower uranium to plutonium ratios may be possible, especially when 20 mg to 50 mg quantities of uranium are being titrated rather than the 100 mg to 300 mg in the study cited in Ref (1). Confirmation of that information should be obtained before this test method is used for ratios of uranium to plutonium less than 2.5.1.2 The amount of uranium determined in the data presented in Section 12 was 20 mg to 50 mg. However, this test method, as stated, contains iron in excess of that needed to reduce the combined quantities of uranium and plutonium in a solution containing 300 mg of uranium with uranium to plutonium ratios greater than or equal to 2.5. Solutions containing up to 300 mg uranium with uranium to plutonium ratios greater than or equal to 2.5 have been analyzed (1) using the reagent volumes and conditions as described in Section 10.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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All plutonium materials covered in this test method are used in the preparation of nuclear-reactor fuels. In order to be suitable for this purpose, the materials must meet specified criteria for plutonium content. This test method is used to verify the plutonium content.A primary standard dichromate such as that available from National Institute of Standards and Technology (NIST) or a dichromate traceable to a primary standard such as New Brunswick Laboratory (NBL) plutonium standard, is required for this technique.1.1 This test method covers the determination of plutonium in unirradiated nuclear-grade plutonium dioxide, uranium-plutonium mixed oxides with uranium (U)/plutonium (Pu) ratios up to 21, plutonium metal, and plutonium nitrate solutions. Optimum quantities of plutonium to measure are 7 to 15 mg.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 and health practices and determine the applicability of regulatory limitations prior to use.

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5.1 This test method is useful for determining the plutonium content of scrap and waste in containers ranging from small cans with volumes of the order of a mL to crates and boxes of several thousand liters in volume. A common application would be to 208-L (55-gal) drums. Total Pu content ranges from 10 mg to 6 kg (1). The upper limit may be restricted depending on specific matrix, calibration material, criticality safety, or counting equipment considerations. 5.2 This test method is applicable for U.S. Department of Energy shipper/receiver confirmatory measurements (9), nuclear material diversion detection, and International Atomic Energy Agency attributes measurements (10). 5.3 This test method should be used in conjunction with a scrap and waste management plan that segregates scrap and waste assay items into material categories according to some or all of the following criteria: bulk density, the chemical forms of the plutonium and the matrix, americium to plutonium isotopic ratio, and hydrogen content. Packaging for each category should be uniform with respect to size, shape, and composition of the container. Each material category might require calibration standards and may have different Pu mass limits. 5.4 Bias in passive neutron coincidence measurements is related to item size and density, the homogeneity and composition of the matrix, and the quantity and distribution of the nuclear material. The precision of the measurement results is related to the quantity of nuclear material, the (α,n) reaction rate, and the count time of the measurement. 5.4.1 For both benign matrix and matrix specific measurements, the method assumes the calibration reference materials match the items to be measured with respect to the homogeneity and composition of the matrix, the neutron moderator and absorber content, and the quantity of nuclear material, to the extent they affect the measurement. 5.4.2 Measurements of smaller containers containing scrap and waste are generally more accurate than measurements of larger items. 5.4.3 It is recommended that where feasible measurements be made on items with homogeneous contents. Heterogeneity in the distribution of nuclear material, neutron moderators, and neutron absorbers have the potential to cause biased results. 5.5 The coincident neutron production rates measured by this test method are related to the mass of the even number isotopes of plutonium. If the relative abundances of these isotopes are not accurately known, biases in the total Pu assay value will result. 5.6 Typical count times are in the range of 300 to 3600 s. 5.7 Reliable results from the application of this method require training of the personnel who package the scrap and waste prior to measurement and of personnel who perform the measurements. Training guidance is available from ANSI 15.20, Guides C986, C1009, C1068, and C1490. 1.1 This test method describes the nondestructive assay of scrap or waste for plutonium content using passive thermal-neutron coincidence counting. This test method provides rapid results and can be applied to a variety of carefully sorted materials in containers as large as several thousand liters in volume. The test method applies to measurements of 238Pu,  240Pu, and 242Pu and has been used to assay items whose total plutonium content ranges from 10 mg to 6 kg (1) .2 1.2 This test method requires knowledge of the relative abundances of the Pu isotopes to determine the total Pu mass (Test Method C1030). 1.3 This test method may not be applicable to the assay of scrap or waste containing other spontaneously fissioning nuclides. 1.3.1 This test method may give biased results for measurements of containers that include large amounts of hydrogenous materials. 1.3.2 The techniques described in this test method have been applied to materials other than scrap and waste (2, 3). 1.4 This test method assumes the use of shift-register-based coincidence technology (4). 1.5 Several other techniques that are often encountered in association with passive neutron coincidence counting exist. These include neutron multiplicity counting (5, 6, Test Method C1500), add-a-source analysis for matrix correction (7), flux probes also for matrix compensation, cosmic-ray rejection (8) to improve precision close to the detection limit, and alternative data collection electronics such as list mode data acquisition. Passive neutron coincidence counting may also be combined with certain active interrogation schemes as in Test Methods C1316 and C1493. Discussions of these established techniques are not included in this method. 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 was developed to measure plutonium in environmental waters or waters released to the environment and to determine whether or not the plutonium concentration exceeds the maximum amount allowable by regulatory statutes.1.1 This test method covers the determination of alpha-particle-emitting isotopes of plutonium concentrations over 0.01 Bq/L (0.3 pCi/L) in water by means of chemical separations and alpha pulse-height analysis (alpha-particle spectrometry). Due to overlapping alpha-particle energies, this method cannot distinguish 239Pu from 240Pu. Plutonium is chemically separated from a 1-L water sample by coprecipitation with ferric hydroxide, anion exchange and electrodeposition. The test method applies to soluble plutonium and to suspended particulate matter containing plutonium. In the latter situation, an acid dissolution step is required to assure that all of the plutonium dissolves.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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards are given in Section 9.

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1.1 This test method is applicable to the assay or purity determination of plutonium metal of 98% purity or higher. Uranium and iron are known interferences and must be determined separately. Their respective corrections must then be made to the assay value. 1.2 The recommended amount of plutonium determined in the titration is 210 to 240 mg. 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.

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1.1 This test method is applicable to the determination of uranium (U) and plutonium (Pu) concentrations and their isotopic abundances (Note 1) in solutions which result from the dissolution of nuclear reactor fuels either before or after irradiation. A minimum sample size of 50 [mu]g of irradiated U will contain sufficient Pu for measurement and will minimize the effects of cross contamination by environment U. Note 1—The isotopic abundance of Pu can be determined by this test method; however, interference from U may be encountered. This interference may be due to (1) inadequate chemical separation of uranium and plutonium, (2) uranium contamination within the mass spectrometer, and (3) uranium contamination in the filament. One indication of uranium contamination is a changing 238/239 ratio during the mass spectrometer run, in which case, a meaningful Pu analysis cannot be obtained on that run. If inadequate separation is the problem, a second pass through the separation may remove the uranium. If contamination in the mass spectrometer or on the filaments is the problem, use of a larger sample, for example, 1 μg, on the filament may ease the problem. A recommended alternative method of determining Pu isotopic abundance without U interference is alpha spectroscopy using Practice D3084. The Pu abundance should be obtained by determining the ratio of alpha particle activity of Pu to the sum of the activities of Pu and Pu. (1) The contribution of Pu and Pu to the alpha activity differs from their isotopic abundances due to different specific activities. 1.2 The procedure is applicable to dissolver solutions of uranium fuels containing plutonium, aluminum, stainless steel, or zirconium. Interference from other alloying constituents has not been investigated and no provision has been made in the test method for fuels used in the Th U fuel cycle. 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.

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5.1 This test method is intended for determination of loose or tapped bulk density or both for PuO2 powders or compounds in the nuclear industry. It is intended for use when the quantity of available material for performing the measurements is limited because of reasons such as nuclear safety or laboratory scale limits on nuclear inventory.5.2 This test method can be applied to other metal powders in the nuclear industry provided that appropriate validation has been performed.5.3 Values of loose bulk density obtained using this test method should be used with caution since they can vary considerably depending on factors such as the initial state of dispersion of the test specimen, height-to-diameter ratio of the specimen in the graduated cylinder, the dryness of the powder, and operator-to-operator variation (for example, the speed with which the sample is poured into the cylinder).5.4 The data from the tapped bulk density test can be used to estimate the needed volume of small containers holding a fixed mass of powder that has been compacted.5.5 This test method may be useful for the determination of the Carr Compressibility Index as described in Test Method D6393.1.1 This test method specifies a method for the determination of loose and tapped bulk density of plutonium oxide (PuO2) powder.1.2 This test method is applicable when limited quantities of powder are available for performance of the measurements. Alternative test methods, such as Test Methods B527 or D7481, may be used when sufficient quantities are available.1.3 This test method contains notes that are explanatory and are not part of the mandatory requirements of the method.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. Some specific hazards statements are given in Section 7 on Hazards.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 test method is useful for determining the plutonium content of items such as impure Pu oxide, mixed Pu/U oxide, oxidized Pu metal, Pu scrap and waste, Pu process residues, and weapons components.5.2 Measurements made with this test method may be suitable for safeguards or waste characterization requirements such as:5.2.1 Nuclear materials accountability,5.2.2 Inventory verification (7),5.2.3 Confirmation of nuclear materials content (8),5.2.4 Resolution of shipper/receiver differences (9),5.2.5 Excess weapons materials inspections (10, 11),5.2.6 Safeguards termination on waste (12, 13),5.2.7 Determination of fissile equivalent content (14).5.3 A significant feature of neutron multiplicity counting is its ability to capture more information than neutron coincidence counting because of the availability of a third measured parameter, leading to reduced measurement bias for most material categories for which suitable precision can be attained. This feature also makes it possible to assay some in-plant materials that are not amenable to conventional coincidence counting, including moist or impure plutonium oxide, oxidized metal, and some categories of scrap, waste, and residues (10).5.4 Calibration for many material types does not require representative standards. Thus, the technique can be used for inventory verification without calibration standards (7), although measurement bias may be lower if representative standards were available.5.4.1 The repeatability of the measurement results due to counting statistics is related to the quantity of nuclear material, interfering neutrons, and the count time of the measurement (15) .5.4.2 For certain materials such as small Pu, items of less than 1 g, some Pu-bearing waste, or very impure Pu process residues where the (α,n) reaction rate overwhelms the triples signal, multiplicity information may not be useful because of the poor counting statistics of the triple coincidences within practical counting times (12).5.5 For pure Pu metal, pure oxide, or other well-characterized materials, the additional multiplicity information is not needed, and conventional coincidence counting will provide better repeatability because the low counting statistics of the triple coincidences are not used. Conventional coincidence information can be obtained either by changing to coincidence analyzer mode, or analyzing the multiplicity data in coincidence mode.5.6 The mathematical analysis of neutron multiplicity data is based on several assumptions that are detailed in Annex A1. The mathematical model considered is a point in space, with assumptions that neutron detection efficiency, die-away time, and multiplication are constant across the entire item (16, 17) . As the measurement deviates from these assumptions, the biases will increase.5.6.1 Bias in passive neutron multiplicity measurements is related to deviations from the “point model” such as variations in detection efficiency, matrix composition, or distribution of nuclear material in the item's interior.5.6.2 Heterogeneity in the distribution of nuclear material, neutron moderators, and neutron absorbers may introduce biases that affect the accuracy of the results. Measurements made on items with homogeneous contents will be more accurate than those made on items with inhomogeneous contents.1.1 This test method describes the nondestructive assay of plutonium in forms such as metal, oxide, scrap, residue, or waste using passive neutron multiplicity counting. This test method provides results that are usually more accurate than conventional neutron coincidence counting. The method can be applied to a large variety of plutonium items in various containers including cans, 208-L drums, or 1900-L Standard Waste Boxes. It has been used to assay items whose plutonium content ranges from 1 g to 1000s of g.1.2 There are several electronics or mathematical approaches available for multiplicity analysis, including the multiplicity shift register, the Euratom Time Correlation Analyzer, and the List Mode Module, as described briefly in Ref. (1).21.3 This test method is primarily intended to address the assay of 240Pu-effective by moments-based multiplicity analysis using shift register electronics (1, 2, 3) and high efficiency neutron counters specifically designed for multiplicity analysis.1.4 This test method requires knowledge of the relative abundances of the plutonium isotopes to determine the total plutonium mass (See Test Method C1030).1.5 This test method may also be applied to modified neutron coincidence counters (4) which were not specifically designed as multiplicity counters (that is, HLNCC, AWCC, etc), with a corresponding degradation of results.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 and health practices and determine the applicability of regulatory limitations prior to use.

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This specification covers sinterable nuclear-grade plutonium dioxide powders obtained by the oxalate precipitation route, calcination, or any other equivalent process acceptable to the buyer. Included is plutonium dioxide of various isotopic compositions as normally prepared by in-reactor neutron irradiation of natural or slightly enriched uranium, or recycled plutonium mixed with uranium. The material shall conform to required chemical compositions of plutonium, uranium, americium, impurities (boron, cadmium, carbon, chlorine, chromium, fluorine, iron, gadolinium, nickel, nitride nitrogen, and thorium), equivalent boron, and gamma activity. Materials shall also adhere to physical property requirements as to cleanliness and workmanship, particle size, and surface area.1.1 This specification covers nuclear grade PuO2 powder. It applies to PuO2 of various isotopic compositions as normally prepared by in-reactor neutron irradiation of natural or slightly enriched uranium or by in-reactor neutron irradiation of recycled plutonium mixed with uranium.1.2 There is no discussion of or provision for preventing criticality incidents, nor are health and safety requirements, the avoidance of hazards, or shipping precautions and controls discussed. Observance of this specification does not relieve the user of the obligation to be aware of and conform to all applicable international, national, or federal, state, and local regulations pertaining to possessing, shipping, processing, or using source or special nuclear material. For examples in the U.S. Government, relevant documents are Code of Federal Regulations, Title 10 Nuclear Safety Guide, U.S. Atomic Energy Commission Report TID-70162, and “Handbook of Nuclear Safety”, H. K. Clark, U.S. Atomic Energy Commission Report, 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 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 A soil sampling and analysis program provides a direct means of determining the concentration and distribution of radionuclides in soil. A soil analysis program has the most significance for the preoperational monitoring program to establish baseline concentrations prior to the operation of a nuclear facility. Soil analysis, although useful in special cases involving unexpected releases, is a poor technique for assessing small incremental releases and is therefore not recommended as a method for routine monitoring releases of radioactive material. Nevertheless, because soil is an integrator and a reservoir of long-lived radionuclides, and serves as an intermediary in several of the plutonium pathways of potential importance to humans, knowledge of the concentration of plutonium in soil is essential.1.1 This test method covers the determination of plutonium in soils at levels of detection dependent on count time, sample size, detector, background, and tracer yield. This test method describes one acceptable approach to the determination of plutonium in soil.1.2 This test method is designed for 10 g of soil, previously collected and treated as described in Practices C998 and C999, but sample sizes up to 50 g may be analyzed by this test method. This test method may not be able to completely dissolve all forms of plutonium in the soil matrix.1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 10.1.5 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 These test methods are designed to show whether a given material meets the purchaser's specifications.4.1.1 An assay is performed to determine whether the material has the specified plutonium content.4.1.2 Determination of the isotopic content of the plutonium is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.4.1.3 Impurity content is verified by a variety of methods to ensure that the maximum concentration limit of specified impurities is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC).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, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal to determine compliance with specifications.1.2 The analytical procedures appear in the following order:  SectionsDissolution Procedure 2Plutonium by Controlled-Potential Coulometry 3Plutonium by Amperometric Titration with Iron (II) 2Plutonium by Ceric Sulfate Titration Test Method 3Plutonium by Diode Array Spectrophotometry 3Uranium by Arsenazo I Spectrophotometric Test Method 8 – 10Thorium by Thorin Spectrophotometric Test Method 11 – 13Iron by 1,10-Phenanthroline Spectrophotometric Test Method 14 – 16Iron by 2,2ʹ-Bipyridyl Spectrophotometric Test Method 17 – 23Impurities by ICP-AES  Chloride by the Thiocyanate Spectrophotometric Test Method 24 – 26Fluoride by Distillation-Spectrophotometric Test Method 27–28Nitrogen by Distillation-Nessler Reagent Spectrophotometric Test Method 29–30Carbon by the Direct Combustion-Thermal Conductivity Test Method 31 – 33Sulfur by Distillation-Spectrophotometric Test Method 34 – 36Isotopic Composition by Mass Spectrometry 37 and 38Plutonium-238 Isotopic Abundance by Alpha Spectrometry  Americium-241 by Extraction and Gamma Counting 39 – 41Americium-241 by Gamma Counting 3Gamma-Emitting Fission Products, Uranium, and Thorium by Gamma-Ray Spectroscopy 42 – 49Rare Earths by Copper Spark Spectrochemical Test Method 50 – 52Tungsten, Niobium (Columbium), and Tantalum by Spectro- chemical Test Method 53 – 55Sample Preparation for Spectrographic Analysis for Trace Impuri- ties 56 – 601.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific safeguard and safety hazards statements, see Section 6.1.5 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 are used in nuclear reactor fuel and must be analyzed to ensure that they meet acceptance criteria for isotopic composition as described in Specifications C833 and C1008. The criteria are set by mutual agreement between the manufacturer and end user (or between buyer and seller). This standard practice is used to separate chemically the isobaric interferences from 238U and 238Pu and from 241Am and 241Pu, and from other impurities prior to isotopic abundance determination by TIMS.5.2 In facilities where perchloric acid use is authorized, the separation in Test Method C698 may be used prior to isotopic abundance determination. Uranium and plutonium content as well as isotopic abundances using TIMS can be determined by using this separation practice and by following Test Methods C698, C1625, or C1672.1.1 This practice is an alternative to Practice C1411 for the ion exchange separation in small mass samples (~5 μg of plutonium and up to 0.5 mg of uranium in 1 mL of solution) of uranium and plutonium from each other and from other impurities for subsequent isotopic abundance and content analysis by thermal ionization mass spectrometry (TIMS). In addition to being adapted to smaller sample sizes, this practice also avoids the use of hydrochloric acid (HCl) and hydrofluoric acid (HF) and does not require the use of two anion exchange columns as required in Practice C1411.1.2 In chemically unseparated samples isobaric nuclides at mass 238 (238U and 238Pu), and mass 241 (241Pu and 241Am) will be measured together thus compromising the accuracy of the results of isotopic composition of Pu. Therefore, chemical separation of elements is essential prior to isotopic analyses. Concentrations and volumes given in the paragraphs below can be modified for larger sample sizes, different types of anion exchange resin, etc.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 and health practices and determine the applicability of regulatory limitations prior to use.

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4.1 These test methods are designed to show whether a given material meets the purchaser's specifications.4.1.1 An assay is performed to determine whether the material has the specified plutonium content.4.1.2 Determination of the isotopic content of the plutonium in the plutonium-nitrate solution is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.4.1.3 Impurity content is determined by a variety of methods to ensure that the maximum concentration limit of specified impurities is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC).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, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications.1.2 The analytical procedures appear in the following order:  Sections Plutonium by Controlled-Potential Coulometry 2Plutonium by Amperometric Titration with Iron(II) 2Plutonium by Diode Array Spectrophotometry  Free Acid by Titration in an Oxalate Solution 8 to 15Free Acid by Iodate Precipitation-Potentiometric Titration  Test Method 16 to 22Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33Thorium by Thorin Spectrophotometric Test Method 34 to 42Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50Impurities by ICP-AES  Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58Fluoride by Distillation-Spectrophotometric Test Method 59 to 66Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74Isotopic Composition by Mass Spectrometry 75 to 76Plutonium-238 Isotopic Abundance by Alpha Spectrometry  Americium-241 by Extraction and Gamma Counting 77 to 85Americium-241 by Gamma Counting 86 to 94Gamma-Emitting Fission Products, Uranium, and Thorium by Gamma-Ray Spectroscopy 94 to 102Rare Earths by Copper Spark Spectrochemical Test Method 103 to 105Tungsten, Niobium (Columbium), and Tantalum by Spectro- chemical Test Method 106 to 114Sample Preparation for Spectrographic Analysis for General Impurities 115 to 1181.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific safeguard and safety hazard statements, see Section 6.1.5 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 test method allows the determination of 241Am in a plutonium solution without separation of the americium from the plutonium. It is generally applicable to any solution containing 241Am.5.2 The 241Am in solid plutonium materials may be determined when these materials are dissolved (see Practice C1168).5.3 When the plutonium solution contains unacceptable levels of fission products or other materials, this method may be used following a tri-n-octylphosphine oxide (TOPO) extraction, ion exchange or other similar separation techniques (see Test Methods C758 and C759).5.4 This test method is less subject to interferences from plutonium than alpha counting since the energy of the gamma ray used for the analysis is better resolved from other gamma rays than the alpha particle energies used for alpha counting.5.5 The minimal sample preparation reduces the amount of sample handling and exposure to the analyst.5.6 This test method is applicable only to homogeneous solutions. This test method is not suitable for solutions containing solids.5.7 Solutions containing 241Am at concentrations as little as 1 × 10−5 g/L may be analyzed using this method. The lower limit depends on the detector used and the counting geometry. Solutions containing high concentrations may be analyzed following an appropriate dilution.1.1 This test method covers the quantitative determination of 241Am by gamma-ray spectrometry in plutonium nitrate solution samples that do not contain significant amounts of radioactive fission products or other high specific activity gamma-ray emitters.1.2 This test method can be used to determine the 241Am in samples of plutonium metal, oxide and other solid forms, when the solid is appropriately sampled and dissolved.1.3 The values stated in SI units are to be regarded as standard. Additionally, the non-SI units of electron volts, kiloelectron volts, and liters are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.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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