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ASTM C1235-99 Standard Test Method for Plutonium by Titanium(III)/Cerium(IV) Titration (Withdrawn 2005) Withdrawn, No replacement 发布日期 :  1970-01-01 实施日期 : 

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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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