C26.05 - Methods of Test

SIGNIFICANCE AND USE
5.1 Specific gamma-ray emitting radionuclides in UF6 are identified and quantified using a high-resolution gamma-ray energy analysis system, which includes a high-resolution germanium detector. This test method shall be used to meet the health and safety specifications of C787, C788, and C996 regarding applicable fission products in reprocessed uranium solutions. This test method may also be used to provide information to parties such as conversion facilities on the level of uranium decay products in such materials. Pa-231 is a specific uranium decay product that may be present in uranium ore concentrate and is amenable to analysis by gamma spectrometry.
SCOPE
1.1 This test method covers the measurement of gamma energy emitted from fission products in uranium hexafluoride (UF6) and uranyl nitrate solution. This test method may also be used to measure the concentration of some uranium decay products. It is intended to provide a method for demonstrating compliance with UF6 Specifications C787 and C996, uranyl nitrate Specification C788, and uranium ore concentrate Specification C967.  
1.2 The lower limit of detection is estimated at 5000 MeV Bq/kg (MeV kg-1/s-1) of uranium and is the square root of the sum of the squares of the individual reporting limits of the nuclides to be measured. The limit of detection was determined on a pure, aged natural uranium (ANU) solution. The value is dependent upon the detector efficiency and background that can be achieved.  
1.3 The fission product nuclides to be measured are 106Ru/106Rh, 103Ru, 137Cs, 144Ce, 144Pr, 141Ce, 95Zr, 95Nb, and 125Sb. Among the uranium decay product nuclides that may be measured is 231Pa. Other gamma energy-emitting fission and uranium decay nuclides present in the spectrum at detectable levels should be identified and quantified as required by the data quality objectives.  
1.4 The values stated in SI units are to be regarded as standard. Additionally, the non-SI units of kiloelectron volts and megaelectron volts 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.

SIGNIFICANCE AND USE
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 evapo...
SCOPE
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 m...

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
5.1 This practice may be used to determine concentrations of elements leached from nuclear waste materials (glasses, ceramics, cements) using an aqueous leachant. If the nuclear waste material is radioactive, a suitably contained and shielded ICP-AES spectrometer system with a filtered exit-gas system must be used, but no other changes in the practice are required. The leachant may be deionized water or any aqueous solution containing less than 1 % total solids.  
5.2 This practice as written is for the analysis of solutions containing 1 % nitric acid. It can be modified to specify the use of the same or another mineral acid at the same or higher concentration. In such cases, the only change needed in this practice is to substitute the preferred acid and concentration value whenever 1 % nitric acid appears here. It is important that the acid type and content of the reference and check solutions closely match the leachate solutions to be analyzed.  
5.3 This practice can be used to analyze leachates from static leach testing of waste forms using Test Method C1220.
SCOPE
1.1 This practice is applicable to the determination of low concentration and trace elements in aqueous leachate solutions produced by the leaching of nuclear waste materials, using inductively coupled plasma-atomic emission spectroscopy (ICP-AES).  
1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioactive waste material.  
1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1 % total dissolved solids.  
1.4 This practice should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction.  
1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.  
1.6 This practice contains notes that are explanatory and are not part of the mandatory requirements of the method.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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.  
1.9 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.

SIGNIFICANCE AND USE
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.
SCOPE
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  
Section  
1  
Dissolution of Plutonium Metal with Hydrochloric Acid at Room Temperature  
9  
2  
Dissolution of Plutonium Metal with Hydrochloric Acid and Heating  
10  
3  
Dissolution of Plutonium Metal with Sulfuric Acid  
11  
4  
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed
Oxide by the Sealed-Reflux Technique  
12  
5  
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxides by Sodium Bisulfate Fusion  
13  
6  
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired Plutonium Oxide in Beakers  
14  
7  
Open-Vessel (with Reflux Condenser) Dissolution of Plutonium Oxide Powder  
15  
8  
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Powder  
16  
9  
Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder  
17  
10  
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Pellets  
18  
1.5 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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
5.1 Uranium hexafluoride is a basic material used to produce nuclear reactor fuel. To be suitable for this purpose, the material must meet criteria for isotopic composition. This test method is designed to determine whether the material meets the requirements described in Specifications C787 and C996.
SCOPE
1.1 This test method is applicable to the isotopic analysis of uranium hexafluoride (UF6) with  235U concentrations less than or equal to 5 % and 234U,  236U concentrations of 0.0002 to 0.1 %.  
1.2 This test method may be applicable to the analysis of the entire range of 235U isotopic compositions providing that adequate Certified Reference Materials (CRMs or traceable standards) are available.  
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.

SIGNIFICANCE AND USE
5.1 Uranium material is used as a fuel in certain types of nuclear reactors. To be suitable for use as nuclear fuel, the starting material shall meet certain specifications such as those described in Specifications C753, C776, C787, C833, C967, C996, and C1008, or as specified by the purchaser. The isotope amount ratios of uranium material can be measured by mass spectrometry following this test method to ensure that they meet the specification.  
5.2 The MTE method can be used for a wide range of sample sizes even in samples containing as low as 20 µg of uranium. If the uranium sample is in the form of uranium hexafluoride, it has to be converted into a uranium nitrate solution for measurement by the MTE method. The concentration of the loading solution for MTE has to be in the range of 1 mg/g to 6 mg/g to allow a sample loading of 2 µg to 6 µg of uranium. A minimum loading of 3 µg uranium per filament is strongly recommended. This is needed to have a sufficient and stable ion signal especially for the two minor isotopes (234U and 236U) thus enabling the internal calibration of SEM versus the Faraday cups using the 234U ion beam signal during the measurement.  
5.3 Until now, the instrument capabilities for the MTE method have only been implemented on the TRITON™ TIMS instrument.5 Therefore, all recommendations for measurement parameters in this test method are specified for the TRITON instrument. The manufacturers of other TIMS instruments (for example, IsotopX and Nu Instruments) have indicated plans to implement the modifications needed in their instruments to use the MTE method.  
5.4 The MTE method described here can also be extended to measurement of elements other than uranium. Note that the MTE method has already been implemented for plutonium and calcium.
SCOPE
1.1 This test method describes the determination of the isotope amount ratios of uranium material as nitrate solutions by the modified total evaporation (MTE) method using a thermal ionization mass spectrometer (TIMS) instrument.  
1.2 The analytical performance in the determination of the 235U/238U major isotope amount ratio by MTE is similar to the (“classical”) total evaporation (TE) method as described in C1672. However, in the MTE method, the evaporation process is interrupted on a regular basis to allow measurements and subsequent corrections for background from peak tailing, perform internal calibration of a secondary electron multiplier (SEM) detector versus the Faraday cups, peak centering, and ion source refocusing. Performing these calibrations and corrections on a regular basis during the measurement, improves precision, and significantly reduces uncertainties for the minor isotope amount ratios 234U/238U and 236U/238U as compared to the TE method.  
1.3 In principle, the MTE method may yield major isotope amount ratios without the need for mass fractionation correction. However, depending on the measurement conditions, small variations are observed between sample turrets. Therefore, a small correction based on measurements of a certified reference material is recommended to improve consistency. The uncertainty around the mass fractionation correction factor usually includes unity.  
1.4 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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 issu...

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
4.1 The materials covered that must meet ASTM specifications are uranium metal and uranium oxide.  
4.2 Uranium materials are used as nuclear reactor fuel. For this use, these materials must meet certain criteria for uranium content, uranium-235 enrichment, and impurity content, as described in Specifications C753 and C776. The material is assayed for uranium to determine whether the content is as specified.  
4.3 Uranium alloys, refractory uranium materials, and uranium containing scrap and ash are unique uranium materials for which the user must determine the applicability of this practice. In general, these unique uranium materials are dissolved with various acid mixtures or by fusion with various fluxes.
SCOPE
1.1 This practice covers dissolution treatments for uranium materials that are applicable to the test methods used for characterizing these materials for uranium elemental, isotopic, and impurities determinations. Dissolution treatments for the major uranium materials assayed for uranium or analyzed for other components are listed.  
1.2 The treatments, in order of presentation, are as follows:    
Procedure Title  
Section  
Dissolution of Uranium Metal and Oxide with Nitric Acid  
8.1  
Dissolution of Uranium Oxides with Nitric Acid and Residue
Treatment  
8.2  
Dissolution of Uranium-Aluminum Alloys in Hydrochloric Acid
with Residue Treatment  
8.3  
Dissolution of Uranium Scrap and Ash by Leaching with Nitric
Acid and Treatment of Residue by Carbonate Fusion  
8.4  
Dissolution of Refractory Uranium-Containing Material by
Carbonate Fusion  
8.5  
Dissolution of Uranium—Aluminum Alloys
Uranium Scrap and Ash, and Refractory
Uranium-Containing Materials by
Microwave Treatment  
8.6  
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. Specific hazards statements are given in Section 7.  
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.

SIGNIFICANCE AND USE
5.1 The determination of actinides by alpha spectrometry is an essential function of many environmental and other programs. Alpha spectrometry allows the identification and quantification of most alpha-emitting actinides. Although numerous separation methods are used, the final sample preparation technique has historically been by electrodeposition (Practice C1284). However, electrodeposition may have some drawbacks, such as time required, incompatibility with prior chemistry, thick deposits, and low recoveries. These problems may be minimized by using the neodymium fluoride coprecipitation method whose performance is well documented (1-6).4 To a lesser extent cerium fluoride has been used (7) but is not addressed in this practice.  
5.2 The sample mounting technique described in this practice is rapid, adds an additional purification step, since only those elements that form insoluble fluorides are mounted, and the sample and filter media can be dissolved and remounted if problems occur. The recoveries are better and resolution approaches normal in electrodeposited samples. Recoveries are sufficiently high that for survey work, if quantitative recoveries are not necessary, tracers can be omitted. Drawbacks to this technique include use of very hazardous hydrofluoric acid and the possibility of a non-reproducible and ill-defined counting geometry from filters that are not flat and may not be suitable for long retention. Also, although the total turn around time for coprecipitation may be less than for electrodeposition, coprecipitation requires more time and attention from the analyst.
SCOPE
1.1 This practice covers the preparation of separated fractions of actinides for alpha spectrometry. It is applicable to any of the actinides that can be dissolved in dilute hydrochloric acid. Examples of applicable samples would be the final elution from an ion exchange separation or the final strip from a solvent extraction separation.2  
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. For a specific hazard statement, see Section 9.  
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.

SIGNIFICANCE AND USE
5.1 This guide offers several options for the determination of 99Tc in soil samples. Sample sizes of up to 200 g are possible, depending on the method chosen to extract Tc from the soil matrix. It is up to the user to determine if it is appropriate for the intended use of the final data.
SCOPE
1.1 This guide is intended to serve as a reference for laboratories wishing to perform 99Tc analyses in soil. Several options are given for selection of a tracer and for the method of extracting the Tc from the soil matrix. Separation of Tc from the sample matrix is performed using an extraction chromatography resin. Options are then given for the determination of the 99Tc activity in the original sample. It is up to the user to determine which options are appropriate for use, and to generate acceptance data to support the chosen procedure.  
1.2 Due to the various extraction methods available, various tracers used, variable detection methods used, and lack of certified reference materials for 99Tc in soil, there is insufficient data to support a single method written as a standard method.  
1.3 The values stated in SI units are to be regarded as standard, except where the non-SI unit of molar, M, is used for the concentration of chemicals and reagents. The values given in parentheses after SI units are provided for information only and are not considered 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.

SIGNIFICANCE AND USE
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)
SCOPE
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.

SIGNIFICANCE AND USE
5.1 Factors governing selection of a method for the determination of uranium include available quantity of sample, homogeneity of material sampled, sample purity, desired level of reliability, and facility available equipment.  
5.2 This uranium assay method is referenced in the Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets (Test Methods C696) and in the Test Methods for Chemical, Mass Spectrometric, and Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions (Test Methods C799). This uranium assay method may also be used for uranium hexafluoride and uranium ore concentrate. This test method determines 20 mg to 200 mg of uranium; is applicable to product, fuel, and scrap material after the material is dissolved; is tolerant towards most metallic impurity elements usually specified in product and fuel; and uses no special equipment.  
5.3 The ruggedness of the titration method has been studied for both the volumetric (6) and the weight (7)  titration of uranium with dichromate.  
5.4 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.  
5.4.1 When used in conjunction with the appropriate certified reference materials (SRM6 or CRM), this procedure can demonstrate traceability to the national measurement base. However, use of the 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 assure that its application to safeguards has the approval of the proper regulatory authorities.
SCOPE
1.1 This test method, commonly referred to as the Modified Davies and Gray technique, covers the titration of uranium in product, fuel, and scrap materials after the material is dissolved. The test method is versatile and has been ruggedness tested. With appropriate sample preparation, this test method can give precise and unbiased uranium assays over a wide variety of material types (1, 2).2 Details of the titration procedure in the presence of plutonium with appropriate modifications are given in Test Method C1204.  
1.2 Uranium levels titrated are usually 20 mg to 50 mg, but up to 200 mg uranium can be titrated using the reagent volumes stated in this test method.  
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 safeguard and safety precaution statements, see Section 5.  
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.

SIGNIFICANCE AND USE
4.1 The test methods in this standard are designed to show whether a given material meets the specifications prescribed in Specification C967.  
4.2 Because of the variability of matrices of uranium-ore concentrate and the limited availability of suitable reference or calibration materials, the precision and bias of these test methods should be established by each individual laboratory that will use them. The precision and bias statements given for each test method are those reported by various laboratories and can be used as a guideline.  
4.3 Instrumental test methods such as X-ray fluorescence and emission spectroscopy can be used for the determination of some impurities where such equipment is available.
SCOPE
1.1 These test methods cover procedures for the chemical and atomic absorption analysis of uranium-ore concentrates to determine compliance with the requirements prescribed in Specification C967.  
1.2 The analytical procedures appear in the following order:    
Sections    
Uranium by Ferrous Sulfate Reduction—Potassium Dichromate
Titrimetry  
9    
Nitric Acid-Insoluble Uranium  
10 to 18  
Extractable Organic Material  
19 to 26  
Determination of Arsenic  
27  
Carbonate by CO2 Gravimetry  
28 to 34  
Fluoride by Ion-Selective Electrode  
35 to 42  
Halides by Volhard Titration  
43 to 50  
Phosphorus by Spectrophotometry  
52 to 60  
Determination of Silicon  
61  
Determination of Thorium  
62  
Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-
dium by Atomic Absorption Spectrophotometry  
63 to 72  
Potassium and Sodium by Atomic Absorption
Spectrophotometry  
73 to 82  
Boron by Spectrophotometry  
83 to 92  
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. A specific precautionary statement is given in Section 7.  
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.

SIGNIFICANCE AND USE
5.1 The test method within this standard is used to demonstrate uranium ore-concentrate material meets the moisture specification defined in Specification C967 or other applicable requirements.
SCOPE
1.1 This test method is used to determine compliance with Specification C967 for the requirements of moisture in uranium ore concentrates (UOC). A procedure is given to determine the approximate temperature for drying the UOC; normally 110 °C but possibly 165 °C for uranyl peroxides. The dried uranium ore-concentrate resulting from this procedure is then used for performing additional analyses described in Specification C967.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are mathematical equivalents that are provided for information only and are not considered 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.

SIGNIFICANCE AND USE
5.1 The guide is applicable to the analysis of materials to demonstrate compliance with the specifications set forth in Specifications C787 and C996. Some other specifications may be expressed in terms of mass of  232U per mass of only  238U (see ISO 21847–3:2007).
SCOPE
1.1 This guide covers the determination of  232U in uranium hexafluoride by alpha spectrometry.  
1.2 The values stated in SI units are to be regarded as standard, except where the non-SI unit of molar, M, is used for the concentration of chemicals and reagents. The unit of electronvolt (eV) is outside the SI but its use with the SI is accepted by the International Committee for Weights and Measures (CIPM, Comité International des Poids et Mesures) and the U. S. National Institute of Science and Technology (NIST). 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.

SIGNIFICANCE AND USE
5.1 Uranium material is used as a fuel in certain types of nuclear reactors. To be suitable for use as nuclear fuel, the starting material shall meet certain specifications such as those described in Specifications C753, C776, C787, C833, C967, C996, and C1008, or as specified by the purchaser. The 235U/238U isotope amount ratios and the amount content of uranium material can be measured by mass spectrometry following this test method to ensure that they meet the specification.  
5.2 The double spike method has been used for studies of uranium fractionation effects in isotope geochemistry and cosmochemistry, for uranium source attribution in nuclear forensics and for investigation of conversion or sampling processes in nuclear industry and nuclear safeguards (7-11). Most recently, the double spike method has been used for the validation of the Cristallini sampling method of UF6   (12 and 13). The double spike method can be used for a wide range of sample sizes even in samples containing as low as 50 μg of uranium. The concentration of the loading solution for the DS method has to be in the range of 1 to 6 mg/g to allow a sample loading of 4 to 6 μg of uranium. A minimum loading of 4 μg uranium per filament is recommended.  
5.3 The measurement of 236U/238U ratios using this method is not possible due to the large isobaric interference from the 236U ion beam of the double spike onto the 236U ion beam from the sample (>50.000 times for close to natural material, for example, like IRMM-184).  
5.4 The application of the double spike method for measurements of 235U/238U ratio is limited by the isobaric interference between the 236U from the double spike material and the 236U contained in the sample. As a consequence, the method is not suitable for samples which contain significant amounts of 236U due to prior neutron capture from 235U in the predecessor materials. For samples with 236U/238U ratios higher than about 10–6, the double spike method should be applied with...
SCOPE
1.1 This test method describes the determination of the isotope amount ratios of uranium material as nitrate solutions by the double spike (DS) method using a thermal ionization mass spectrometer (TIMS) instrument.  
1.2 The analytical performance in the determination of the 235U/238U major isotope amount ratio by the DS method is five to ten times better in terms of the internal and external reproducibility compared to the (“classical”) total evaporation (TE) method as described in Test Method C1672 and the “modified total evaporation” (MTE) as described in Test Method C1832. This is due to the use of an internal rather than external mass fractionation correction by using a double spike material with a known or certified 233U/236U isotope ratio, which is mixed with the sample prior to the measurement, either during the sample preparation or directly on the TIMS filament.  
1.3 The DS method cannot be applied for the determination of the 236U/238U minor isotope amount ratio, and is also not recommended for the determination of the 234U/238U minor isotope amount ratio.  
1.4 In case the uranium amount concentration of the double spike is known or certified, the uranium amount concentration of the sample can be determined using the isotope dilution mass spectrometry (IDMS) method as described in Test Method C1672, by blending the sample gravimetrically with the double spike and performing a DS measurement.  
1.5 An external mass fractionation correction by measurements of a certified reference material loaded on different filaments and measured in the same measurement sequence, as recommended for TE and required for MTE measurements, is not necessary for the DS method. However, for quality control (QC) purposes it is recommended to perform DS measurements of low enriched or natural uranium isotopic reference materials on a regular basis.  
1.6 The DS method can only be applied to uranium samples with relative isotope ...

SIGNIFICANCE AND USE
5.1 Uranium hexafluoride used to produce nuclear-reactor fuel must meet certain criteria for its isotopic composition. This test method may be used to help determine if sample materials meet the criteria described in Specifications C787 and C996.
SCOPE
1.1 This test method covers a quantitative test method applicable to determining the mass percent of uranium isotopes in uranium hexafluoride (UF6) samples. This method as described is for concentrations of  235U between 0.1 and 10 mass %, and  234U and  236U between 0.0001 and 0.1 mass %.  
1.2 This test method is for laboratory analysis by a gas mass spectrometer with a multi-collector.  
1.3 This standard complements Test Methods C761, the double-standard method for gas mass spectrometers using a single collector, by providing a method for spectrometers using a multi-collector.  
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
5.1 One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities (that is,  232Th and 238U). Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest.  
5.2 The degree of actual mass bias is variable and is dependent upon instrument tune parameters. This standard practice uses universal interference equations to derive a mass bias correction that is specific to the instrument parameters and tune used for sample data acquisition and not based on a historical average.  
5.3 Mass bias correction uses the instrument software interference equations and does not require additional subsequent off-line calculations.  
5.4 The methodology that this standard practice is based on has been used for the determination of 232Th and  237Np in enriched uranium solutions and the determination of  241Am in plutonium and uranium legacy oxides following dissolution and ion extraction chromatography separation.  
5.5 Data presented in Section 12 were developed using a quadrupole ICP-MS. This practice can also be applied to high resolution ICP-MS with appropriate validation.
SCOPE
1.1 This practice provides guidance for an alternate linear calibration for the determination of selected actinide isotopes in appropriately prepared aqueous solutions by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). This alternate calibration is mass bias adjusted using thorium-232 (232Th) and uranium-238 (238U) standards. One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities. Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest.  
1.2 The instrument response for a series of determinations of known concentration of 232Th and 238U defines the mass versus response relationship. For each standard concentration, the slope of the line defined by 232Th and  238U is used to derive linear calibration curves for each mass of interest using interference equations. The mass bias corrected calibration curves, although generated from interference equations, are specific to the instrument operating parameters and tuning in effect at the time of data acquisition. Because interference equations are part of the normal ICP-MS manufacturer's software package, this calibration methodology is widely applicable.  
1.3 For this standard practice, the actinide atomic mass range that has been studied is from AMU 232 to 244. Guidance for an extended range of AMU 228 to 248 is given in this practice.  
1.4 Using this practice, analyte concentrations are reported at each AMU and not by element total (that is, 239Pu versus 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, 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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
5.1 This test method is designed to determine whether a given material meets the purchaser's specification for plutonium content. This method may also be used, with sufficient qualification, for process control or accountability measurements associated with nuclear materials processing.
SCOPE
1.1 This test method describes the determination of total plutonium as plutonium(III) in nitrate and chloride solutions. The technique is applicable to solutions resulting from plutonium dioxide powders and pellets (Test Methods C697), nuclear grade mixed oxides (Test Methods C698), plutonium metal (Test Methods C758), and plutonium nitrate solutions (Test Methods C759). Solid samples are dissolved using the appropriate dissolution techniques described in Practice C1168. The use of this technique for other plutonium-bearing materials has been reported (1-6),2 but final determination of applicability must be made by the user. The applicable concentration range for plutonium sample solutions is 10 to 200 g Pu/L.
Note 1: As directly measured in the spectrophotometer, concentrations will be approximately 0.8 to 4.0 g Pu/L. Sample solutions are diluted to reach this target range. For solid samples, select the sample size and dissolved solution weight to yield sample solutions in the 10 to 30 g Pu/L range. With special preparation and spectral analysis techniques, the method has been applied to nitrate solutions in the 0.1 to 10 g Pu/L range.  
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.

SIGNIFICANCE AND USE
5.1 Uranium hexafluoride is normally produced and handled in large (typically 1- to 14-ton) quantities and must, therefore be characterized by reference to representative samples. The samples are used to determine compliance with the applicable commercial Specifications C996 and C787 by means of the appropriate test method (for example, Test Method C761 and references therein). The quantities involved, physical properties, chemical reactivity, and hazardous nature of UF6 are such that for representative sampling, specially designated equipment must be used and operated in accordance with the most carefully controlled and stringent procedures. This practice indicates appropriate principles, equipment and procedures currently in use for subsampling of liquid UF6. It is used by UF6 converters, enrichers and fuel fabricators to review the effectiveness of existing procedures or to design equipment and procedures for future use. Other subsampling procedures such as UF6 vapor sampling are not directly representative of the chemical quality of liquid UF6.  
5.2 It is emphasized that this test guide is not meant to address conventional or nuclear criticality safety issues, nor does it address the conditioning of subsample tubes to make them suitable for transport.
SCOPE
1.1 This practice is applicable to subsampling uranium hexafluoride (UF6), using heat liquefaction techniques, from bulk containers, obtained in conformance with Practices C1052, C1703, and C1883, into smaller sample containers, which are required for laboratory analyses.  
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 It is assumed that the liquid UF6 being sampled comprises a single quality and quantity of material. This practice does not address any special additional arrangement that might be required for taking proportional or composite samples.  
1.4 The number of samples to be taken, their nominal sample weight, and their disposition shall be agreed upon between the parties.  
1.5 The scope of this practice does not include provisions for preventing criticality incidents.  
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.  
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
5.1 This test method provides the speed and high decontamination factors attainable with liquid-liquid extraction of the actinides and eliminates filtration techniques that are more time consuming.  
5.2 This test method provides a precise determination of americium in concentrations normally found in environmental samples.
SCOPE
1.1 This test method covers the determination of 241Am in soil by means of chemical separations and alpha spectrometry. It is designed to analyze up to 10 g of soil or other sample matrices that contain up to 30 mg of combined rare earths. This test method allows the determination of 241Am concentrations from ambient levels to applicable standards.  
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.

SIGNIFICANCE AND USE
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, respecti...
SCOPE
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.

SIGNIFICANCE AND USE
5.1 This test method is useful for the determination of concentrations of metals in many waste streams from various nuclear and non-nuclear manufacturing processes. The test method is useful for characterizing liquid wastes and liquid wastes containing undissolved solids prior to treatment, storage, or stabilization. It has the capability for the simultaneous determination of up to 26 elements.  
5.2 The applicable concentration ranges of the elements analyzed by this procedure are listed in Table 1.
SCOPE
1.1 This test method covers the determination of trace, minor, and major elements in waste streams by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) following an acid digestion of the sample. Waste streams from manufacturing processes of nuclear and non-nuclear materials can be analyzed. This test method is applicable to the determination of total metals. Results from this test method can be used to characterize waste received by treatment facilities and to formulate appropriate treatment recipes. The results are also usable in process control within waste treatment facilities.  
1.2 This test method is applicable only to waste streams that contain radioactivity levels that do not require special personnel or environmental protection.  
1.3 A list of the elements determined in waste streams and the corresponding lower reporting limit is found in Table 1.  
1.4 This test method has been used successfully for treatment of a large variety of waste solutions and industrial process liquids. The composition of such samples is highly variable, both between waste stream types and within a single waste stream. As a result of this variability, a single acid digestion scheme may not be expected to succeed with all sample matrices. Certain elements may be recovered on a semi-quantitative basis, while most results will be highly quantitative.  
1.5 This test method should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction.  
1.6 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.  
1.7 This test method contains notes that are explanatory and are not part of the mandatory requirements of the method.  
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.9 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.  
1.10 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.

SIGNIFICANCE AND USE
5.1 Because soil is an integrator and a reservoir of long-lived radionuclides, and serves as an intermediary in several pathways of potential exposure to humans, knowledge of the concentration of 90Sr in soil is essential. 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, may not be able to assess small incremental releases.
SCOPE
1.1 This test method is applicable to the determination of 90Sr in soil at levels of detection dependent on count time, sample size, detector efficiency, background, and chemical yield.  
1.2 This test method is designed for the analysis of 10 g of soil, previously collected and treated as described in Practices C998 and C999. This test method may not be able to completely dissolve all soil matrices.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
5.1 This test method is used to analyze soil for alpha-emitting uranium isotopes. It can be used to establish baseline uranium levels and to monitor depositions from nuclear facilities.
SCOPE
1.1 This test method covers the determination of alpha-emitting uranium isotopes in soil. This test method describes one acceptable approach to the determination of uranium isotopes in soil.2  
1.2 The test method is designed to analyze 10 g of soil. This test method may not be able to completely dissolve all forms of uranium in the soil matrix. Studies have indicated that the use of hydrofluoric acid to dissolve soil has resulted in lower values than results using total dissolution by fusion.  
1.3 The lower limit of detection is dependent on count time, sample size, detector, background, and tracer yield. The chemical yield averaged 78 % in a single laboratory evaluation, and 66 % in an interlaboratory collaborative study.  
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
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. Specific precautionary statements are given in Section 11.  
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.

SIGNIFICANCE AND USE
4.1 Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, 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 Specifications C753 and C776.  
4.1.1 An assay is performed to determine whether the material has the minimum uranium content specified on a dry weight basis.  
4.1.2 The stoichiometry of the oxide powder is useful for predicting its sintering behavior in the pellet production process.  
4.1.3 Determination of the isotopic content of the uranium in the uranium dioxide powder is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.  
4.1.4 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).  
4.1.5 Determination of the oxygen-to-uranium ratio is performed on the completed pellets to determine whether they have the appropriate stoichiometry for optimal performance during irradiation.
SCOPE
1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets to determine compliance with specifications.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.3 The analytical procedures appear in the following order:
Sections  
Uranium by Ferrous Sulfate Reduction in Phosphoric Acid and Dichromate Titration Method  
2  
Uranium and Oxygen Uranium Atomic Ratio by the Ignition (Gravimetric) Impurity Correction Method  
3  
Carbon (Total) by Direct Combustion-Thermal Conductivity Method  
2  
Total Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method  
3    
Moisture by the Coulometric, Electrolytic Moisture Analyzer Method  
8 – 15    
Nitrogen by the Kjeldahl Method  
16 – 23    
Isotopic Uranium Composition by Multiple-Filament Surface Ionization Mass Spectrometric Method  
4  
Spectrochemical Determination of Trace Elements in High-Purity Uranium Dioxide  
5  
Silver, Spectrochemical Determination of, by Gallium Oxide Carrier D-C Arc Technique  
5    
Rare Earths by Copper Spark-Spectrochemical Method  
2  
Impurity Elements by a Spark-Source Mass Spectrographic Method  
2  
Surface Area by Nitrogen Absorption Method  
24 – 30    
Total Gas in Reactor-Grade Uranium Dioxide Pellets  
2  
Thorium and Rare Earth Elements by Spectroscopy  
2  
Hydrogen by Inert Gas Fusion  
3    
Uranium Isotopic Analysis by Mass Spectrometry  
2  
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.

SIGNIFICANCE AND USE
5.1 This test method is used to detect possible exposures to uranium isotopes from occupational operations that may result in elimination via the urinary tract.
SCOPE
1.1 This test method is applicable to the determination of uranium in urine at levels of detection dependent on sample size, count time, detector background, and tracer yield. It is designed as a screening tool for detection of possible exposure of occupational workers.  
1.2 This test method is designed for 50 mL of urine. This test method does not address the sampling protocol or sample preservation methods associated with its use.  
1.3 Test Method C1844 offers an alternative method for the analysis of uranium in urine using ICP-MS detection.  
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. A specific precautionary statement is given in Section 9.  
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.

SIGNIFICANCE AND USE
5.1 This method is capable of measuring the concentration of boron, silicon, and technetium in UF6. Limits for these contaminants are set in Specifications C787 and C996.
SCOPE
1.1 This test method covers the determination of boron, silicon, and technetium in hydrolyzed uranium hexafluoride (UF6) by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) after separation of the uranium by solid phase extraction.  
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. Some specific hazards statements are given in Section 7 on Hazards.  
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.

SIGNIFICANCE AND USE
5.1 The test method is capable of measuring uranium isotopic abundances of 234U, 235U, 236U, and 238U as required by Specifications C787 and C996.
SCOPE
1.1 This test method covers the isotopic abundance analysis of 234U, 235U, 236U, and 238U in samples of hydrolysed uranium hexafluoride (UF6) by inductively coupled plasma source, multicollector, mass spectrometry (ICP-MC-MS). The method applies to material with  235U abundance in the range of 0.2 to 6 % mass. This test method is also described in ASTM STP 1344.  
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
4.1 The test methods in this method are designed to show whether a given material is in accordance with Specification C922.
SCOPE
1.1 These test methods cover procedures for the analysis of sintered gadolinium oxide-uranium dioxide pellets to determine compliance with specifications.  
1.2 The analytical procedures appear in the following order:    
Section  
Carbon (Total) by Direct Combustion—Thermal Conductivity Method  
2  
C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method  
3  
Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method  
4  
C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide  
3  
Gadolinia Content by Energy-Dispersive X-Ray Spectrometry  
4  
C1456 Test Method for Determination of Uranium or Gadolinium (or both) in Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray Fluorescence (XRF)  
3  
Hydrogen by Inert Gas Fusion  
4  
C1457 Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction  
3  
Isotopic Uranium Composition by Multiple-Filament Surface-Ionization Mass Spectrometric Method  
2  
C1413 Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride And Uranyl Nitrate Solutions By Thermal Ionization Mass Spectrometry  
3  
C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis  
3  
Nitrogen by Distillation—Nessler Reagent (Photometric) Method  
7 to 17  
Oxygen-to-Metal Ratio of Sintered Gadolinium Oxide-Uranium Dioxide Pellets  
4  
C1430 Test Method for Determination of Uranium, Oxygen to Uranium (O/U), and Oxygen to Metal (O/M) in Sintered Uranium Dioxide and Gadolinia-Uranium Dioxide Pellets by Atmospheric Equilibration  
3  
Spectrochemical Determination of Trace Impurity Elements  
4  
C1517 Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission Spectroscopy  
3  
Total Gas by Hot Vacuum Extraction  
2  
Ceramographic Determination of Free Gd2O3 and Free UO2 to Estimate the Homogeneity of (U,Gd)O2 Pellets  
18 to 25  
Ceramographic Determination of Average Grain Size by Linear Intercept after Chemical Etching  
26 to 33  
1.3 The values stated in SI units are to be regarded as 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.

SIGNIFICANCE AND USE
5.1 The test method is designed to show whether or not a material meets the specifications as given in Specifications C753 or C776.  
5.2 The powder’s stoichiometry is useful for predicting the oxide's sintering behavior in the pellet production process.
SCOPE
1.1 This test method covers the determination of uranium and the oxygen to uranium atomic ratio in nuclear grade uranium dioxide powder and pellets.  
1.2 This test method does not include provisions for preventing criticality accidents or requirements for health and safety. Observance of this test method does not relieve the user of the obligation to be aware of and conform to all international, national, or federal, state and local regulations pertaining to possessing, shipping, processing, or using source or special nuclear material.  
1.3 This test method also is applicable to UO3 and U3O8 powder.  
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.

SIGNIFICANCE AND USE
4.1 Uranyl nitrate solution is used as a feed material for conversion to the hexafluoride as well as for direct conversion to the oxide. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, isotopic composition, acidity, radioactivity, and impurity content. These methods are designed to show whether a given material meets the specifications for these items described in Specification C788.  
4.1.1 An assay is performed to determine whether the material has the specified uranium content.  
4.1.2 Determination of the isotopic content of the uranium is made to establish whether the effective fissile content is in accordance with the purchaser’s specifications.  
4.1.3 Acidity, organic content, and alpha, beta, and gamma activity are measured to establish that they do not exceed their maximum limits.  
4.1.4 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded. Impurity concentrations are also required for calculation of the equivalent boron content (EBC), and the total equivalent boron content (TEBC).
SCOPE
1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solution to determine compliance with specifications.  
1.2 The analytical procedures appear in the following order:    
Sections  
Determination of Uranium  
8  
Specific Gravity by Pycnometry  
16 – 21  
Free Acid by Oxalate Complexation  
22 – 28  
Determination of Thorium  
29  
Determination of Chromium  
30  
Determination of Molybdenum  
31  
Halogens Separation by Steam Distillation  
32 – 36  
Fluoride by Specific Ion Electrode  
37 – 43  
Halogen Distillate Analysis: Chloride, Bromide, and Iodide by
Amperometric Microtitrimetry  
44  
Determination of Chloride and Bromide  
45  
Determination of Sulfur by X-Ray Fluorescence  
46  
Sulfate Sulfur by (Photometric) Turbidimetry  
47  
Phosphorus by the Molybdenum Blue (Photometric) Method  
55 – 62  
Silicon by the Molybdenum Blue (Photometric) Method  
63 – 70  
Carbon by Persulfate Oxidation-Acid Titrimetry  
71  
Conversion to U3O8  
72 – 75  
Boron by Emission Spectrography  
A  
Impurity Elements by Spark Source Mass Spectrography  
77  
Isotopic Composition by Thermal Ionization Mass Spectrometry  
78  
Uranium-232 by Alpha Spectrometry  
79 – 85  
Total Alpha Activity by Direct Alpha Counting  
86 – 92  
Fission Product Activity by Beta Counting  
93 – 99  
Entrained Organic Matter by Infrared Spectrophotometry  
100  
Fission Product Activity by Gamma Counting  
101  
Determination of Arsenic  
102  
Determination of Impurities for the EBC Calculation  
103  
Determination of Technetium 99  
104  
Determination of Plutonium and Neptunium  
105  
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.  Specific precautionary statements are given in 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.

SIGNIFICANCE AND USE
5.1 Uranium hexafluoride is a basic material used to prepare nuclear reactor fuel. To be suitable for this purpose the material must meet criteria for uranium content, isotopic composition and metallic impurities in Specification C787 and C996. This practice results in the complete dissolution of the sample for uranium and impurities analysis, and determination of isotopic distribution by mass spectrometry as described in, for example, Test Methods C761.
SCOPE
1.1 This practice covers the dissolution of UF6 from a P-10 tube to provide solutions for analysis.  
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. For specific safeguard and safety precaution statements, see Section 9.  
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.

ABSTRACT
These practices cover three standard technique for dissolving glass samples containing radioactive, nuclear, and mixed wastes. These techniques used together or independently will produce solutions that can be analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), atomic absorption spectrometry (AAS), radiochemical methods and wet chemical techniques for major components, minor components and radionuclides. The practices for dissolving silicate matrix samples each require the sample to be initially dried and ground to a fine powder. The first practice involves the mixing and fusion of the sample with sodium tetraborate (Na2B4O7) and sodium carbonate (Na2CO4) in a muffle for a given amount of time and temperature. The sample is then cooled, dissolved in hydrochloric acid, and diluted to appropriate volume for analyses. The second practice, on the other hand, involves the fusion of the sample with potassium hydroxide (KOH) or sodium peroxide (Na2O2) using an electric bunsen burner, dissolving the fused sample in water and dilute HCl, and making to volume for analyses. Finally, the third practice involves the dissolution of the sample using a microwave oven. The ground sample is digested in a microwave oven using a mixture of hydrofluoric (HF) and nitric (HNO3) acids. Boric acid is added to the resulting solution to complex excess fluoride ions.
SCOPE
1.1 These practices cover techniques suitable for dissolving glass samples that may contain nuclear wastes. These techniques used together or independently will produce solutions that can be analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), atomic absorption spectrometry (AAS), radiochemical methods and wet chemical techniques for major components, minor components and radionuclides.  
1.2 One of the fusion practices and the microwave practice can be used in hot cells and shielded hoods after modification to meet local operational requirements.  
1.3 The user of these practices must follow radiation protection guidelines in place for their specific laboratories.  
1.4 Additional information relating to safety is included in the text.  
1.5 The dissolution techniques described in these practices can be used for quality control of the feed materials and the product of plants vitrifying nuclear waste materials in glass.  
1.6 These practices are introduced to provide the user with an alternative means to Test Methods C169 for dissolution of waste containing glass in shielded facilities. Test Methods C169 is not practical for use in such facilities and with radioactive materials.  
1.7 The ICP-AES methods in Test Methods C1109 and C1111 can be used to analyze the dissolved sample with additional sample preparation as necessary and with matrix effect considerations. Additional information as to other analytical methods can be found in Test Method C169.  
1.8 Solutions from this practice may be suitable for analysis using ICP-MS after establishing laboratory performance criteria and verification that the criteria can be met. For example, Test Methods C1287 or C1637 may be used with additional sample preparation as necessary and appropriate matrix effect considerations.  
1.9 The values stated in SI units are to be regarded as standard. Units in parentheses are for information only.  
1.10 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 Sections 10, 20, and 30.  
1.11 This international standard was developed in accordance with internationally recognized principles on standardization established in the De...

SIGNIFICANCE AND USE
5.1 Nuclear-grade reactor fuel material must meet certain criteria, such as those described in Specifications C753, C776, C778, and C833. Included in these criteria is the uranium isotopic composition. This test method is designed to demonstrate whether or not a given material meets an isotopic requirement and whether the effective fissile content is in compliance with the purchaser's specifications.
SCOPE
1.1 This test method is applicable to the determination of the isotopic composition of uranium (U) in nuclear-grade fuel material. The following isotopic weight percentages are determined using a quadrupole inductively coupled plasma-mass spectrometer (Q-ICP-MS):  233U,  234U,  235U,  236U, and  238U. The analysis can be performed on various material matrices after acid dissolution and sample dilution into water or dilute nitric (HNO3) acid. These materials include: fuel product, uranium oxide, uranium oxide alloys, uranyl nitrate (UNH) crystals, and solutions. The sample preparation discussed in this test method focuses on fuel product material but may be used for uranium oxide or a uranium oxide alloy. Other preparation techniques may be used and some references are given. Purification of the uranium by anion-exchange extraction is not required for this test method, as it is required by other test methods such as radiochemistry and thermal ionization mass spectroscopy (TIMS). This test method is also described in ASTM STP 13442.  
1.2 The  233U isotope is primarily measured as a qualitative measure of its presence by comparing the  233U peak intensity to a background point since it is not normally found present in materials. The example data presented in this test method do not contain any  233U data. A  233U enriched standard is given in Section 8, and it may be used as a quantitative spike addition to the other standard materials listed.  
1.3 A single standard calibration technique is used. Optimal accuracy (or a low bias) is achieved through the use of a single standard that is closely matched to the enrichment of the samples. The intensity or concentration is also adjusted to within a certain tolerance range to provide good statistical counting precision for the low-abundance isotopes while maintaining a low bias for the high-abundance isotopes, resulting from high-intensity dead time effects. No blank subtraction or background correction is utilized. Depending upon the standards chosen, enrichments between depleted and 97 % can be quantified. The calibration and measurements are made by measuring the intensity ratios of each low-abundance isotope to the intensity sum of  233U,  234U,  235U,  236U, and  238U. The high-abundance isotope is obtained by difference.  
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only. The instrument is calibrated and the samples measured in units of isotopic weight percent (Wt %). For example, the  235U enrichment may be stated as Wt %  235U or as g  235U/100 g of U. Statements regarding dilutions, particularly for μg/g concentrations or lower, are given assuming a solution density of 1.0 since the uranium concentration of a solution is not important when making isotopic ratio measurements other than to maintain a reasonably consistent intensity within a tolerance range.  
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. Specific precautionary statements are given in Section 9.  
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 ...

SIGNIFICANCE AND USE
5.1 Uranium hexafluoride used to produce nuclear fuel must meet certain criteria for its isotopic composition as described in Specifications C787 and C996.
SCOPE
1.1 This method applies to the determination of isotopic composition in hydrolyzed nuclear grade uranium hexafluoride. It covers isotopic abundance of 235U between 0.1 and 5.0 % mass fraction, abundance of 234U between 0.0055 and 0.05 % mass fraction, and abundance of  236U between 0.0003 and 0.5 % mass fraction. This test method may be applicable to other isotopic abundance providing that corresponding standards are available.  
1.2 This test method can apply to uranyl nitrate solutions. This can be achieved either by transforming the uranyl nitrate solution to a uranyl fluoride solution prior to the deposition on the filaments or directly by depositing the uranyl nitrate solution on the filaments. In the latter case, a calibration with uranyl nitrate standards must be performed.  
1.3 This test method can also apply to other nuclear grade matrices (for example, uranium oxides) by providing a chemical transformation to uranyl fluoride or uranyl nitrate solution.  
1.4 Units—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.

SIGNIFICANCE AND USE
5.1 This test method is applicable to samples containing 1 to 10 % gadolinium oxide and 90 to 99 % uranium oxide on the “as received” basis. The method may be used to determine concentration of either uranium, gadolinium, or both.  
5.2 Either wavelength-dispersive or energy-dispersive X-ray fluorescence systems may be used provided the software accompanying the system is able to accommodate the use of internal standards.
SCOPE
1.1 This test method describes the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of gadolinium or uranium (or both) in gadolinium oxide-uranium oxide pellets or powders.  
1.2 This test method requires the use of appropriate internal standard(s). Care must be taken to ascertain that samples analyzed by this method do not contain the internal standard element(s) or that this contamination has been corrected for mathematically whenever present. Such corrections are not addressed in this test method.  
1.3 This standard contains notes that are explanatory and are not part of the mandatory requirements of the standard.  
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. Specific precautions are given in Section 8 and various notes throughout the method.  
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.

SIGNIFICANCE AND USE
5.1 Plutonium oxide powder is a component of MOX fuel. This test method can be used to determine whether the carbon and sulfur contents of the PuO2 powder meets the requirements of Specifications C757 and C753 or other requirements as defined by agreement between the nuclear and fuel supplier and the customer.  
5.2 MOX is used as a nuclear-reactor fuel. To be used as a fuel, MOX materials must meet specifications on the impurity element contents in them. Examples of these requirements are given in Specification C833.  
5.3 This method is suitable for pure plutonium oxide powder.
SCOPE
1.1 This test method is for the determination of the carbon and sulfur contents in plutonium oxide (PuO2) powder. The method utilizes an induction furnace purged with oxygen for combustion of the sample. Carbon dioxide and sulfur dioxide produced by the combustion are swept into absorption cells and quantified by infrared absorption spectrophotometers. This test method is an alternative to the methods for carbon and sulfur given in Test Method C697.  
1.2 Determination of the carbon and sulfur contents in nuclear-grade sintered mixed oxide (MOX) fuel pellets requires the use of larger samples and is addressed in Test Method C1853.  
1.3 The values stated in SI units are to be regarded as standard. Units of measurement in parentheses are included for information only.  
1.4 This standard may involve hazardous materials, operations, and equipment. 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.

SIGNIFICANCE AND USE
5.1 This test method is applicable to aqueous solutions of uranium containing 0.05 to 20 g uranium per litre of solution presented to the spectrometer.  
5.2 Either wavelength-dispersive or energy-dispersive X-ray fluorescence systems may be used provided the software accompanying the system is able to accommodate the use of internal standards.
SCOPE
1.1 This test method covers the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of mineral acid solutions containing uranium.  
1.2 This test method is valid for those solutions containing 0.05 to 20 g uranium/L as presented to the spectrometer. Higher concentrations may be covered by appropriate dilutions.  
1.3 The values stated in SI units are to be regarded as 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. Specific precautionary statements are given in Section 9 and Note 1.  
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.