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ASTM E402-02

(Test Method)

Standard Test Method for Spectrographic Analysis of Uranium Oxide (U3O8)by Gallium Oxide-Carrier Technique (Withdrawn 2007)

Standard Test Method for Spectrographic Analysis of Uranium Oxide (U<sub>3</sub>O<sub>8</sub>)by Gallium Oxide-Carrier Technique (Withdrawn 2007)

SCOPE
1.1 This test method covers the semiquantitative spectrographic analysis of high-purity U3O8 for the 32 elements in the ranges indicated in Table 1. (Quantitative analyses of boron, chromium, iron, magnesium, manganese, nickel, and other impurities can be performed using densitometric methods.)
1.2 The test method can be applied to those samples of uranium and uranium compounds, or both, which can be converted to the black oxide (U3O8) and which are of approximately 99.5 % purity or better.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method covers the semiquantitative spectrographic analysis of high-purity U3O8 for the 32 elements in the ranges indicated in Table 1.
Formerly under the jurisdiction of Committee E01 of Analytical Chemistry for Metals, Ores, and Related Materials, this test method was withdrawn in June 2007.

General Information

Status
Withdrawn
Publication Date
09-Oct-2002
Withdrawal Date
10-Jun-2007
ICS
27.120.30 - Fissile materials and nuclear fuel technology
Technical Committee
E01 - Analytical Chemistry for Metals, Ores, and Related Materials
Drafting Committee
E01.02 - Ores, Concentrates, and Related Metallurgical Materials
Current Stage
Ref Project

Relations

Replaces
ASTM E402-95 - Standard Test Method for Spectrographic Analysis of Uranium Oxide (U<sub>3</sub>O<sub>8</sub>)by Gallium Oxide-Carrier Technique
Effective Date
10-Oct-2002

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ASTM E402-02 - Standard Test Method for Spectrographic Analysis of Uranium Oxide (U<sub>3</sub>O<sub>8</sub>)by Gallium Oxide-Carrier Technique (Withdrawn 2007)ASTM E402-02 - Standard Test Method for Spectrographic Analysis of Uranium Oxide (U<sub>3</sub>O<sub>8</sub>)by Gallium Oxide-Carrier Technique (Withdrawn 2007)
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ASTM E402-02 - Standard Test Method for Spectrographic Analysis of Uranium Oxide (U<sub>3</sub>O<sub>8</sub>)by Gallium Oxide-Carrier Technique (Withdrawn 2007)
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please
contact ASTM International (www.astm.org) for the latest information.
Designation: E 402 – 02
Standard Test Method for
Spectrographic Analysis of Uranium Oxide (U O )by
3 8
1
Gallium Oxide-Carrier Technique
This standard is issued under the fixed designation E402; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope the comparison standards. The sample is mixed with pure
gallium sesquioxide (Ga O ) in the ratio of 98 parts U O to 2
1.1 This test method covers the semiquantitative spectro- 2 3 3 8
parts Ga O . If densitometric determinations are desired, the
2 3
graphicanalysisofhigh-purityU O forthe32elementsinthe
3 8
Ga O used in the mixture contains 1% chromium or 1%
ranges indicated in Table 1. (Quantitative analyses of boron, 2 3
cobaltbyweight.Thechromiumorcobaltisusedasaninternal
chromium, iron, magnesium, manganese, nickel, and other
standard element in the spectrochemical analysis. The U O -
impurities can be performed using densitometric methods.) 3 8
Ga O mixture is placed in a special cupped electrode and
2 3
1.2 The test method can be applied to those samples of
excited in a d-c arc. Varying amounts of impurities either in
uranium and uranium compounds, or both, which can be
vapor form or as solid particles are carried up into the arc
converted to the black oxide (U O ) and which are of approxi-
3 8
stream, along with the vaporized Ga O , for excitation. The
mately 99.5% purity or better. 2 3
spectrum is recorded on a photographic plate and the selected
1.3 This standard does not purport to address all of the
lines are either visually compared with standard plates or
safety concerns, if any, associated with its use. It is the
photometrically measured and compared with synthetically
responsibility of the user of this standard to establish appro-
prepared standards according to standard spectrochemical
priate safety and health practices and determine the applica-
procedures.
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents
5.1 Impurities in the uranium used as fuel for nuclear
2.1 ASTM Standards:
reactors may affect the nuclear chain reaction. Their concen-
E115 Practice for Photographic Processing in Optical
2
trations must be closely controlled. This method provides a
Emission Spectrographic Analysis
technique for their determination.
E116 Practice for Photographic Photometry in Spectro-
2
chemical Analysis
6. Apparatus
E130 Practice for Designation of Shapes and Sizes of
2 6.1 Sample Preparation Equipment:
Graphite Electrodes
6.1.1 Sample-Carrier Mixers, either a highly polished agate
E135 Terminology Relating to Analytical Chemistry for
2 mortar and pestle, or a clean plastic capsule with a plastic ball
Metals, Ores, and Related Materials
and a mechanical mixer.
3. Terminology 6.2 Balances, torsion type, with capacities up to 1000 mg,
capable of weighing 60.1 mg accurately. When samples are
3.1 Fordefinitionsoftermsusedinthistestmethod,referto
hand ground it may be necessary to have a balance capacity of
Terminology E135.
2.500 g.
4. Summary of Test Method
6.3 Muffle Furnace, capable of 1000°C.
6.4 Excitation Source, capable of providing a 14-A d-c arc
4.1 The as-received sample is ignited to U O . It is impor-
3 8
(short-circuit).
tant that the sample be in the same physical oxide form as are
6.5 Excitation Stand, conventional type with adjustable
water cooled electrode holders.
1
This test method is under the jurisdiction of ASTM Committee E01 on
6.6 Spectrograph,grating,providingpreexposureandexpo-
Analytical Chemistry for Metals, Ores and Related Materials and is the direct
˚
sure timers, wavelength coverage from 2250 to 8650 A,a
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
˚
reciprocal linear dispersion of at least 5 A/mm and sufficient
lurgical Materials.
˚
Current edition approved October 10, 2002. Published June 2003. Originally resolving power to separate cadmium 2288.02 A from arsenic
approved in 1970. Last previous edition approved in 1995 as 402–95. ˚
2288.12 A.
2
Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please
contact ASTM International (www.astm.org) for the latest information.
E402–02
A
TABLE 1 Elements and Analytical Ranges
Concentration Range, Concentration Range, Concentration Range,
Element Element Element
ppm ppm ppm
Antimony 1 to 200 Arsenic 10 to 200 Gold 1 to 100
Beryllium 1 to
...

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1.1 This test method covers the semiquantitative spectrographic analysis of high-purity U O  for the 32 elements in the ranges indicated in Table 1. (Quantitative analyses of boron, chromium, iron, magnesium, manganese, nickel, and other impurities can be performed using densitometric methods.)  
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FIG. 1 27Al(n,α)24Na Cross Section, from IRDFF-II Library, with EXFOR Experimental Data  
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This specification covers finished sintered and ground (uranium-plutonium) dioxide pellets for use in thermal reactors. It applies to uranium-plutonium dioxide pellets containing plutonium additions up to 15 % weight. The diversity of manufacturing methods shall be recognized by which uranium-plutonium dioxide pellets are produced and the many special requirements for chemical and physical characterization that may be imposed by the operating conditions to which the pellets will be subjected in specific reactor systems. The following are different chemical requirements that shall be determined: uranium content, plutonium content, impurity content, stoichiometry, moisture content, gas content, and americium-241 content. Nuclear requirements such as isotopic content, plutonium equivalent at a given date, equivalent boron content, and reactivity shall also be determined. Physical properties of the pellets like dimensions, density, grain size, pore morphology, plutonium-oxide homogeneity, plutonium-oxide particle size, plutonium-oxide particle distribution, integrity, and surface cracks shall be determined as well. The surfaces of finished pellets shall be visually free of loose chips, oil, macroscopic inclusions, and foreign materials. An estimate of the fuel pellet irradiation stability shall be obtained unless adequate allowance for such effects are factored into the fuel rod design. The estimate of the stability shall consist of either conformance to the thermal stability test as specified in the or by adequate correlation of manufacturing process or microstructure to in-reactor behavior, or both.
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1.1 This terminology standard contains terms, definitions, descriptions of terms, nomenclature, and explanations of acronyms and symbols specifically associated with standards under the jurisdiction of Committee C26 on Nuclear Fuel Cycle. The content of this terminology standard may also be applicable to documents not under the jurisdiction of Committee C26, in which case this terminology standard may be referenced in those documents.  
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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.

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ASTM
ASTM C1455-14(2023)(Test Method)
Standard Test Method for Nondestructive Assay of Special Nuclear Material Holdup Using Gamma-Ray Spectroscopic Methods

SIGNIFICANCE AND USE
5.1 Measurement results from this test method assists in demonstrating regulatory compliance in such areas as safeguards SNM inventory control, criticality control, waste disposal, and decontamination and decommissioning (D&D). This test method can apply to the measurement of holdup in process equipment or discrete items whose gamma-ray absorption properties may be measured or estimated. This method may be adequate to accurately measure items with complex distributions of radioactive and attenuating material, however, the results are subject to larger measurement uncertainties than measurements of less complex distributions of radioactive material.  
5.2 Scan—A scan is used to provide a qualitative indication of the extent, location, and the relative quantity of holdup. It can be used to plan or supplement the quantitative measurements.  
5.3 Nuclide Mapping—Nuclide mapping measures the relative isotopic composition of the holdup at specific locations. It can also be used to detect the presence of radionuclides that emit radiation which could interfere with the assay. Nuclide mapping is best performed using a high resolution detector (such as HPGe) for best nuclide and interference detection. If the holdup is not isotopically homogeneous at the measurement location, that measured isotopic composition will not be a reliable estimate of the bulk isotopic composition.  
5.4 Quantitative Measurements—These measurements result in quantification of the mass of the measured nuclides in the holdup. They include all the corrections, such as attenuation, and descriptive information, such as isotopic composition, that are available  
5.4.1 High quality results require detailed knowledge of radiation sources and detectors, transmission of radiation, calibration, facility operations and error analysis. Judicious use of subject matter experts is required (Guide C1490).  
5.5 Holdup Monitoring—Periodic re-measurement of holdup at a defined point using the same technique and a...
SCOPE
1.1 This test method describes gamma-ray methods used to nondestructively measure the quantity of 235U or  239Pu present as holdup in nuclear facilities. Holdup may occur in any facility where nuclear material is processed, in process equipment, in exhaust ventilation systems and in building walls and floors.  
1.2 This test method includes information useful for management, planning, selection of equipment, consideration of interferences, measurement program definition, and the utilization of resources  (1, 2, 3, 4) .2  
1.3 The measurement of nuclear material hold up in process equipment requires a scientific knowledge of radiation sources and detectors, transmission of radiation, calibration, facility operations and uncertainty analysis. It is subject to the constraints of the facility, management, budget, and schedule; plus health and safety requirements. The measurement process includes defining measurement uncertainties and is sensitive to the form and distribution of the material, various backgrounds, and interferences. The work includes investigation of material distributions within a facility, which could include potentially large holdup surface areas. Nuclear material held up in pipes, ductwork, gloveboxes, and heavy equipment, is usually distributed in a diffuse and irregular manner. It is difficult to define the measurement geometry, to identify the form of the material, and to measure it without interference from adjacent sources of radiation.  
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...

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