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ASTM C1000-05

(Test Method)

Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry

Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry

SIGNIFICANCE AND USE
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.
1.2 The test method is designed to analyze 10 g of soil; however, the sample size may be varied to 50 g depending on the activity level. 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 efficiency, background, and tracer yield. The chemical recovery averaged 78 % in a single laboratory evaluation, and 66 % in an interlaboratory collaborative study.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. A specific precautionary statement is given in Section 10.

General Information

Status
Historical
Publication Date
31-May-2005
ICS
17.240 - Radiation measurements
Technical Committee
C26 - Nuclear Fuel Cycle
Drafting Committee
C26.05 - Methods of Test
Current Stage
Ref Project

Relations

Replaces
ASTM C1000-00 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry
Effective Date
01-Jun-2005
Replaced By
ASTM C1000-11 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry
Effective Date
01-Feb-2011
Referred By
ASTM C1475-17 - Standard Guide for Determination of Neptunium-237 in Soil
Effective Date
01-Jun-2005
Referred By
ASTM C1473-19 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Urine by Alpha Spectrometry
Effective Date
01-Jun-2005
Referred By
ASTM E1893-15(2021) - Standard Guide for Selection and Use of Portable Radiological Survey Instruments for Performing In Situ Radiological Assessments to Support Unrestricted Release from Further Regulatory Controls
Effective Date
01-Jun-2005

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ASTM C1000-05 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha SpectrometryASTM C1000-05 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry
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ASTM C1000-05 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:C1000–05
Standard Test Method for
Radiochemical Determination of Uranium Isotopes in Soil by
1
Alpha Spectrometry
This standard is issued under the fixed designation C1000; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope C999 Practice for Soil Sample Preparation for the Determi-
nation of Radionuclides
1.1 This test method covers the determination of alpha-
C1163 Practice for Mounting Actinides for Alpha Spec-
emitting uranium isotopes in soil. This test method describes
trometry Using Neodymium Fluoride
one acceptable approach to the determination of uranium
2
C1284 Practice for Electrodeposition of the Actinides for
isotopes in soil.
Alpha Spectrometry
1.2 The test method is designed to analyze 10 g of soil;
D1193 Specification for Reagent Water
however, the sample size may be varied to 50 g depending on
D3084 Practice for Alpha-Particle Spectrometry of Water
the activity level. This test method may not be able to
D3648 Practices for the Measurement of Radioactivity
completely dissolve all forms of uranium in the soil matrix.
Studies have indicated that the use of hydrofluoric acid to
3. Summary of Test Method
dissolve soil has resulted in lower values than results using
3.1 A soil sample with uranium-232 tracer added is heated
total dissolution by fusion.
to destroy organic matter and dissolved with a mixture of
1.3 The lower limit of detection is dependent on count time,
hydrofluoric acid and nitric acid.The uranium is coprecipitated
sample size, detector efficiency, background, and tracer yield.
with ferric hydroxide and the precipitate is dissolved with
The chemical recovery averaged 78 % in a single laboratory
hydrochloricacid.Ironisremovedbyextractionwithisopropyl
evaluation, and 66 % in an interlaboratory collaborative study.
ether, and plutonium, radium, and thorium are separated from
1.4 This standard does not purport to address all of the
uranium by anion exchange. Uranium is electrodeposited on a
safety concerns, if any, associated with its use. It is the
stainless steel disk and determined by alpha spectrometry. As
responsibility of the user of this standard to establish appro-
an option, the uranium may be prepared for alpha spectromet-
priate safety and health practices and determine the applica-
ric measurement by using coprecipitation with neodymium
bility of regulatory limitations prior to use. A specific precau-
fluoride.
tionary statement is given in Section 10.
4. Significance and Use
2. Referenced Documents
3 4.1 This test method is used to analyze soil for alpha-
2.1 ASTM Standards:
emitting uranium isotopes. It can be used to establish baseline
C998 Practice for Sampling Surface Soil for Radionuclides
uranium levels and to monitor depositions from nuclear facili-
ties.
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
5. Interferences
Test.
5.1 Protactinium-231 may not be completely separated by
CurrenteditionapprovedJune1,2005.PublishedJuly2005.Originallyapproved
in 1983. Last previous edition approved in 2000 as C1000 – 00. DOI: 10.1520/ the procedure and could interfere with the determination of
C1000-05.
uranium-233 or uranium-234 because it has the following
2
Casella, V. A., Bishop, C. T., and Glosby, A. A., “Radiometric Method for the
alpha energies in MeV: 5.06, 5.03, 5.01, 4.95 and 4.73 (see
Determination of Uranium in Soil andAir,” U.S. Environmental ProtectionAgency,
AppendixX1).Ifneptuniumispresentinthesampleintheplus
EPA-600/7-80-019, Las Vegas, NV, February 1980; and in Practices D3084 and
D3648.
four oxidation state, it will co-elute with the uranium.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.2 Since uranium-232 is added as a tracer, it can not be
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
determined in soil. Uranium-232 is rarely present in soil
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. samples. If present in significant quantities relative to the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C1000–05
5
activity of uranium-232 tracer added, uranium-232 will lead to 7.7 Anion Exchange Resin —Type 1 anion exchange resin,
an overestimation of the chemical yield and a low bias in 8% cross-linked, 100-200 mesh, chloride form. Prepare a resin
uranium results. slurry by soaking the resin in 8M HCl
...

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4.1 Because of concerns for safety and the protection of nuclear materials from theft, stringent specifications are placed on chemical processes and the chemical and physical properties of nuclear materials. Strict requirements for the control and accountability of nuclear materials are imposed on the users of those materials. Therefore, when analyses are made by a laboratory to support a project such as the fabrication of nuclear fuel materials, various performance requirements may be imposed on the laboratory. One such requirement is often the use of qualified methods. Their use gives greater assurance that the data produced will be satisfactory for the intended use of those data. A qualified method will help assure that the data produced will be comparable to data produced by the same qualified method in other laboratories.  
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Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry

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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.
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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.  
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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.  
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ASTM C1718-10(2019)(Test Method)
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5.1 The TGS provides a nondestructive means of mapping the attenuation characteristics and the distribution of the radionuclide content of items on a voxel by voxel basis. Typically in a TGS analysis a vertical layer (or segment) of an item will be divided into a number of voxels. By comparison, a segmented gamma scanner (SGS) can determine matrix attenuation and radionuclide concentrations only on a segment by segment basis.  
5.2 It has been successfully used to quantify  238Pu, 239Pu, and 235U. SNM loadings from 0.5 g to 200 g of 239Pu (5, 6), from 1 g to 25 g of 235U (7), and from 0.1 to 1 g of 238Pu have been successfully measured. The TGS technique has also been applied to assaying radioactive waste generated by nuclear power plants (NPP). Radioactive waste from NPP is dominated by activation products (for example, 54Mn, 58Co, 60Co,  110mAg) and fission products (for example, 137Cs,  134Cs). The radionuclide activities measured in NPP waste is in the range from 3.7E+04 Bq to 1.0E+07 Bq. Some results of TGS application to non-SNM radionuclides can be found in the literature  (8).  
5.3 The TGS technique is well suited for assaying items that have heterogeneous matrices and that contain a non-uniform radionuclide distribution.  
5.4 Since the analysis results are obtained on a voxel by voxel basis, the TGS technique can in many situations yield more accurate results when compared to other gamma ray techniques such as SGS.  
5.5 In determining the radionuclide distribution inside an item, the TGS analysis explicitly takes into account the cross talk between various vertical layers of the item.  
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1.2.1 Spent nuclear fuel reprocessing and fuel production.  
1.2.2 Homogeneous aqueous solutions contained in cylindrical vials or cuvettes. HKED systems may use two separate sample containers, namely a rectangular cuvette for KED and a cylindrical vial for XRF. Alternatively, there are HKED systems that use a sample contained in a single cylindrical vial, for both K-Edge and XRF.  
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1.2.6 Solutions which contain uranium and plutonium with uranium concentration of 150 to 250 g/L and a U:Pu ratio of 100:1 typically, in the presence of fission products with β, γ, activity of up to 10 TBq/L.
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5.1 The following methods assist in demonstrating regulatory compliance in such areas as safeguards (Special Nuclear Material), inventory control, criticality control, decontamination and decommissioning, waste disposal, holdup and shipping.  
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1.7 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.  
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5.1 This test method is applicable to organic solutions containing 20 to 2000 μg uranium per mL of solution presented to the spectrometer for the solution techniques or 200 to 50 000 μg uranium per g using the fused pellet technique.  
5.2 Either wavelength-dispersive or energy-dispersive XRF systems may be used, provided that the software accompanying the system is able to accommodate the use of internal standards.
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1.1 This test method covers the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of oils and organic solutions containing uranium. Two different preparation techniques are described.  
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1.3 This test method requires the use of an appropriate internal standard. Care must be taken to ascertain that samples analyzed by this test method do not contain the internal standard or that this contamination, whenever present, has been corrected for mathematically. Such corrections are not addressed in this procedure. Care must be taken that the internal standard and sample medium are compatible; that is, samples must be miscible with tri- n-butyl phosphate (TBP) and must not remove the internal standard from solution. Alternatively, a scatter line may be used as the internal standard.2  
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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1.4 The values stated in SI units are to be regarded as the standard.  
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5.1 This practice was developed for the purpose of summarizing the various generic radiometric techniques, equipment, and practices that are used for the measurement of radioactivity.
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General Information  
6 – 11  
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12 – 22  
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23 – 33  
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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.  
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