ASTM C1000-19

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

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.

General Information

• Status: Published
• Publication Date: 31-Oct-2019
• ICS: 17.240 - Radiation measurements
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1000-11 - Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry
• Effective Date: 01-Nov-2019
• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C1284-18 - Standard Practice for Electrodeposition of the Actinides for Alpha Spectrometry
• Effective Date: 01-Jun-2018
• Refers: ASTM C999-17 - Standard Practice for Soil Sample Preparation for the Determination of Radionuclides
• Effective Date: 01-Jun-2017
• Refers: ASTM C998-17 - Standard Practice for Sampling Surface Soil for Radionuclides
• Effective Date: 01-Jun-2017
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jan-2014
• Refers: ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jun-2013
• Refers: ASTM C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013
• Refers: ASTM D3084-05(2012) - Standard Practice for Alpha-Particle Spectrometry of Water
• Effective Date: 01-Jun-2012
• Refers: ASTM D3648-04(2011) - Standard Practices for the Measurement of Radioactivity
• Effective Date: 01-Jan-2011
• Refers: ASTM C859-10b - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Nov-2010
• Refers: ASTM C859-10a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Aug-2010
• Refers: ASTM C1284-10 - Standard Practice for Electrodeposition of the Actinides for Alpha Spectrometry
• Effective Date: 01-Jun-2010
• Refers: ASTM C999-05(2010)e1 - Standard Practice for Soil Sample Preparation for the Determination of Radionuclides
• Effective Date: 01-Jun-2010

Overview

ASTM C1000-19: Standard Test Method for Radiochemical Determination of Uranium Isotopes in Soil by Alpha Spectrometry provides laboratories, regulators, and environmental professionals with a validated approach for measuring alpha-emitting uranium isotopes in soil. Developed by ASTM International, this test method is essential for environmental monitoring, site assessment, and compliance related to uranium and radioactive material handling.

The test method enables accurate evaluation of uranium isotope concentrations in soil samples-critical for establishing baseline levels, monitoring deposition from nuclear facilities, and supporting radiological assessments. Adhering to internationally recognized standards, ASTM C1000-19 ensures reliable, quality-assured data for environmental decision-making.

Key Topics

• Alpha Spectrometry of Uranium in Soil: The standard describes a laboratory method using alpha spectrometry to quantify various uranium isotopes, including U-234, U-235, U-236, and U-238.
• Sample Preparation: Guidance is provided for collecting and preparing soil samples (typically 10 g, variable as needed) using proper dissolution and separation techniques.
• Radiochemical Separation: Uranium is separated from other radionuclides through dissolution, co-precipitation, ether extraction, and ion exchange for high-precision analysis.
• Analytical Sensitivity: Factors such as sample size, detector efficiency, background, and tracer chemical yield all affect the limit of detection. Interlaboratory studies report chemical yields from 66% to 78%.
• Interference and Calibration: The method addresses potential interference from protactinium-231 and neptunium. Uranium-232 is used as a tracer for recovery and calibration.
• Safety Considerations: Detailed safety guidance for handling radioactive materials and hazardous reagents (especially hydrofluoric acid) is outlined, stressing the use of proper laboratory procedures and personal protective equipment.

Applications

The ASTM C1000-19 standard has broad practical utility in both regulatory and research settings, such as:

• Environmental Remediation: Assess the impact of past and present nuclear site operations on soil uranium levels.
• Nuclear Facility Monitoring: Track and monitor uranium deposition in soils surrounding nuclear plants and processing facilities.
• Baseline Environmental Studies: Establish natural background concentrations of uranium isotopes prior to industrial developments or environmental remediation efforts.
• Compliance Testing: Support regulatory reporting and compliance by providing reliable uranium isotope measurements.
• Academic Research: Facilitate studies in environmental radioactivity, geochemistry, and nuclear materials science.
• Quality Assurance: The method provides controls and calibration steps necessary for high-quality, defensible data.

Related Standards

ASTM C1000-19 references related ASTM standards that support consistency and completeness in uranium isotope determination:

• ASTM C859 - Terminology Relating to Nuclear Materials
• ASTM C998 - Practice for Sampling Surface Soil for Radionuclides
• ASTM C999 - Practice for Soil Sample Preparation for the Determination of Radionuclides
• ASTM C1163 - Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
• ASTM C1284 - Practice for Electrodeposition of the Actinides for Alpha Spectrometry
• ASTM D1193 - Specification for Reagent Water
• ASTM D3084 - Practice for Alpha-Particle Spectrometry of Water
• ASTM D3648 - Practices for the Measurement of Radioactivity
• ASTM D7282 - Practice for Set-up, Calibration, and Quality Control of Instruments Used for Radioactivity Measurements

Summary

Adoption of ASTM C1000-19 ensures a validated, internationally recognized method for determining uranium isotopes in soil via alpha spectrometry. Environmental professionals rely on this standard for accurate, traceable, and repeatable results that withstand regulatory and scientific scrutiny-supporting safe nuclear operations, public health, and environmental stewardship.

Keywords: uranium isotopes, alpha spectrometry, soil analysis, radiochemical determination, ASTM C1000-19, environmental monitoring, radioactive contamination, nuclear standards.

Standards Content (Sample)

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.
Designation: C1000 − 19
Standard Test Method for
Radiochemical Determination of Uranium Isotopes in Soil by
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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of alpha-
C859 Terminology Relating to Nuclear Materials
emitting uranium isotopes in soil. This test method describes
C998 Practice for Sampling Surface Soil for Radionuclides
one acceptable approach to the determination of uranium
C999 Practice for Soil Sample Preparation for the Determi-
isotopes in soil.
nation of Radionuclides
1.2 The test method is designed to analyze 10 g of soil.This
C1163 Practice for MountingActinides forAlpha Spectrom-
testmethodmaynotbeabletocompletelydissolveallformsof
etry Using Neodymium Fluoride
uranium in the soil matrix. Studies have indicated that the use
C1284 Practice for Electrodeposition of the Actinides for
of hydrofluoric acid to dissolve soil has resulted in lower Alpha Spectrometry
values than results using total dissolution by fusion. D1193 Specification for Reagent Water
D3084 Practice for Alpha-Particle Spectrometry of Water
1.3 The lower limit of detection is dependent on count time,
D3648 Practices for the Measurement of Radioactivity
sample size, detector, background, and tracer yield. The
D7282 Practice for Set-up, Calibration, and Quality Control
chemicalyieldaveraged78 %inasinglelaboratoryevaluation,
of Instruments Used for Radioactivity Measurements
and 66 % in an interlaboratory collaborative study.
3. Terminology
1.4 The values stated in SI units are to be regarded as
3.1 Except as otherwise defined herein, definition of terms
standard. The values given in parentheses are for information
are given in Terminology C859.
only.
1.5 This standard does not purport to address all of the 4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 Asoil sample to which U tracer is added is heated to
responsibility of the user of this standard to establish appro-
destroy organic matter and dissolved with a mixture of hydro-
priate safety, health, and environmental practices and deter-
fluoric acid and nitric acid. The uranium is coprecipitated with
mine the applicability of regulatory limitations prior to use.
ferric hydroxide and the precipitate is dissolved with hydro-
Specific precautionary statements are given in Section 11.
chloric acid. Iron is removed by extraction with isopropyl
ether, and plutonium, radium, and thorium are separated from
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard- uranium by anion exchange. Uranium is electrodeposited on a
stainless steel disk and determined by alpha spectrometry. As
ization established in the Decision on Principles for the
an option, the uranium may be prepared for alpha spectromet-
Development of International Standards, Guides and Recom-
ric measurement by using coprecipitation with neodymium
mendations issued by the World Trade Organization Technical
fluoride.
Barriers to Trade (TBT) Committee.
5. Significance and Use
5.1 This test method is used to analyze soil for alpha-
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
emitting uranium isotopes. It can be used to establish baseline
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
uranium levels and to monitor depositions from nuclear facili-
Test.
Current edition approved Nov. 1, 2019. Published December 2019. Originally
ties.
approved in 1983. Last previous edition approved in 2011 as C1000 – 11. DOI:
10.1520/C1000-19.
2 3
Casella, V. A., Bishop, C. T., and Glosby, A. A., “Radiometric Method for the For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Determination of Uranium in Soil andAir,” U.S. Environmental ProtectionAgency, contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
EPA-600/7-80-019, Las Vegas, NV, February 1980; and in Practices D3084 and Standards volume information, refer to the standard’s Document Summary page on
D3648. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1000 − 19
6. Interferences 8.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined
6.1 Protactinium-231 may not be completely separated by
in Specification D1193, Type III.
the procedure and could interfere with the determination of
233 234
Uor U because it has the following alpha energies in 8.3 Reagent purity shall be such that the measured radioac-
MeV: 5.06, 5.03, 5.01, 4.95, and 4.73 (see Appendix X1). If
tivityofblanksamplesdoesnotexceedthecalculatedprobable
neptunium is present in the sample in the plus four oxidation uncertainty of the measurement.
state, it will co-elute with the uranium.
8.4 Ammonium Hydroxide (0.15 M)—Mix 10 mL of con-
6.2 Since U is added as a tracer, it can not be determined centrated ammonium hydroxide with water and dilute to 1 L.
insoil.Uranium-232israrelypresentinsoilsamples.Ifpresent
8.5 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
in significant quantities relative to the activity of U tracer
monium hydroxide (NH OH). Keep tightly capped to mini-
232 4
added, U will lead to an overestimation of the chemical
mize the uptake of carbon dioxide.
yield and a low bias in uranium results.
8.6 Ammonium Sulfate Solution (1 M)—Dissolve 132 g of
(NH ) SO in water and dilute to 1 L.
7. Apparatus
4 2 4
8.7 Anion Exchange Resin —Type 1 anion exchange resin,
7.1 Alpha Pulse Height Analysis System:
8 % cross-linked, 100 to 200 mesh, chloride form. Prepare a
7.1.1 A system consisting of a charged particle detector
resin slurry by soaking the resin in 8 M HCl and transfer the
capable of 50 keV or less resolution on samples electrodepos-
slurry to an ion exchange column so that the resin column is
ited on a flat mirror-finished stainless steel disk is required.
approximately 10 cm high.
7.1.2 The resolution is defined as the width of an alpha peak
whenthecountsoneithersideofthepeakareequaltoone-half
8.8 Ferric Chloride Solution (0.18 M in 0.5 M HCl)—
of the counts at the maximum of the peak (full width at half
Dissolve 48 g of FeCl.6HOin0.5 M HCl and dilute to 1 L.
3 2
maximum height (FWHM)).
8.9 Hydriodic Acid (48 %)—Concentrated hydriodic acid
7.1.3 The counting efficiency of the system should be
(HI).
greater than 15 % and the background in the energy region of
each peak should be less than 0.010 cpm.
8.10 Hydrochloric Acid (0.5 M)—Mix 42 mL of concen-
7.1.4 Aregular program of measurement control operations trated HCl with water and dilute to 1 L.
should be conducted for the alpha spectrometry system such as
8.11 Hydrochloric Acid (1 M)—Mix 83 mL of concentrated
regular background checks, daily source check to determine
HCl with water and dilute to 1 L.
system stability, control charting, and careful handling of
8.12 Hydrochloric Acid (6 M)—Mix 500 mL of concen-
samples during changing. See Practice D7282.
trated HCl with water and dilute to 1 L.
7.2 Beakers and Covers (TFE-fluorocarbon), 250 mL.
8.13 Hydrochloric Acid (8 M)—Mix 667 mL of concen-
7.3 Porcelain Crucible, 60 mL.
trated HCl with water and dilute to 1 L.
7.4 Centrifuge and Bottles, 250-mL capacity.
8.14 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
7.5 Ion Exchange Columns, 1.3 cm inside diameter by
chloric acid (HCl).
15 cm long with 100 mL reservoir.
8.15 Hydrochloric Acid-Hydriodic Acid Solution (HCl-
7.6 Automatic Pipettes, 0.1 to 1.0 mL with disposable tips.
HI)—Mix 1 mL of concentrated HI with 50 mL of 6 M HCl.
Prepare immediately before use.
7.7 Furnace, able to maintain 600 °C.
8.16 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
7.8 Separatory funnels, 250 mL.
acid (HF).
8. Reagents
8.17 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
8.1 Purity of Reagents—Reagent grade chemicals shall be (HNO ).
used in all tests. Unless otherwise indicated, it is intended that
8.18 Uranium-232, Standard Solution.
all reagents conform to the specifications of the Committee on
8.19 Boric Acid—Solid.
Analytical Reagents of theAmerican Chemical Society, where
such specifications are available. Other grades may be used,
8.20 Isopropyl Ether.
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
9. Sampling
the determination.
9.1 Collect the sample in accordance with Practice C998.
9.2 Prepare the sample for analysis in accordance with
4 Practice C999.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, AG1-X8 from BioRad Laboratories (Hercules, CA) and A8-B500-M-CL from
MD. Eichrom Technoloigies, Inc.(Lisle, IL) have been found to be satisifactory.
C1000 − 19
10. Calibration and Standardization 12.1.12 Wash the residue with 10 mL of 1 M HCl,
232 centrifuge, and add the washing to the supernate.
10.1 If a standard U solution
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C1000 − 11 C1000 − 19
Standard Test Method for
Radiochemical Determination of Uranium Isotopes in Soil by
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
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. 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. A specific precautionary statement isSpecific precautionary statements are given
in Section 1011.
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.
2. Referenced Documents
2.1 ASTM Standards:
C859 Terminology Relating to Nuclear Materials
C998 Practice for Sampling Surface Soil for Radionuclides
C999 Practice for Soil Sample Preparation for the Determination of Radionuclides
C1163 Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
C1284 Practice for Electrodeposition of the Actinides for Alpha Spectrometry
D1193 Specification for Reagent Water
D3084 Practice for Alpha-Particle Spectrometry of Water
D3648 Practices for the Measurement of Radioactivity
D7282 Practice for Set-up, Calibration, and Quality Control of Instruments Used for Radioactivity Measurements
3. Terminology
3.1 Except as otherwise defined herein, definition of terms are given in Terminology C859.
4. Summary of Test Method
4.1 A soil sample with uranium-232to which U tracer is added is heated to destroy organic matter and dissolved with a
mixture of hydrofluoric acid and nitric acid. The uranium is coprecipitated with ferric hydroxide and the precipitate is dissolved
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved Feb. 1, 2011Nov. 1, 2019. Published February 2011December 2019. Originally approved in 1983. Last previous edition approved in 20052011
as C1000 – 05.C1000 – 11. DOI: 10.1520/C1000-11.10.1520/C1000-19.
Casella, V. A., Bishop, C. T., and Glosby, A. A., “Radiometric Method for the Determination of Uranium in Soil and Air,” U.S. Environmental Protection Agency,
EPA-600/7-80-019, Las Vegas, NV, February 1980; and in Practices D3084 and D3648.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1000 − 19
with hydrochloric acid. Iron is removed by extraction with isopropyl ether, and plutonium, radium, and thorium are separated from
uranium by anion exchange. Uranium is electrodeposited on a stainless steel disk and determined by alpha spectrometry. As an
option, the uranium may be prepared for alpha spectrometric measurement by using coprecipitation with neodymium fluoride.
5. 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.
6. Interferences
6.1 Protactinium-231 may not be completely separated by the procedure and could interfere with the determination of
233 234
uranium-233U or uranium-234U because it has the following alpha energies in MeV: 5.06, 5.03, 5.01, 4.954.95, and 4.73 (see
Appendix X1). If neptunium is present in the sample in the plus four oxidation state, it will co-elute with the uranium.
6.2 Since uranium-232U is added as a tracer, it can not be determined in soil. Uranium-232 is rarely present in soil samples.
232 232
If present in significant quantities relative to the activity of uranium-232U tracer added, uranium-232U will lead to an
overestimation of the chemical yield and a low bias in uranium results.
7. Apparatus
7.1 Alpha Pulse Height Analysis System:
7.1.1 A system consisting of a charged particle detector capable of 50 keV or less resolution on samples electrodeposited on
a flat mirror-finished stainless steel disk is required.
7.1.2 The resolution is defined as the width of an alpha peak when the counts on either side of the peak are equal to one-half
of the counts at the maximum of the peak (full width at half maximum height (FWHM)).
7.1.3 The counting efficiency of the system should be greater than 15 % and the background in the energy region of each peak
should be less than 0.010 cpm.
7.1.4 A regular program of measurement control operations should be conducted for the alpha spectrometry system such as
regular background checks, daily source check to determine system stability, control charting, and careful handling of samples
during changing. See Practice D7282.
7.2 Beakers and Covers (TFE-fluorocarbon), 250 mL.
7.3 Porcelain Crucible, 60 mL.
7.4 Centrifuge and Bottles, 250-mL capacity.
7.5 Ion Exchange Columns, 1.3 cm inside diameter by 15 cm 15 cm long with 100 mL reservoir.
7.6 Automatic Pipettes, 0.1 to 1.0 mL with disposable tips.
7.7 Furnace, able to maintain 600°C.600 °C.
7.8 Separatory funnels, 250 mL.
8. Reagents
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined in
Specification D1193, Type III.
8.3 Reagent purity shall be such that the measured radioactivity of blank samples does not exceed the calculated probable
uncertainty of the measurement.
8.4 Ammonium Hydroxide (0.15 M)—Mix 10 mL of concentrated ammonium hydroxide with water and dilute to 1 L.
8.5 Ammonium Hydroxide (sp gr 0.90)—Concentrated ammonium hydroxide (NH OH). Keep tightly capped to minimize the
uptake of carbon dioxide.
8.6 Ammonium Sulfate Solution (1 M)—Dissolve 132 g of (NH ) SO in water and dilute to 1 L.
4 2 4
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
C1000 − 19
8.7 Anion Exchange Resin —Type 1 anion exchange resin, 8 % cross-linked, 100 to 200 mesh, chloride form. Prepare a resin
slurry by soaking the resin in 8 M HCl and transfer the slurry to an ion exchange column so that the resin column is approximately
10 cm high.
8.8 Ferric Chloride Solution (0.18 M in 0.5 M HCl)—Dissolve 48 g of FeCl . 6H O in 0.5 M HCl and dilute to 1 L.
3 2
8.9 Hydriodic Acid (48 %)—Concentrated hydriodic acid (HI).
8.10 Hydrochloric Acid (0.5 M)—Mix 42 mL of concentrated HCl with water and dilute to 1 L.
8.11 Hydrochloric Acid (1 M)—Mix 83 mL of concentrated HCl with water and dilute to 1 L.
8.12 Hydrochloric Acid (6 M)—Mix 500 mL of concentrated HCl with water and dilute to 1 L.
8.13 Hydrochloric Acid (8 M)—Mix 667 mL of concentrated HCl with water and dilute to 1 L.
8.14 Hydrochloric Acid (sp gr 1.19)—Concentrated hydrochloric acid (HCl).
8.15 Hydrochloric Acid-Hydriodic Acid Solution (HCl-HI)—Mix 1 mL of concentrated HI with 50 mL of 6 M HCl. Prepare
immediately before use.
8.16 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric acid (HF).
8.17 Nitric Acid (sp gr 1.42)—Concentrated nitric acid (HNO ).
8.18 Uranium-232, Standard Solution.
8.19 Boric Acid—Solid.
8.20 Isopropyl Ether.
9. Sampling
9.1 Collect the sample in accordance with Practice C998.
9.2 Prepare the sample for analysis in accordance with Practice C999.
10. Calibration and Standardization
10.1 If a standard uranium-232U solution is not available for use as a tracer, standardize a freshly prepared sample of
uranium-232;U; for guidance refer to Practices D3648. This standard may also be used to establish the counting efficiency of
the alpha spectrometer which then can be used to calculate the chemical yield for each sample.
11. Precautions
11.1 Adequate laboratory facilities, such as fume hoods and controlled ventilation, along with safe techniques, must be used in
this procedure. Extreme care should be exerci
...