ASTM C1647-20
(Practice)Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials
Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials
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.
General Information
- Status
- Published
- Publication Date
- 30-Nov-2020
- Technical Committee
- C26 - Nuclear Fuel Cycle
- Drafting Committee
- C26.05 - Methods of Test
Relations
- Effective Date
- 01-Jan-2024
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Oct-2023
- Effective Date
- 01-Mar-2020
- Effective Date
- 01-Mar-2020
- Effective Date
- 01-Jan-2018
- Effective Date
- 01-Apr-2016
- Effective Date
- 01-Apr-2016
- Effective Date
- 01-Feb-2016
- Effective Date
- 01-Sep-2015
- Effective Date
- 01-Jul-2015
- Effective Date
- 01-Jul-2015
- Effective Date
- 01-Jun-2015
- Effective Date
- 15-Jun-2014
- Effective Date
- 15-Jan-2014
Overview
ASTM C1647-20: Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials provides a robust extraction chromatography column method to separate uranium and/or plutonium from liquid or digested samples prior to impurity analysis. Removing the uranium and plutonium matrix enables more sensitive detection of trace impurities by minimizing signal suppression, particularly when using advanced spectrometric techniques. This standard practice is vital for nuclear material characterization, especially in support of fuel specification compliance and highly accurate impurity quantification.
Key Topics
- Matrix Removal for Trace Metal Analysis: By removing uranium and plutonium before impurity measurement, matrix effects are reduced, resulting in improved detection limits-often between 1–10 parts-per-billion (ppb) when employing techniques like ICP-MS or ICP-AES.
- Extraction Chromatography Method: Utilizes columns packed with specialized resins, such as diamyl, amylphosphonate, to selectively retain uranium and plutonium, allowing impurities to be collected in the effluent for subsequent analysis.
- Compatibility with Analytical Techniques: The purified fractions are suitable for analysis by inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES), or atomic absorption spectrometry (AAS).
- Improved Laboratory Safety: Removal of radioactive matrices means that, in many cases, the remaining impurity solution can be analyzed on standard, non-glove box-enclosed instruments, increasing lab efficiency and reducing risk.
- Interference Mitigation: Special treatment is incorporated to manage potential interference from elements like zirconium, hafnium, niobium, and tantalum.
Applications
The ASTM C1647-20 standard is applied in several key nuclear industry and research contexts, such as:
- Nuclear Fuel Fabrication and Quality Control: Ensures uranium and plutonium materials meet the stringent impurity specifications required for reactor fuel, per standards such as ASTM C753, C757, and C996.
- Impurity Assay in Uranium and Plutonium Compounds: Enables accurate trace element analysis, supporting regulatory compliance and safety assessments.
- Radiochemical Laboratories: Facilitates rapid sample processing and impurity determination, even in settings with limited access to glove-boxes or shielded facilities.
- Reference Method for Other Test Methods: Supports and complements methods such as ASTM C1517 (DC-Arc Spectroscopy), C1287 (ICP-MS of uranium compounds), and C1432 (plutonium impurity analysis).
Related Standards
ASTM C1647-20 is used in conjunction with several related ASTM standards and test methods:
- ASTM C753: Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
- ASTM C757: Specification for Nuclear-Grade Plutonium Dioxide Powder
- ASTM C776, C787, C788, C996: Specifications for various nuclear-grade uranium compounds and solutions
- ASTM C1517: Determination of Metallic Impurities in Uranium by DC-Arc Emission Spectroscopy
- ASTM C1287: Determination of Impurities in Nuclear Grade Uranium Compounds by ICP-MS
- ASTM C1432: Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and ICP-AES Analysis
- ASTM D1193: Specification for Reagent Water
- ASTM C1168, C1347: Practices for preparation and dissolution of plutonium and uranium materials for analysis
Practical Value
By following ASTM C1647-20, laboratories can significantly enhance the reliability and accuracy of impurity analyses in uranium and plutonium matrices. This practice increases analytical sensitivity, reduces potential interferences, and streamlines compliance with nuclear material quality requirements. Adherence to this method also promotes laboratory safety and efficiency by enabling broader use of standard analytical instrumentation for high-precision trace metal assay.
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Frequently Asked Questions
ASTM C1647-20 is a standard published by ASTM International. Its full title is "Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials". This standard covers: 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 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.
ASTM C1647-20 is classified under the following ICS (International Classification for Standards) categories: 71.040.50 - Physicochemical methods of analysis. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM C1647-20 has the following relationships with other standards: It is inter standard links to ASTM C859-24, ASTM C1432-23, ASTM C1168-23, ASTM C787-20, ASTM C996-20, ASTM C1287-18, ASTM C757-16, ASTM C1517-16, ASTM C753-16, ASTM C1168-15, ASTM C787-15, ASTM C996-15, ASTM C1432-15, ASTM C859-14a, ASTM C859-14. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM C1647-20 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
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: C1647 − 20
Standard Practice for
Removal of Uranium or Plutonium, or both, for Impurity
Assay in Uranium or Plutonium Materials
This standard is issued under the fixed designation C1647; 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 C787 Specification for Uranium Hexafluoride for Enrich-
ment
1.1 This practice covers instructions for using an extraction
C788 Specification for Nuclear-Grade Uranyl Nitrate Solu-
chromatography column method for the removal of plutonium
tion or Crystals
or uranium, or both, from liquid or digested oxides or metals
C859 Terminology Relating to Nuclear Materials
prior to impurity measurements. Quantification of impurities
C996 Specification for Uranium Hexafluoride Enriched to
can be made by techniques such as inductively coupled plasma
Less Than 5 % U
mass spectrometry (ICP-MS), inductively coupled plasma
C1168 PracticeforPreparationandDissolutionofPlutonium
atomic emission spectrometry (ICP-AES), or atomic absorp-
Materials for Analysis
tion spectrometry (AAS.)
C1287 Test Method for Determination of Impurities in
1.2 The values stated in SI units are to be regarded as
Nuclear Grade Uranium Compounds by Inductively
standard. No other units of measurement are included in this
Coupled Plasma Mass Spectrometry
standard.
C1347 Practice for Preparation and Dissolution of Uranium
1.3 This standard does not purport to address all of the Materials for Analysis
safety concerns, if any, associated with its use. It is the
C1432 Test Method for Determination of Impurities in
responsibility of the user of this standard to establish appro- Plutonium: Acid Dissolution, Ion Exchange Matrix
priate safety, health, and environmental practices and deter-
Separation, and Inductively Coupled Plasma-Atomic
mine the applicability of regulatory limitations prior to use. Emission Spectroscopic (ICP/AES) Analysis
1.4 This international standard was developed in accor-
C1517 TestMethodforDeterminationofMetallicImpurities
dance with internationally recognized principles on standard- in Uranium Metal or Compounds by DC-Arc Emission
ization established in the Decision on Principles for the
Spectroscopy
Development of International Standards, Guides and Recom-
D1193 Specification for Reagent Water
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
3. Terminology
3.1 Definitions:
2. Referenced Documents
3.1.1 For definitions of terms used in this test method but
2.1 ASTM Standards:
not defined herein, refer to Terminology C859.
C753 Specification for Nuclear-Grade, Sinterable Uranium
Dioxide Powder
4. Summary of Practice
C757 Specification for Nuclear-Grade Plutonium Dioxide
4.1 An aliquot of liquid sample or dissolved solid sample is
Powder for Light Water Reactors
adjusted as needed to 8M nitric acid for plutonium/uranium
C776 Specification for Sintered Uranium Dioxide Pellets for
removal using extraction chromatography. Uranium and pluto-
Light Water Reactors
niumareretainedontheresinandtraceimpuritiesarecollected
in the column effluent. The impurities can be measured by a
variety of techniques.
This practice 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.
5. Significance and Use
Current edition approved Dec. 1, 2020. Published January 2021. Originally
5.1 This practice can be used to separate uranium or
approved in 2006. Last previous edition approved in 2013 as C1647 – 13. DOI:
10.1520/C1647-20.
plutonium, or both, prior to the impurity analysis by various
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
techniques. The removal of uranium and plutonium prior to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
quantification can improve the detection limits by minimizing
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the signal suppression caused by uranium or plutonium when
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1647 − 20
using ICP techniques. Detection limits of ~1–10 part-per- 8.2 Purity of Water—Unless otherwise indicated, references
billion (PPB) may be obtainable by matrix removal. Also, to water shall be understood to mean reagent water as defined
removal of the uranium and plutonium may allow the impuri- in Specification D1193 as Type I.
ties analysis to be performed on a non-glove box enclosed
8.3 Hydrofluoric Acid (28 M)—Concentrated hydrofluoric
instrument.
acid (sp gr 1.2).
5.2 Other test methods exist to determine impurities in
8.4 Nitric Acid (16 M)—Concentrated HNO (sp gr 1.42).
uraniumorplutonium.TestMethodC1517isabletodetermine
8.5 Nitric Acid Solution (8 M)—Add 500 mL of concen-
many impurities in uranium at detection levels of ~1–10
trated nitric acid (sp gr 1.42) to 300 mL of water and dilute to
part-per-million (ppm) by DC-Arc Spectrometry. Test Method
1 L with water.
C1287 is able to determine impurities in uranium at detection
levels of ~100 ppb by ICP-MS. Test Method C1432 provides
8.6 Nitric Acid (8M)—Hydrofluoric Acid (0.05M)—Add
an alternative technique to remove plutonium by ion exchange 500 mL concentrated nitric acid and 1.8 mL concentrated
prior to analysis of the impurities by ICP-AES.
hydrofluoric acid to 250 mL water and dilute to 1 liter with
water.
5.3 This practice can be used to demonstrate compliance
4,5
8.7 Diamyl, Amylphosphonate Resin, 50–100 µm particle
with nuclear fuel specifications, for example, Specifications
C753, C757, C776, C787, C788, and C996. size resin for use with vacuum-assisted flow systems; 100 to
150 µm if using gravity flow systems.
6. Interferences 6
8.8 Polymethacrylate Resin, 100–150 µm particle size
resin.
6.1 Zirconium, hafnium, niobium, and tantalum are retained
on the diamyl, amylphosphonate resin unless hydrofluoric acid
9. Hazards
is added to the nitric acid load/rinse solution. The addition of
9.1 Refer to the laboratory’s chemical hygiene plan and
hydrofluoric acid to recover zirconium, hafnium, niobium, and
tantalum reduces uranium and plutonium retention. For this other applicable guidance for handling chemical and radioac-
tive materials and for the management of radioactive, mixed,
reason, hydrofluoric acid levels must be minimized (typically
<0.05M HF) in the load/rinse solution to prevent uranium or and hazardous waste.
plutonium,orboth,fromelutingfromthecolumnintothetrace
9.2 Hydrofluoric acid is a highly corrosive and toxic acid
metal fraction.
that can severely burn skin, eyes, and mucous membranes.
Hydrofluoric acid differs from other acids because the fluoride
7. Apparatus
ion readily penetrates the skin, causing destruction of deep
tissue layers. Unlike other acids that are rapidly neutralized,
7.1 Large Columns, >13 mL capacity (inner diameter =
hydrofluoricacidreactionswithtissuemaycontinuefordaysif
1.5 cm has been found acceptable) and reservoirs.
left untreated. Familiarization and compliance with the Safety
7.2 Plastic Collection Tubes, 50 mL.
Data Sheet is essential.
7.3 Column Rack, used for gravity flow systems.
10. Procedure
7.4 Polyethylene Frits for columns, 20 µm.
10.1 Column Preparation and Conditioning:
7.5 VacuumBox—Theuseofavacuum-assistedfl
...
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: C1647 − 13 C1647 − 20
Standard Practice for
Removal of Uranium or Plutonium, or both, for Impurity
Assay in Uranium or Plutonium Materials
This standard is issued under the fixed designation C1647; 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 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)(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 safety, health, and healthenvironmental 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.
2. Referenced Documents
2.1 ASTM Standards:
C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder for Light Water Reactors
C776 Specification for Sintered Uranium Dioxide Pellets for Light Water Reactors
C787 Specification for Uranium Hexafluoride for Enrichment
C788 Specification for Nuclear-Grade Uranyl Nitrate Solution or Crystals
C859 Terminology Relating to Nuclear Materials
C996 Specification for Uranium Hexafluoride Enriched to Less Than 5 % U
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1287 Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma
Mass Spectrometry
C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis
C1432 Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and
Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
This practice 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 Jan. 1, 2013Dec. 1, 2020. Published January 2013January 2021. Originally approved in 2006. Last previous edition approved in 20062013 as
C1647 – 06.13. DOI: 10.1520/C1647-13.10.1520/C1647-20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. 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
C1647 − 20
C1517 Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission
Spectroscopy
D1193 Specification for Reagent Water
3. Terminology
3.1 For definitions of terms used in this test method but not defined herein, refer to Terminology C859.
3.1 Definitions:
3.1.1 For definitions of terms used in this test method but not defined herein, refer to Terminology C859.
4. Summary of Practice
4.1 An aliquot of liquid sample or dissolved solid sample is adjusted as needed to 8M nitric acid for plutonium/uranium removal
using extraction chromatography. Uranium and plutonium are retained on the resin and trace impurities are collected in the column
effluent. The impurities can be measured by a variety of techniques.
5. 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.
6. Interferences
6.1 Zirconium, hafnium, niobium, and tantalum are retained on the diamyl, amylphosphonate resin unless hydrofluoric acid is
added to the nitric acid load/rinse solution. The addition of hydrofluoric acid to recover zirconium, hafnium, niobium, and tantalum
reduces uranium and plutonium retention. For this reason, hydrofluoric acid levels must be minimized (typically <0.05M HF) in
the load/rinse solution to prevent uranium or plutonium, or both, from eluting from the column into the trace metal fraction.
7. Apparatus
7.1 Large Columns, >13 mL capacity (inner diameter = 1.5 cm 1.5 cm has been found acceptable) and reservoirs.
7.2 Plastic Collection Tubes, 50 mL.
7.3 Column Rack, used for gravity flow systems.
7.4 Polyethylene Frits for columns, 20 μm.
7.5 Vacuum Box—The use of a vacuum-assisted flow system permits the use of higher eluent flow rates. Gravity flow systems may
be used instead.
8. Reagents
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
C1647 − 20
reagents shall 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. High purity acids may be used to reduce reagent blanks
and to achieve lower detection limits.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined in
Specification D1193 as Type I.
8.3 Hydrofluoric Acid (28 M)—Concentrated hydrofluoric acid (sp gr 1.2).
8.4 Nitric Acid (16 M)—Concentrated HNO (sp gr 1.42).
8.5 Nitric Acid Solution (8 M)—Add 500 mL of concentrated nitric acid (sp gr 1.42) to 300 mL of water and dilute to 1 L with
water.
8.6 Nitric Acid (8M)—Hydrofluoric Acid (0.05M)—Add 500 mL concentrated nitric acid and 1.8 mL concentrated hydrofluoric
acid to 250 mL water and dilute to 1 liter with water.
4,5
8.7 Diamyl, Amylphosphonate Resin, 50–100 μm particle size resin for use with vacuum-assisted flow systems; 100 to 150 μm
if using gravity flow systems.
8.8 Polymethacrylate Resin, 100–150 μm particle size resin.
9. Hazards
9.1 Refer to the laboratory’s chemical hygiene plan and other applicable guidance for handling chemical and radioactive materials
and for the management of radioactive, mixed, and hazardous waste.
9.2 Hydrofluoric acid is a highly corrosive and toxic acid that can severely burn skin, eyes, and mucous membranes. Hydrofluoric
acid is similar to other acids in that the initial extent of a burn depends on the concentration, the temperature and the duratio
...
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