ASTM D3865-09(2015)
(Test Method)Standard Test Method for Plutonium in Water (Withdrawn 2024)
Standard Test Method for Plutonium in Water (Withdrawn 2024)
SIGNIFICANCE AND USE
5.1 This test method was developed to measure plutonium in environmental waters or waters released to the environment and to determine whether or not the plutonium concentration exceeds the maximum amount allowable by regulatory statutes.
SCOPE
1.1 This test method covers the determination of alpha-particle-emitting isotopes of plutonium concentrations over 0.01 Bq/L (0.3 pCi/L) in water by means of chemical separations and alpha pulse-height analysis (alpha-particle spectrometry). Due to overlapping alpha-particle energies, this method cannot distinguish 239Pu from 240Pu. Plutonium is chemically separated from a 1-L water sample by coprecipitation with ferric hydroxide, anion exchange and electrodeposition. The test method applies to soluble plutonium and to suspended particulate matter containing plutonium. In the latter situation, an acid dissolution step is required to assure that all of the plutonium dissolves.
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards are given in Section 9.
WITHDRAWN RATIONALE
This test method covers the determination of alpha-particle-emitting isotopes of plutonium concentrations over 0.01 Bq/L (0.3 pCi/L) in water by means of chemical separations and alpha pulse-height analysis (alpha-particle spectrometry). Due to overlapping alpha-particle energies, this method cannot distinguish 239Pu from 240Pu. Plutonium is chemically separated from a 1-L water sample by coprecipitation with ferric hydroxide, anion exchange and electrodeposition. The test method applies to soluble plutonium and to suspended particulate matter containing plutonium. In the latter situation, an acid dissolution step is required to assure that all of the plutonium dissolves.
Formerly under the jurisdiction of Committee D19 on Water, this test method was withdrawn in February 2024 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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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: D3865 − 09 (Reapproved 2015)
Standard Test Method for
1
Plutonium in Water
This standard is issued under the fixed designation D3865; 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 Applicable Test Methods of Committee D19 on Water
D3084 Practice for Alpha-Particle Spectrometry of Water
1.1 This test method covers the determination of alpha-
D3370 Practices for Sampling Water from Closed Conduits
particle-emitting isotopes of plutonium concentrations over
D5847 Practice for Writing Quality Control Specifications
0.01 Bq/L (0.3 pCi/L) in water by means of chemical separa-
for Standard Test Methods for Water Analysis
tions and alpha pulse-height analysis (alpha-particle spectrom-
etry). Due to overlapping alpha-particle energies, this method
3. Terminology
239 240
cannot distinguish Pu from Pu. Plutonium is chemically
3.1 Definitions:
separated from a 1-L water sample by coprecipitation with
3.1.1 For definitions of terms used in this test method, refer
ferric hydroxide, anion exchange and electrodeposition. The
to Terminology D1129 and Terminology C859.
test method applies to soluble plutonium and to suspended
particulate matter containing plutonium. In the latter situation,
4. Summary of Test Method
an acid dissolution step is required to assure that all of the
4.1 The water sample is acidified and a plutonium isotopic
plutonium dissolves.
236 242
tracer, for example Pu or Pu, is added as a tracer before
1.2 The values stated in SI units are to be regarded as
any chemical separations are performed. Iron is added to the
standard. No other units of measurement are included in this
water as iron (III), and the plutonium is coprecipitated with the
standard.
iron as ferric hydroxide. After decantation and centrifugation,
1.3 This standard does not purport to address all of the the ferric hydroxide precipitate containing the coprecipitated
safety concerns, if any, associated with its use. It is the
plutonium is dissolved, and the solution is adjusted to 8 M in
responsibility of the user of this standard to establish appro- HNO for anion exchange separation.When the sample fails to
3
priate safety and health practices and determine the applica-
dissolve because of the presence of insoluble residue, the
bilityofregulatorylimitationspriortouse.Specifichazardsare residue is treated by a rigorous acid dissolution using concen-
given in Section 9. trated nitric, hydrofluoric, and hydrochloric acids.
4.2 After an anion exchange separation, the plutonium is
2. Referenced Documents
electrodeposited onto a stainless steel disk for counting by
2
2.1 ASTM Standards:
alpha pulse-height analysis using a silicon surface barrier or
C859 Terminology Relating to Nuclear Materials
ion-implanted detector. Table 1 shows the alpha energies of the
C1163 Practice for MountingActinides forAlpha Spectrom-
isotopes of interest in this test method. The absolute activities
238 239/240
etry Using Neodymium Fluoride
of Pu and Pu are calculated independent of discrete
C1284 Practice for Electrodeposition of the Actinides for
detector efficiency and chemical yield corrections by directly
Alpha Spectrometry
comparingthenumberofcountsineachpeakrelativetocounts
236 242
D1129 Terminology Relating to Water
observed from a known activity of Pu or Pu tracer (see
D1193 Specification for Reagent Water
Eq 1).
D2777 Practice for Determination of Precision and Bias of
5. Significance and Use
5.1 This test method was developed to measure plutonium
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
in environmental waters or waters released to the environment
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi-
and to determine whether or not the plutonium concentration
cal Analysis.
exceeds the maximum amount allowable by regulatory stat-
Current edition approved Jan. 1, 2015. Published January 2015. Originally
utes.
approved in 1980. Last previous edition approved in 2009 as D3865 – 09. DOI:
10.1520/D3865-09R15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Interferences
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Thorium-228, when present in the original water sample
Standards volume information, refer to the standard’s Document Summary page on
238
the ASTM website. at concentrations 100 times or greater than Pu has been
Copyright © ASTM International, 100 Barr Harbor Driv
...
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: D3865 − 09 (Reapproved 2015)
Standard Test Method for
1
Plutonium in Water
This standard is issued under the fixed designation D3865; 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 Applicable Test Methods of Committee D19 on Water
D3084 Practice for Alpha-Particle Spectrometry of Water
1.1 This test method covers the determination of alpha-
D3370 Practices for Sampling Water from Closed Conduits
particle-emitting isotopes of plutonium concentrations over
D5847 Practice for Writing Quality Control Specifications
0.01 Bq/L (0.3 pCi/L) in water by means of chemical separa-
for Standard Test Methods for Water Analysis
tions and alpha pulse-height analysis (alpha-particle spectrom-
etry). Due to overlapping alpha-particle energies, this method
3. Terminology
239 240
cannot distinguish Pu from Pu. Plutonium is chemically
3.1 Definitions:
separated from a 1-L water sample by coprecipitation with
3.1.1 For definitions of terms used in this test method, refer
ferric hydroxide, anion exchange and electrodeposition. The
to Terminology D1129 and Terminology C859.
test method applies to soluble plutonium and to suspended
particulate matter containing plutonium. In the latter situation,
4. Summary of Test Method
an acid dissolution step is required to assure that all of the
4.1 The water sample is acidified and a plutonium isotopic
plutonium dissolves.
236 242
tracer, for example Pu or Pu, is added as a tracer before
1.2 The values stated in SI units are to be regarded as
any chemical separations are performed. Iron is added to the
standard. No other units of measurement are included in this
water as iron (III), and the plutonium is coprecipitated with the
standard.
iron as ferric hydroxide. After decantation and centrifugation,
1.3 This standard does not purport to address all of the
the ferric hydroxide precipitate containing the coprecipitated
safety concerns, if any, associated with its use. It is the plutonium is dissolved, and the solution is adjusted to 8 M in
responsibility of the user of this standard to establish appro-
HNO for anion exchange separation. When the sample fails to
3
priate safety and health practices and determine the applica- dissolve because of the presence of insoluble residue, the
bility of regulatory limitations prior to use. Specific hazards are
residue is treated by a rigorous acid dissolution using concen-
given in Section 9.
trated nitric, hydrofluoric, and hydrochloric acids.
4.2 After an anion exchange separation, the plutonium is
2. Referenced Documents
electrodeposited onto a stainless steel disk for counting by
2
2.1 ASTM Standards:
alpha pulse-height analysis using a silicon surface barrier or
C859 Terminology Relating to Nuclear Materials
ion-implanted detector. Table 1 shows the alpha energies of the
C1163 Practice for Mounting Actinides for Alpha Spectrom-
isotopes of interest in this test method. The absolute activities
238 239/240
etry Using Neodymium Fluoride
of Pu and Pu are calculated independent of discrete
C1284 Practice for Electrodeposition of the Actinides for
detector efficiency and chemical yield corrections by directly
Alpha Spectrometry
comparing the number of counts in each peak relative to counts
236 242
D1129 Terminology Relating to Water
observed from a known activity of Pu or Pu tracer (see
D1193 Specification for Reagent Water
Eq 1).
D2777 Practice for Determination of Precision and Bias of
5. Significance and Use
5.1 This test method was developed to measure plutonium
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
in environmental waters or waters released to the environment
and is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemi-
and to determine whether or not the plutonium concentration
cal Analysis.
exceeds the maximum amount allowable by regulatory stat-
Current edition approved Jan. 1, 2015. Published January 2015. Originally
utes.
approved in 1980. Last previous edition approved in 2009 as D3865 – 09. DOI:
10.1520/D3865-09R15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Interferences
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Thorium-228, when present in the original water sample
Standards volume information, refer to the standard’s Document Summary page on
238
the ASTM website. at concentrations 100 times or greater than Pu has been
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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