ASTM D3865-09
(Test Method)Standard Test Method for Plutonium in Water
Standard Test Method for Plutonium in Water
SIGNIFICANCE AND USE
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
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Designation: D3865 − 09
StandardTest 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 D3084 Practice for Alpha-Particle Spectrometry of Water
D3370 Practices for Sampling Water from Closed Conduits
1.1 This test method covers the determination of alpha-
D5847 Practice for Writing Quality Control Specifications
particle-emitting isotopes of plutonium concentrations over
for Standard Test Methods for Water Analysis
0.01 Bq/L (0.3 pCi/L) in water by means of chemical separa-
tions and alpha pulse-height analysis (alpha-particle spectrom-
3. Terminology
etry). Due to overlapping alpha-particle energies, this method
239 240
3.1 Definitions:
cannot distinguish Pu from Pu. Plutonium is chemically
3.1.1 For definitions of terms used in this test method, refer
separated from a 1-L water sample by coprecipitation with
to Terminology D1129 and Terminology C859.
ferric hydroxide, anion exchange and electrodeposition. The
test method applies to soluble plutonium and to suspended
4. Summary of Test Method
particulate matter containing plutonium. In the latter situation,
an acid dissolution step is required to assure that all of the
4.1 The water sample is acidified and a plutonium isotopic
236 242
plutonium dissolves.
tracer, for example Pu or Pu, is added as a tracer before
any chemical separations are performed. Iron is added to the
1.2 The values stated in SI units are to be regarded as
water as iron (III), and the plutonium is coprecipitated with the
standard. No other units of measurement are included in this
iron as ferric hydroxide. After decantation and centrifugation,
standard.
the ferric hydroxide precipitate containing the coprecipitated
1.3 This standard does not purport to address all of the
plutonium is dissolved, and the solution is adjusted to 8 M in
safety concerns, if any, associated with its use. It is the
HNO for anion exchange separation.When the sample fails to
3
responsibility of the user of this standard to establish appro-
dissolve because of the presence of insoluble residue, the
priate safety and health practices and determine the applica-
residue is treated by a rigorous acid dissolution using concen-
bilityofregulatorylimitationspriortouse.Specifichazardsare
trated nitric, hydrofluoric, and hydrochloric acids.
given in Section 9
4.2 After an anion exchange separation, the plutonium is
2. Referenced Documents
electrodeposited onto a stainless steel disk for counting by
2 alpha pulse-height analysis using a silicon surface barrier or
2.1 ASTM Standards:
ion-implanted detector. Table 1 shows the alpha energies of the
C859 Terminology Relating to Nuclear Materials
isotopes of interest in this test method. The absolute activities
C1163 Practice for MountingActinides forAlpha Spectrom-
238 239/240
of Pu and Pu are calculated independent of discrete
etry Using Neodymium Fluoride
detector efficiency and chemical yield corrections by directly
C1284 Practice for Electrodeposition of the Actinides for
comparingthenumberofcountsineachpeakrelativetocounts
Alpha Spectrometry
236 242
observed from a known activity of Pu or Pu tracer (see
D1129 Terminology Relating to Water
Eq 1).
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of
5. Significance and Use
Applicable Test Methods of Committee D19 on Water
5.1 This test method was developed to measure plutonium
in environmental waters or waters released to the environment
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and to determine whether or not the plutonium concentration
and is the direct responsibility of Subcommittee D19.04 .
exceeds the maximum amount allowable by regulatory stat-
Current edition approved Feb. 1, 2009. Published March 2009. Originally
utes.
approved in 1980. Last previous edition approved in 2002 as D3865 – 02. DOI:
10.1520/D3865-09.
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
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D3865 − 09
TABLE 1 Radioactive Decay Characteristics of Isotopes of
(preferably dispo
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D3865–02 Designation:D3865–09
Standard Test Method for
1
Plutonium in Water
This standard is issued under the fixed designation D 3865; 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-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).The isotopes,
240
239 Pu from 238
Due to overlapping alpha-particle energies, this method cannot distinguish Pu, Pu, and Pu, are 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.
1.2Pu. Plutonium is chemically separated from a 1-Lwater 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
2. Referenced Documents
2
2.1 ASTM Standards:
C 859 Terminology Relating to Nuclear Materials
C1192 1163 Test Method Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
C 1284 Practice for Electrodeposition of the Actinides for Alpha Spectrometry
D 1129 Terminology Relating to Water
D 1193 Specification for Reagent Water
D 2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D 3084 Practice for Alpha-Particle Spectrometry of Water
4
D 3370 Practices for Sampling Water
5
D3648Practices for the Measurement of Radioactivity
4
D 3856Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water
5
D5847Practice forWriting Quality Control Specifications for StandardTest Methods forWaterAnalysis Practices for Sampling
Water from Closed Conduits
D 5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D 1129 and Terminology C 859.
4. Summary of Test Method
4.1The water sample is acidified and
236
242
4.1 The water sample is acidified and a plutonium isotopic tracer, for example Pu or Pu, is added as a tracer before any
chemical separations are performed. Iron is added to the water as iron (III), and the plutonium is coprecipitated with the iron as
ferric hydroxide. After decantation and centrifugation, the ferric hydroxide precipitate containing the coprecipitated plutonium is
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.04 .
Current edition approved Feb. 10, 2002. Published May 2002. Originally published as D3865 - 80. Last previous edition D3865 - 97.
Current edition approved Feb. 1, 2009. Published March 2009. Originally approved in 1980. Last previous edition approved in 2002 as D 3865 – 02.
2
Annual Book of ASTM Standards, Vol 12.01.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
1
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D3865–09
dissolved, and the solution is adjusted to 8 M in HNO for anion exchange separation. When the sample fails to dissolve because
3
of the presence of ins
...
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