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ASTM D3865-97

(Test Method)

Standard Test Method for Plutonium in Water

Standard Test Method for Plutonium in Water

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, 239Pu, 240Pu, and 238Pu, 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.
1.2 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.

General Information

Status
Historical
Publication Date
09-Feb-2002
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
D19 - Water
Drafting Committee
D19.04 - Methods of Radiochemical Analysis
Current Stage
Ref Project

Relations

Replaced By
ASTM D3865-02 - Standard Test Method for Plutonium in Water
Effective Date
10-Feb-2002

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ASTM D3865-97 - Standard Test Method for Plutonium in Water
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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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: D 3865 – 97
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope formed. Iron is added to the water as iron (III), and the
plutonium is coprecipitated with the iron as ferric hydroxide.
1.1 This test method covers the determination of alpha-
After decantation and centrifugation, the ferric hydroxide
particle-emitting isotopes of plutonium concentrations over
precipitate containing the coprecipitated plutonium is dis-
0.01 Bq/L 3 pCi/L) in water by means of chemical separations
solved, and the solution is adjusted to 8 M in HNO for anion
3
and alpha pulse-height analysis (alpha-particle spectrometry).
exchange separation. When the sample fails to dissolve be-
The isotopes, plutonium-239, 240, and plutonium-238, are
cause of the presence of insoluble residue, the residue is treated
chemically separated from a 1-L water sample by coprecipita-
by a rigorous acid dissolution using concentrated nitric and
tion with ferric hydroxide, anion exchange and electrodeposi-
hydrofluoric acids.
tion. The test method applies to soluble plutonium and to
4.2 After an anion exchange separation, the plutonium is
suspended particulate matter containing plutonium. In the latter
electrodeposited onto a stainless steel disk for counting by
situation, an acid dissolution step is required to assure that all
alpha pulse-height analysis using a silicon surface barrier or
of the plutonium dissolves.
ion-implanted detector. Table 1 shows the alpha energies of the
1.2 This standard does not purport to address all of the
isotopes of interest in this test method. From the recovery of
safety concerns, if any, associated with its use. It is the
the plutonium-242 tracer, the absolute activities of plutonium-
responsibility of the user of this standard to establish appro-
238 and plutonium-239, 240 can be calculated.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazards are
5. Significance and Use
given in Section 9
5.1 This test method was developed to measure plutonium
in environmental waters or waters released to the environment,
2. Referenced Documents
and to determine whether or not the plutonium concentration
2.1 ASTM Standards:
exceeds the maximum amount allowable by regulatory stat-
2
C 859 Terminology Relating to Nuclear Materials
utes.
3
D 1129 Terminology Relating to Water
3
6. Interferences
D 1193 Specification for Reagent Water
D 2777 Practice for Determination of Precision and Bias of
6.1 Thorium-228 when present at concentrations 100 times
3
Applicable Methods of Committee D-19 on Water
or greater than plutonium-238 has been found to interfere with
4
D 3084 Practice for Alpha Spectrometry of Water
the determination of plutonium-238. Some thorium-228 comes
3
D 3370 Practices for Sampling Water
through the chemical separation procedure and is electrodepos-
4
D 3648 Practices for the Measurement of Radioactivity
ited with the plutonium. If the disk is poorly plated and if the
resolution of the sample as determined by the alpha spectrom-
3. Terminology
eter is not better than 60 keV, the plutonium-238 and the
3.1 Definitions:
thorium-228 may appear as one peak; the principal alpha
3.1.1 For definitions of terms used in this test method, refer
energy of plutonium-238 is 5.50 MeV while that of thorium-
to Terminology D 1129, and C 859.
228 is 5.42 MeV.
4. Summary of Test Method 7. Apparatus
4.1 The water sample is acidified and plutonium-242 is 7.1 Alpha Pulse—Height Analysis System, consisting of a
added as a tracer before any chemical separations are per- silicon surface barrier, or ion-implanted detector, supporting
electronics, and pulse-height analyzer capable of giving a
resolution of 50 keV WHM or better with a sample electrode-
1
This test method is under the jurisdiction of ASTM Committee D-19 on Water
posited on a flat, mirror-finished stainless steel disk. The
and is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemi-
counting efficiency of the system should be greater than 15 %
cal Analysis.
Current edition approved Aug. 10, 1997. Published October 1997. Originally
and the background in the energy region of each peak should
e1
published as D 3865 - 80. Last previous edition D 3865 - 90 .
be less than ten counts in 60 000 s.
2
Annual Book of ASTM Standar
...

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1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 The Reporting Range for the target analytes are listed in Table 1.  
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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.  
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