ASTM D3865-02

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Designation:D3865–02
Standard Test Method for
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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 D 3856 Guide for Good Laboratory Practices in Laborato-
4
ries Engaged in Sampling and Analysis of Water
1.1 This test method covers the determination of alpha-
D 5847 Practice for Writing Quality Control Specifications
particle-emitting isotopes of plutonium concentrations over
5
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
239 240 238
etry). The isotopes, Pu, Pu, and Pu, are 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 D 1129 and Terminology C 859.
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
242
4.1 The water sample is acidified and Pu is added as a
plutonium dissolves.
tracer before any chemical separations are performed. Iron is
1.2 This standard does not purport to address all of the
added to the water as iron (III), and the plutonium is copre-
safety concerns, if any, associated with its use. It is the
cipitated with the iron as ferric hydroxide. After decantation
responsibility of the user of this standard to establish appro-
and centrifugation, the ferric hydroxide precipitate containing
priate safety and health practices and determine the applica-
the coprecipitated plutonium is dissolved, and the solution is
bilityofregulatorylimitationspriortouse.Specifichazardsare
adjusted to 8 M in HNO for anion exchange separation.When
3
given in Section 9
the sample fails to dissolve because of the presence of
insoluble residue, the residue is treated by a rigorous acid
2. Referenced Documents
dissolution using concentrated nitric, hydrofluoric, and hydro-
2.1 ASTM Standards:
2 chloric acids.
C 859 Terminology Relating to Nuclear Materials
4.2 After an anion exchange separation, the plutonium is
C 1192 Test Method for Mounting Actinides for Alpha
3 electrodeposited onto a stainless steel disk for counting by
Spectrometry Using Neodymium Fluoride
alpha pulse-height analysis using a silicon surface barrier or
C 1284 Practice for Electrodeposition of the Actinides for
2 ion-implanted detector.Table 1 shows the alpha energies of the
Alpha Spectrometry
4 isotopes of interest in this test method. From the recovery of
D 1129 Terminology Relating to Water
242 238 239/240
4 the Pu tracer, the absolute activities of Pu and Pu
D 1193 Specification for Reagent Water
can be calculated.
D 2777 Practice for Determination of Precision and Bias of
4
Applicable Methods of Committee D19 on Water
5. Significance and Use
5
D 3084 Practice for Alpha Spectrometry of Water
5.1 This test method was developed to measure plutonium
4
D 3370 Practices for Sampling Water
5 in environmental waters or waters released to the environment,
D 3648 Practices for the Measurement of Radioactivity
and to determine whether or not the plutonium concentration
exceeds the maximum amount allowable by regulatory stat-
utes.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.04 .
6. Interferences
Current edition approved Feb. 10, 2002. Published May 2002. Originally
228
published as D 3865 - 80. Last previous edition D 3865 - 97.
6.1 Th when present at concentrations 100 times or
2
238
Annual Book of ASTM Standards, Vol 12.01.
greater than Pu has been found to interfere with the
3
Annual Book of ASTM Standards, Vol 15.02.
238 228
4 determination of Pu. Some Th comes through the
Annual Book of ASTM Standards, Vol 11.01.
5
Annual Book of ASTM Standards, Vol 11.02. chemical separation procedure and is electrodeposited with the
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D3865–02
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TABLE 1 Radioactive Decay Characteristics of Isotopes of
tee onAnalytical Reagents of theAmerican Chemical Society.
A
Interest in the Determination of Plutonium in Water
Other grades may be used, provided it is first ascertained that
Half Life Principal Alpha Energies in MeV
the reagent is of sufficiently high purity
...