ASTM D4922-94e1
(Test Method)Standard Test Method for Determination of Radioactive Iron in Water
Standard Test Method for Determination of Radioactive Iron in Water
SCOPE
1.1 This test method covers the determination of 55Fe in the presence of 59Fe by liquid scintillation counting. The a-priori minimum detectable concentration for this test method is E-3 Bq/mL.
1.2 This test method was developed principally for the quantitative determination of 55Fe. However, after proper calibration of the liquid scintillation counter with reference standards of each nuclide, 59Fe may also be quantified.
1.3 This test method was used successfully with Type III reagent water conforming to Specification D1193. It is the responsibility of the user to ensure the validity of this test method for waters of untested matrices.
1.4 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. For a specific hazard statement, see Section 9.
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NOTICE: This standard has either been superseded and replaced by a new version or
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e1
Designation: D 4922 – 94
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
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Determination of Radioactive Iron in Water
This standard is issued under the fixed designation D 4922; 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
e NOTE—Editorial changes were made throughout in August 1995.
1. Scope this test method or in Terminology D 1129, refer to other
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published glossaries.
1.1 This test method covers the determination of iron-55 in
the presence of iron-59 by liquid scintillation counting. The
4. Summary of Test Method
a-priori minimum detectable concentration for this test method
4.1 This test method describes the effective separation of
is 7.4 E-3 Bq/mL.
iron from the interfering cations of manganese, cobalt, zirco-
1.2 This test method was developed principally for the
nium, niobium, and cesium by anion exchange using various
quantitative determination of iron-55. However, after proper
molarity acid washes. Subsequent elution of the iron is
calibration of the liquid scintillation counter with reference
followed by phosphate precipitation to remove any residual
standards of each nuclide, iron-59 may also be quantitated.
zinc. The iron phosphate precipitate is dissolved in phosphoric
1.3 This test method was used successfully with Type III
acid and water and mixed with liquid scintillation cocktail. The
reagent water conforming to Specification D 1193. It is the
chemical yield is determined by the recovery of iron carrier
responsibility of the user to ensure the validity of this test
using atomic absorption spectrophotometry or any procedure
method for waters of untested matrices.
described in Test Method D 1068.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 Radioactive iron is produced by neutron activation of
priate safety and health practices and determine the applica-
water, reactor fuel cladding material, and reactor structural
bility of regulatory limitations prior to use. For a specific
2 components. It is, therefore, of significance as an indicator of
hazard statement, see Section 9.
the corrosion of reactor parts.
2. Referenced Documents 5.2 This technique effectively removes other activation and
fission products such as isotopes of iodine, zinc, manganese,
2.1 ASTM Standards:
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cobalt, and cesium by the addition of hold-back carriers and an
D 1068 Test Methods for Iron in Water
3 anion exchange technique. The fission products (zirconium-95
D 1129 Terminology Relating to Water
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and niobium-95) are selectively eluted with hydrochloric-
D 1193 Specifications for Reagent Water
hydrofluoric acid washes. The iron is finally separated from
D 2777 Practice for Determination of Precision and Bias of
+2
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Zn by precipitation of FePO at a pH of 3.0.
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Applicable Methods of Committee D-19 on Water
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D 3370 Practices for Sampling Water
6. Interferences
6.1 Samples of reactor origin will also contain iron-59 after
3. Terminology
other radioactive contaminants have been removed by anion
3.1 Definitions—For definitions of terms used in this test
exchange (see Fig. 1). Iron-59 is also an activation product
method, refer to Terminology D 1129. For terms not defined in
which decays by b-g emission and will be a source of
interference in the quantitative determination of iron-55. The
large difference in the energies of their characteristic decay
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emissions makes it possible to determine appropriate factors to
This test method is under the jurisdiction of ASTM Committee D-19 on Water
and is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemi-
correct for the iron-59 spectral cross-talk in the iron-55 region.
cal Analysis.
6.2 Quenching, which may be caused by a number of
Current edition approved Sept. 15, 1994. Published November 1994. Originally
factors, results in a reduction in the light output from the
published as D 4922 – 89. Last previous edition D 4922 – 89.
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Currie, L., “Limits for Qualitative Detection and Quantitative Determina- sample. The subsequent decrease in the spectral pulse height
tion,’’ Analytical Chemistry, 40, 1968, pp. 586–593.
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Annual Book of ASTM Standards, Vol 11.01.
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“American National Standard Glossary of Terms,’’ Nuclear Science and
Technology (ANSI N1.1), American National Standards Institute, 1430 Broadway,
New York, NY 10018.
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