ASTM D4922-09
(Test Method)Standard Test Method for Determination of Radioactive Iron in Water
Standard Test Method for Determination of Radioactive Iron in Water
SIGNIFICANCE AND USE
Radioactive iron is produced by neutron activation of stable iron. Its concentration in reactor coolant is used to monitor the corrosion of reactor parts such as reactor fuel-cladding material and reactor structural components.
This technique effectively removes other activation and fission products such as isotopes of iodine, zinc, manganese, cobalt, and cesium by the addition of hold-back carriers and an anion exchange technique. The fission products (zirconium-95 and niobium-95) are selectively eluted with hydrochloric-hydrofluoric acid washes. The iron is finally separated from Zn+2 by precipitation of FePO4 at a pH of 3.0.
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 7.4 Bq/L.
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 D 1193. 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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Designation: D4922 − 09
StandardTest Method for
1
Determination of Radioactive Iron in Water
This standard is issued under the fixed designation D4922; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
55
1.1 This test method covers the determination of Fe in the 3.1 Definitions—For definitions of terms used in this test
59
presence of Fe by liquid scintillation counting. The a-priori method, refer to Terminology D1129. For terms not defined in
minimum detectable concentration for this test method is 7.4 this test method or in Terminology D1129, refer to other
2 4
Bq/L. published glossaries.
1.2 This test method was developed principally for the
4. Summary of Test Method
55
quantitative determination of Fe. However, after proper cali-
4.1 This test method describes the effective separation of
bration of the liquid scintillation counter with reference stan-
59
iron from the interfering cations of manganese, cobalt,
dards of each nuclide, Fe may also be quantified.
zirconium, niobium, and cesium by anion exchange using acid
1.3 This test method was used successfully with Type III
washes of various molarities. Subsequent elution of the iron is
reagent water conforming to Specification D1193.Itisthe
followed by phosphate precipitation to remove any residual
responsibility of the user to ensure the validity of this test
zinc.The iron phosphate precipitate is dissolved in phosphoric
method for waters of untested matrices.
acidandwaterandmixedwithliquidscintillationcocktail.The
1.4 This standard does not purport to address all of the
chemical yield is determined by the recovery of iron carrier
safety concerns, if any, associated with its use. It is the
using atomic absorption spectrophotometry.Alternatively, any
responsibility of the user of this standard to establish appro-
procedure described in Test Method D1068 may be used, but
priate safety and health practices and determine the applica-
this will need to be validated by the user prior to reporting
bility of regulatory limitations prior to use. For a specific
sample results.
hazard statement, see Section 9.
5. Significance and Use
2. Referenced Documents
5.1 Radioactive iron is produced by neutron activation of
3
2.1 ASTM Standards:
stable iron. Its concentration in reactor coolant is used to
D1068Test Methods for Iron in Water
monitor the corrosion of reactor parts such as reactor fuel-
D1129Terminology Relating to Water
cladding material and reactor structural components.
D1193Specification for Reagent Water
5.2 This technique effectively removes other activation and
D2777Practice for Determination of Precision and Bias of
fission products such as isotopes of iodine, zinc, manganese,
Applicable Test Methods of Committee D19 on Water
cobalt,andcesiumbytheadditionofhold-backcarriersandan
D3370Practices for Sampling Water from Closed Conduits
anion exchange technique. The fission products (zirconium-95
D5847Practice for Writing Quality Control Specifications
and niobium-95) are selectively eluted with hydrochloric-
for Standard Test Methods for Water Analysis
hydrofluoric acid washes. The iron is finally separated from
D7282Practice for Set-up, Calibration, and Quality Control
+2
Zn by precipitation of FePO at a pH of 3.0.
4
of Instruments Used for Radioactivity Measurements
6. Interferences
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
59
6.1 Samples of reactor origin will also contain Fe after
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi-
other radioactive contaminants have been removed by anion
cal Analysis.
59
Current edition approved July 15, 2009. Published August 2009. Originally
exchange (see Fig. 1). Fe is also an activation product which
approved in 1989. Last previous edition approved in 2001 as D4922–01. DOI:
decays by β-γ emission and will be a source of interference in
10.1520/D4922-09.
55
the quantitative determination of Fe. The large difference in
2
Currie, L., “Limits for Qualitative Detection and Quantitative Determination,”
Analytical Chemistry, Vol. 40, 1968, pp. 586–593.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM “American National Standard Glossary of Terms,” Nuclear Science and
Standards volume information, refer to the standard’s Document Summary page on Technology (ANSI N1.1), American National Standards Institute, 1430 Broadway,
the ASTM website. New York, NY 10018.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428
...
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:D4922–01 Designation:D4922–09
Standard Test Method for
1
Determination of Radioactive Iron in Water
This standard is issued under the fixed designation D4922; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
55 59
1.1 This test method covers the determination of Fe in the presence of Fe by liquid scintillation counting. The a-priori
2
minimum detectable concentration for this test method is 7.4 E-3 Bq/mL. Bq/L.
55
1.2 This test method was developed principally for the quantitative determination of Fe. However, after proper calibration of
59
the liquid scintillation counter with reference standards of each nuclide, Fe 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.
2. Referenced Documents
3
2.1 ASTM Standards:
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water
D1193 Specifications for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D-19D19 on Water
3
D3370 Practices for Sampling Water Practices for Sampling Water from Closed Conduits
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D7282 Practice for Set-up, Calibration, and Quality Control of Instruments Used for Radioactivity Measurements
3. Terminology
3.1 Definitions: —ForFor definitions of terms used in this test method, refer to Terminology D1129. For terms not defined in
4
this test method or in Terminology D1129, refer to other published glossaries.
4. Summary of Test Method
4.1 This test method describes the effective separation of iron from the interfering cations of manganese, cobalt, zirconium,
niobium, and cesium by anion exchange using acid washes of various molarities. Subsequent elution of the iron is followed by
phosphate precipitation to remove any residual zinc.The iron phosphate precipitate is dissolved in phosphoric acid and water and
mixed with liquid scintillation cocktail. The chemical yield is determined by the recovery of iron carrier using atomic absorption
spectrophotometryo.Alternatively,anyproceduredescribedinTestMethodD1068maybeused,butthiswillneedtobevalidated
by the user prior to reporting sample results.
5. Significance and Use
5.1 Radioactive iron is produced by neutron activation of stable iron. Its concentration in reactor coolant is used to monitor the
corrosion of reactor parts such as reactor fuel-cladding material and reactor structural components.
5.2 Thistechniqueeffectivelyremovesotheractivationandfissionproductssuchasisotopesofiodine,zinc,manganese,cobalt,
and cesium by the addition of hold-back carriers and an anion exchange technique. The fission products (zirconium-95 and
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemical
Analysis.
´1
Current edition approved Aug. 10, 2001. Published November 2001. Originally published as D4922–89. Last previous edition D4922–94 .
Current edition approved July 15, 2009. Published August 2009. Originally approved in 1989. Last previous edition approved in 2001 as D4922–01.
2
Currie, L., “Limits for Qualitative Detection and Quantitative Determination,” Analytical Chemistry, Vol. 40, 1968, pp. 586–593.
3
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book ofASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
4
“AmericanNationalStandardGlossaryofTerms,” Nuclear Science and Technology (ANSI N1.1),AmericanNationalStandardsInstitute,1430Broadway,NewYork,NY
10018.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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