ASTM D4922-01

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 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.

General Information

• Status: Historical
• Publication Date: 09-Aug-2001
• ICS: 13.060.50 - Examination of water for chemical substances
• ICS: 13.060.60 - Examination of physical properties of water
• Technical Committee: D19 - Water
• Drafting Committee: D19.04 - Methods of Radiochemical Analysis

Relations

• Replaces: ASTM D4922-94e1 - Standard Test Method for Determination of Radioactive Iron in Water
• Effective Date: 10-Aug-2001
• Replaced By: ASTM D4922-09 - Standard Test Method for Determination of Radioactive Iron in Water
• Effective Date: 15-Jul-2009

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4922–01
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Summary of Test Method
55
1.1 This test method covers the determination of Fe in the 4.1 This test method describes the effective separation of
59
presence of Fe by liquid scintillation counting. The a-priori iron from the interfering cations of manganese, cobalt, zirco-
minimum detectable concentration for this test method is 7.4 nium, niobium, and cesium by anion exchange using acid
2
E-3 Bq/mL. washes of various molarities. Subsequent elution of the iron is
1.2 This test method was developed principally for the followed by phosphate precipitation to remove any residual
55
quantitative determination of Fe. However, after proper cali- zinc.The iron phosphate precipitate is dissolved in phosphoric
bration of the liquid scintillation counter with reference stan- acidandwaterandmixedwithliquidscintillationcocktail.The
59
dards of each nuclide, Fe may also be quantified. chemical yield is determined by the recovery of iron carrier
1.3 This test method was used successfully with Type III using atomic absorption spectrophotometry or any procedure
reagent water conforming to Specification D1193.Itisthe described in Test Method D1068.
responsibility of the user to ensure the validity of this test
5. Significance and Use
method for waters of untested matrices.
5.1 Radioactive iron is produced by neutron activation of
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the stable iron. Its concentration in reactor coolant is used to
monitor the corrosion of reactor parts such as reactor fuel-
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- cladding material and reactor structural components.
5.2 This technique effectively removes other activation and
bility of regulatory limitations prior to use. For a specific
hazard statement, see Section 9. fission products such as isotopes of iodine, zinc, manganese,
cobalt,andcesiumbytheadditionofhold-backcarriersandan
2. Referenced Documents
anion exchange technique. The fission products (zirconium-95
2.1 ASTM Standards: and niobium-95) are selectively eluted with hydrochloric-
3
D1068 Test Methods for Iron in Water hydrofluoric acid washes. The iron is finally separated from
3 +2
D1129 Terminology Relating to Water Zn by precipitation of FePO at a pH of 3.0.
4
3
D1193 Specifications for Reagent Water
6. Interferences
D2777 Practice for Determination of Precision and Bias of
59
3
6.1 Samples of reactor origin will also contain Fe after
Applicable Methods of Committee D-19 on Water
3
D3370 Practices for Sampling Water other radioactive contaminants have been removed by anion
59
exchange (see Fig. 1). Fe is also an activation product which
3. Terminology
decays by b-g emission and will be a source of interference in
55
3.1 Definitions—For definitions of terms used in this test the quantitative determination of Fe. The large difference in
method,refertoTerminologyD1129.Fortermsnotdefinedin the energies of their characteristic decay emissions makes it
59
this test method or in Terminology D1129, refer to other possibletodetermineappropriatefactorstocorrectforthe Fe
55
4
published glossaries. spectral cross-talk in the Fe region.
6.2 Quenching, which may be caused by a number of
factors, results in a reduction in the light output from the
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
sample. The subsequent decrease in the spectral pulse height
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi-
will cause variations in the counting efficiency with varying
cal Analysis.
Current edition approvedAug. 10, 2001. Published November 2001. Originally
degrees of quench. For this reason, it is necessary to monitor
e1
published as D4922–89. Last previous edition D4922–94 . 55 59
both the changes in the Fe efficiency and the Fe cross-talk
2
Currie, L., “Limits for Qualitative Detection and Quantitative Determination,”
55
in the Fe region as a function of quench. This technique
Analytical Chemistry, 40, 1968, pp. 586–593.
3
Annual Book of ASTM Standards, Vol 11.01. recommends the use of the automatic external standard ratio
4
“American National Standard Glossary of Terms,” Nuclear Science and
supplied by most liquid scintillation counters to monitor the
Technology (ANSI N1.1), American National Standards Instit
...