ASTM D4922-09(2016)e1

Standard Test Method for Determination of Radioactive Iron in Water

SIGNIFICANCE AND USE
5.1 Fe-55 is formed in reactor coolant systems of nuclear reactors by activation of stable iron. The 55Fe is not completely removed by waste processing systems and some is released to the environment by means of normal waste liquid discharges. Power plants are required to monitor these discharges for 55Fe as well as other radionuclides.  
5.2 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.2  
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: 31-Dec-2015
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
´1
Designation: D4922 − 09 (Reapproved 2016)
Standard Test Method for
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.
ε NOTE—Editorial corrections were made to 5.1 in January 2016.
1. Scope D7282Practice for Set-up, Calibration, and Quality Control
55 of Instruments Used for Radioactivity Measurements
1.1 This test method covers the determination of Fe in the
presence of Fe by liquid scintillation counting. The a-priori
3. Terminology
minimum detectable concentration for this test method is 7.4
3.1 Definitions—For definitions of terms used in this test
Bq/L.
method, refer to Terminology D1129. For terms not defined in
1.2 This test method was developed principally for the
this test method or in Terminology D1129, refer to other
quantitative determination of Fe. However, after proper cali-
published glossaries.
bration of the liquid scintillation counter with reference stan-
dards of each nuclide, Fe may also be quantified.
4. Summary of Test Method
1.3 This test method was used successfully with Type III
4.1 This test method describes the effective separation of
reagent water conforming to Specification D1193.Itisthe
iron from the interfering cations of manganese, cobalt,
responsibility of the user to ensure the validity of this test
zirconium, niobium, and cesium by anion exchange using acid
method for waters of untested matrices.
washes of various molarities. Subsequent elution of the iron is
1.4 This standard does not purport to address all of the
followed by phosphate precipitation to remove any residual
safety concerns, if any, associated with its use. It is the
zinc.The iron phosphate precipitate is dissolved in phosphoric
responsibility of the user of this standard to establish appro-
acidandwaterandmixedwithliquidscintillationcocktail.The
priate safety and health practices and determine the applica-
chemical yield is determined by the recovery of iron carrier
bility of regulatory limitations prior to use. For a specific
using atomic absorption spectrophotometry.Alternatively, any
hazard statement, see Section 9.
procedure described in Test Methods D1068 may be used, but
this will need to be validated by the user prior to reporting
2. Referenced Documents
sample results.
2.1 ASTM Standards:
5. Significance and Use
D1068Test Methods for Iron in Water
D1129Terminology Relating to Water
5.1 Fe-55 is formed in reactor coolant systems of nuclear
D1193Specification for Reagent Water
reactorsbyactivationofstableiron.The Feisnotcompletely
D2777Practice for Determination of Precision and Bias of
removed by waste processing systems and some is released to
Applicable Test Methods of Committee D19 on Water
the environment by means of normal waste liquid discharges.
D3370Practices for Sampling Water from Closed Conduits
Power plants are required to monitor these discharges for Fe
D5847Practice for Writing Quality Control Specifications
as well as other radionuclides.
for Standard Test Methods for Water Analysis
5.2 This technique effectively removes other activation and
fission products such as isotopes of iodine, zinc, manganese,
This test method is under the jurisdiction ofASTM Committee D19 on Water
cobalt,andcesiumbytheadditionofhold-backcarriersandan
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi-
anion exchange technique. The fission products (zirconium-95
cal Analysis.
and niobium-95) are selectively eluted with hydrochloric-
Current edition approved Jan. 1, 2016. Published January 2016. Originally
approved in 1989. Last previous edition approved in 2009 as D4922–09. DOI: hydrofluoric acid washes. The iron is finally separated from
+2
10.1520/D4922-09R16E01.
Zn by precipitation of FePO at a pH of 3.0.
Currie, L., “Limits for Qualitative Detection and Quantitative Determination,”
Analytical Chemistry, Vol. 40, 1968, pp. 586–593.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. 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 19428-2959. United States
´1
D4922 − 09 (2016)
7. Apparatus
7.1 Liquid Scintillation Counter, with an automatic external
standard and multiple energy region of interest (ROI) capabili-
ties.
7.2 GlassScintillationVials,20-mLvialsexhibitingsuitable
optical reproducibility so as not to cause erratic results among
samples.
7.3 Atomic Absorption Spectrophotometer.
7.4 Variable Speed Peristaltic Pump, with controller. Pump
speed should be between 5 and 8 mL/min.
7.5 Centrifuge, using 100 mL centrifuge tubes.
7.6 Volumetric Flasks.
7.7 Anion Exchange Columns:
7.7.1 Columns—Commercially available plastic drying
tubes and ends (40 mLvolume, 1.5 cm diameter, 15 cm long).
7.7.2 Tubing—Pump inlet tubing, approximately 45.7 cm
(18 in.) in length, and pump outlet tubing, approximately 76.2
FIG. 1 Percent of Total Radionuclide Activity Removed Per Acid
cm (30 in.) in length.
Wash
7.7.3 Polyethylene Porous Disc—35-µm pore size and 3.2
mm thick.
8. Reagents and Materials
6. Interferences
8.1 Purity of Reagents—Reagent grade chemicals shall be
usedforalltests.Unlessotherwiseindicated,itisintendedthat
6.1 Samples of reactor origin will also contain Fe after
all reagents shall conform to the specifications of the Commit-
other radioactive contaminants have been removed by anion
tee onAnalytical Reagents of theAmerican Chemical Society,
exchange (see Fig. 1). Fe is also an activation product which
where such specifications are available. Other grades may be
decays by β-γ emission and will be a source of interference in
used, provided it is first ascertained that the reagent is of
the quantitative determination of Fe. The large difference in
sufficiently high purity to permit its use without lessening the
the energies of their characteristic decay emissions makes it
accuracy of the determination.
possibletodetermineappropriatefactorstocorrectforthe Fe
spectral cross-talk in the Fe region.
8.2 Purity of Water—Unless otherwise indicated, references
towatershallbeunderstoodtomeanreagentwaterconforming
6.2 Quenching, which may be caused by a number of
to Specification D1193, Type III.
factors, results in a reduction in light output from the sample.
Thesubsequentdecreaseinthespectralpulseheightwillcause
8.3 Resin—AGl-X8,AG1-X10, 200–400 mesh; 25 mL pre-
variations in the counting efficiency with varying degrees of
viously equilibrated with 125 mL concentrated hydrochloric
quench. For this reason, it is necessary to monitor both the
acid.
55 59
changes in the Fe efficiency and the Fe cross-talk in the
8.4 Scintillation Cocktail—Commercially prepared Insta-
55Fe region as a function of quench. This technique recom-
Gelscintillatororequivalentnon-ionicdetergentscintillatorof
mendstheuseoftheautomaticexternalstandardratiosupplied 6
the octyl-phenyl polyglycol ether type.
by most liquid scintillation counters to monitor the amount of
NOTE 2—To obtain a clear aqueous final sample, the sample volume
quench in a sample.
must be kept below 1.8 mLwith the addition of 15 mLInsta-Gel. It is the
6.3 Thefinalheatingofthesamplesolutionwilldriveoffall
responsibility of the user to determine the optimum sample volume to
cocktail volume to obtain a clear homogeneous solution for any other
excess hydrochloric acid, ammonia, and water. These sub-
liquid scintillation cocktail used.
stances are, therefore, effectively removed as possible quench-
ing agents.
6.4 Scintillation stock or sample solutions which have been
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
exposed to light must be dark adapted to avoid erratic results
listed by the American Chemical Society, see Annual Standards for Laboratory
due to light activation of the scintillator.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
NOTE 1—It is the responsibility of the user to determine the required
MD.
dark adaptation period for the specific cocktail used.
Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime
is Insta-Gel scintillator, available from PerkinElmer Life and Analytical Sciences,
6.5 The stable iron content in a sample will interfere in the
940 Winter Street, Waltham, MA 02451. If you are aware of alternative suppliers,
determination of the chemical recovery. Since the amount of
please provide this information to ASTM International Headquarters. Your com-
stable iron in a sample will depend on its sources, a correction
ments will receive careful consideration at a meeting of the responsible technical
for the iron in the sample must be made. committee, which you may attend.
´1
D4922 − 09 (2016)
8.5 Ammonium Hydroxide(NH OH)—Concentrated (ap- 8.24 Fe Standard Solution—Traceable to a national stan-
proximately 15M) (sp gr 0.90). dards laboratory such as National Institute of Standards and
Technology (NIST) or UK National Physical Laboratory
8.6 Ammonium Phosphate (0.5 M)—Dissolve 66 g of am-
(NPL).
moniummonohydrogenphosphate[(NH ) HPO ]inwaterand
4 2 4
dilute to 1000 mL with water in a volumetric flask.
8.25 Fe Standard Solution—Traceable to a national stan-
dards laboratory such as NIST or NPL.
8.7 Cesium Carrier Solution (1 mg/1 mL)—Cesium as
cesium chloride (CsCl) in dilute hydrochloric acid.
9. Hazards
8.8 Cobalt Carrier Solution (1 mg/1 mL)—Cobalt as cobalt
9.1 HF is extremely hazardous and should be used in a
chloride (CoCl ) in dilute hydrochloric acid.
well-ventilated hood. Wear rubber gloves, safety glasses or
8.9 Hydrochloric Acid (sp gr 1.187)—Concentrated HCl.
goggles,andalaboratorycoat.AvoidbreathinganyHFfumes.
8.10 Hydrochloric Acid 10 M—Dilute 833 mL of concen-
Clean all spills and wash thoroughly after using HF. Also, do
trated hydrochloric acid in 100 mL water and dilute to 1000
not add HF to any glassware for it is a significant hazard and
mL with water in a volumetric flask.
can affect analytical accuracy.
8.11 Hydrochloric Acid 6 M—Dilute 500 mL of concen-
10. Sampling
tratedhydrochloricacidin400mLofwater,diluteto1000mL
with water in a volumetric flask.
10.1 Collect samples in accordance with procedures pre-
sented in Practices D3370, as applicable.
8.12 Hydrochloric Acid 4 M—Dilute 333 mL of concen-
tratedhydrochloricacidin600mLofwater,diluteto1000mL
10.2 If the sample is not acidified at the time of collection,
with water in a volumetric flask.
20mLofconcentratedHClorHNO shouldbeaddedper1000
8.13 Hydrochloric Acid 0.5 M—Dilute 42 mL of concen- mL of sample. After acidification of the sample, the sample
should be allowed to sit overnight prior to analysis.
tratedhydrochloricacidin900mLofwater,diluteto1000mL
with water in a volumetric flask.
11. Calibration
8.14 Hydrochloric Acid 0.01 M—Dilute 20 mL of 0.5 M
HCl in 900 mL of water, dilute to 1000 mL with water in a
11.1 The reference standard for both iron isotopes will
volumetric flask. contain 5 mg iron carrier. Add 6 drops of concentrated
phosphoric acid to the carrier solution and heat on a hot plate
8.15 Hydrochloric (6 M)-Hydrofluoric Acid (0.5 M)—
until it clears. This will drive off any excess hydrochloric acid
Dilute 500 mL of concentrated hydrochloric acid (HCl) (sp gr
and water (to less than 0.5 mL but do not allow to bake dry).
1.187)and20mLof49%concentratedhydrofluoricacid(HF)
Add1mLofwaterandswirlintheglassvial.Thisfinalcarrier
in 400 mL of water, dilute to 1000 mL with water in a plastic
solutionshouldbecolorless.Coolthevialtoroomtemperature.
or TFE-fluorocarbon volumetric flask.
Spike with the appropriate isotope and add 15 mL of scintil-
+3 7
8.16 Iron Carrier Solution (Fe as ferric chloride) —
lation cocktail. Cap and shake until the mixture is clear; this
Dissolve 5.00 g of metallic iron in 300 mL of 6 M HCl, filter,
step ensures that the proper sample volume to scintillation
dilute to 1 L, and calibrate using an atomic absorption
cocktail volume ratio is obtained for a clear, homogeneous
spectrophotometer (Test Methods D1068).
solution. The volume of the reference standard should be such
+2
8.17 Manganese Carrier Solution (1 mg/1 mL)—Mn in that its addition to the sample does not cause additional
dilute nitric acid (HNO ). quench.
+5
8.18 Niobium Carrier Solution (1 mg/1 mL)—Nb in 5%
11.2 Prepare a series of quenched Fe standards and a
7 59
hydrofluoric acid (1+9 M).
seriesofquenched Festandardsusingvariousweightsofiron
carrier or concentration or volumes, or both, of acid. Use the
8.19 Nitric Acid (sp gr 1.42)—Concentrated (HNO ).
least quenched standards in each set to optimize the liquid
8.20 Phosphoric Acid (sp gr 1.834)—Concentrated
scintillationcounter(LSC)discriminatorsettingsandamplifier
(H PO ). 55
3 4
gain. Ensure that the Fe spectrum does not spill over into
8.21 Sodium Hydroxide (6 M)—Dissolve 24 g sodium hy- the Fe ROI. If your instrument does not allow for multiple
droxide (NaOH) in 90 mL water, allow to cool, and dilute to nuclides to be optimized follow Practice D7282 for instrument
100 mLwith water and store in plastic bottles; a commercially optimization.
prepared solution may also be used.
11.3 Count each set of standards with the LSC automatic
+2
8.22 Zinc Carrier Solution (1 mg/mL)—Zn in dilute
externalstandardratioselectedontoobtainapproximately1%
hydrochloric acid.
counting statistics (approximately 10 000 counts) in the ROI.
+4
8.23 Zirconium Carrier Solution (1 mg/mL)—Zr in dilute
11.4 Prepare a curve of the Fe efficiency versus the
hydrochloric acid.
external standard ratio.
11.5 Prepare a crosstalk (XT) curve of the ratio of Fe
55 59 59
counts in the Fe ROI to the Fe counts in the Fe ROI
Commercially available atomic absorption reference standards in 1 mg=1mL
concentrations may be used as carriers. versus the external standard ratio.
´1
D4922 − 09 (2016)
11.6 Additional guidance on the set-up, calibration and 12.12 Calculate the ratio (Eq 2), the amount remaining
calibratio
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D4922 − 09 D4922 − 09 (Reapproved 2016)
Standard Test Method for
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial corrections were made to 5.1 in January 2016.
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
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 Fe. However, after proper calibration of
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
2.1 ASTM Standards:
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 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—For definitions of terms used in this test method, refer to Terminology D1129. For terms not defined in 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
spectrophotometry. Alternatively, any procedure described in Test MethodMethods D1068 may be used, but this will need to be
validated by the user prior to reporting sample results.
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.
Current edition approved July 15, 2009Jan. 1, 2016. Published August 2009January 2016. Originally approved in 1989. Last previous edition approved in 20012009 as
D4922 – 01.D4922 – 09. DOI: 10.1520/D4922-09.10.1520/D4922-09R16E01.
Currie, L., “Limits for Qualitative Detection and Quantitative Determination,” Analytical Chemistry, Vol. 40, 1968, pp. 586–593.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
“American National Standard Glossary of Terms,” Nuclear Science and Technology (ANSI N1.1), American National Standards Institute, 1430 Broadway, New York, NY
10018.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D4922 − 09 (2016)
FIG. 1 Percent of Total Radionuclide Activity Removed Per Acid Wash
5. Significance and Use
5.1 Radioactive iron is produced by neutron Fe-55 is formed in reactor coolant systems of nuclear reactors by activation of
stable iron. ItsThe concentration in reactor coolant is used to monitor the corrosion of reactor parts such Fe is not completely
removed by waste processing systems and some is released to the environment by means of normal waste liquid discharges. Power
plants are required to monitor these discharges for as reactor fuel-cladding material and reactor structural components.Fe as well
as other radionuclides.
5.2 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
+2
niobium-95) are selectively eluted with hydrochloric-hydrofluoric acid washes. The iron is finally separated from Zn by
precipitation of FePO at a pH of 3.0.
6. Interferences
6.1 Samples of reactor origin will also contain Fe after other radioactive contaminants have been removed by anion exchange
(see Fig. 1). Fe is also an activation product which decays by β-γ emission and will be a source of interference in the quantitative
determination of Fe. The large difference in the energies of their characteristic decay emissions makes it possible to determine
59 55
appropriate factors to correct for the Fe spectral cross-talk in the Fe region.
6.2 Quenching, which may be caused by a number of factors, results in a reduction in light output from the sample. The
subsequent decrease in the spectral pulse height will cause variations in the counting efficiency with varying degrees of quench.
55 59 55
For this reason, it is necessary to monitor both the changes in the Fe efficiency and the Fe cross-talk in the Fe region as a
function of quench. This technique recommends the use of the automatic external standard ratio supplied by most liquid
scintillation counters to monitor the amount of quench in a sample.
6.3 The final heating of the sample solution will drive off all excess hydrochloric acid, ammonia, and water. These substances
are, therefore, effectively removed as possible quenching agents.
6.4 Scintillation stock or sample solutions which have been exposed to light must be dark adapted to avoid erratic results due
to light activation of the scintillator.
NOTE 1—It is the responsibility of the user to determine the required dark adaptation period for the specific cocktail used.
6.5 The stable iron content in a sample will interfere in the determination of the chemical recovery. Since the amount of stable
iron in a sample will depend on its sources, a correction for the iron in the sample must be made.
7. Apparatus
7.1 Liquid Scintillation Counter, with an automatic external standard and multiple energy region of interest (ROI) capabilities.
7.2 Glass Scintillation Vials, 20-mL vials exhibiting suitable optical reproducibility so as not to cause erratic results among
samples.
7.3 Atomic Absorption Spectrophotometer.
´1
D4922 − 09 (2016)
7.4 Variable Speed Peristaltic Pump, with controller. Pump speed should be between 5 and 8 mL/min.
7.5 Centrifuge, using 100 mL centrifuge tubes.
7.6 Volumetric Flasks.
7.7 Anion Exchange Columns:
7.7.1 Columns—Commercially available plastic drying tubes and ends (40 mL volume, 1.5 cm diameter, 15 cm long).
7.7.2 Tubing—Pump inlet tubing, approximately 45.7 cm (18 in.) in length, and pump outlet tubing, approximately 76.2 cm (30
in.) in length.
7.7.3 Polyethylene Porous Disc—35-μm pore size and 3.2 mm thick.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used for all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193, Type III.
8.3 Resin—AGl-X8, AG1-X10, 200–400 mesh; 25 mL previously equilibrated with 125 mL concentrated hydrochloric acid.
8.4 Scintillation Cocktail—Commercially prepared Insta-Gel scintillator or equivalent non-ionic detergent scintillator of the
octyl-phenyl polyglycol ether type.
NOTE 2—To obtain a clear aqueous final sample, the sample volume must be kept below 1.8 mL with the addition of 15 mL Insta-Gel. It is the
responsibility of the user to determine the optimum sample volume to cocktail volume to obtain a clear homogeneous solution for any other liquid
scintillation cocktail used.
8.5 Ammonium Hydroxide (NH OH)—Concentrated (approximately 15M) (sp gr 0.90).
8.6 Ammonium Phosphate (0.5 M)—Dissolve 66 g of ammonium monohydrogen phosphate [(NH ) HPO ] in water and dilute
4 2 4
to 1000 mL with water in a volumetric flask.
8.7 Cesium Carrier Solution (1 mg/1 mL)—Cesium as cesium chloride (CsCl) in dilute hydrochloric acid.
8.8 Cobalt Carrier Solution (1 mg/1 mL)—Cobalt as cobalt chloride (CoCl ) in dilute hydrochloric acid.
8.9 Hydrochloric Acid (sp gr 1.187)—Concentrated HCl.
8.10 Hydrochloric Acid 10 M—Dilute 833 mL of concentrated hydrochloric acid in 100 mL water and dilute to 1000 mL with
water in a volumetric flask.
8.11 Hydrochloric Acid 6 M—Dilute 500 mL of concentrated hydrochloric acid in 400 mL of water, dilute to 1000 mL with
water in a volumetric flask.
8.12 Hydrochloric Acid 4 M—Dilute 333 mL of concentrated hydrochloric acid in 600 mL of water, dilute to 1000 mL with
water in a volumetric flask.
8.13 Hydrochloric Acid 0.5 M—Dilute 42 mL of concentrated hydrochloric acid in 900 mL of water, dilute to 1000 mL with
water in a volumetric flask.
8.14 Hydrochloric Acid 0.01 M—Dilute 20 mL of 0.5 M HCl in 900 mL of water, dilute to 1000 mL with water in a volumetric
flask.
8.15 Hydrochloric—Hydrochloric (6 M)-Hydrofluoric Acid (0.5 M)—Dilute 500 mL of concentrated hydrochloric acid (HCl)
(sp gr 1.187) and 20 mL of 49 % concentrated hydrofluoric acid (HF) in 400 mL of water, dilute to 1000 mL with water in a plastic
or TFE-fluorocarbon volumetric flask.
+3 7
8.16 Iron Carrier Solution (Fe as ferric chloride) —Dissolve 5.00 g of metallic iron in 300 mL of 6 M HCl, filter, dilute to
1 L, and calibrate using an atomic absorption spectrophotometer (Test Methods D1068).
+2 7
8.17 Manganese Carrier Solution (1 mg/1 mL)—Mn in dilute nitric acid (HNO ).
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
The sole source of supply of the apparatus known to the committee at this time is Insta-Gel scintillator, available from PerkinElmer Life and Analytical Sciences, 940
Winter Street, Waltham, MA 02451. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive
careful consideration at a meeting of the responsible technical committee, which you may attend.
Commercially available atomic absorption reference standards in 1 mg = 1 mL concentrations may be used as carriers.
´1
D4922 − 09 (2016)
+5 7
8.18 Niobium Carrier Solution (1 mg/1 mL)—Nb in 5 % hydrofluoric acid (1 + 9 M).
8.19 Nitric Acid (sp gr 1.42)—Concentrated (HNO ).
8.20 Phosphoric Acid (sp gr 1.834)—Concentrated (H PO ).
3 4
8.21 Sodium Hydroxide (6 M)—Dissolve 24 g sodium hydroxide (NaOH) in 90 mL water, allow to cool, and dilute to 100 mL
with water and store in plastic bottles; a commercially prepared solution may also be used.
+2 7
8.22 Zinc Carrier Solution (1 mg/mL)—Zn in dilute hydrochloric acid.
+4 7
8.23 Zirconium Carrier Solution (1 mg/mL)—Zr in dilute hydrochloric acid.
8.24 Fe Standard Solution—Traceable to a national standards laboratory such as National Institute of Standards and
Technology (NIST) or UK National Physical Laboratory (NPL).
8.25 Fe Standard Solution—Traceable to a national standards laboratory such as NIST or NPL.
9. Hazards
9.1 HF is extremely hazardous and should be used in a well-ventilated hood. Wear rubber gloves, safety glasses or goggles, and
a laboratory coat. Avoid breathing any HF fumes. Clean all spills and wash thoroughly after using HF. Also, do not add HF to any
glassware for it is a significant hazard and can affect analytical accuracy.
10. Sampling
10.1 Collect samples in accordance with procedures presented in Practices D3370, as applicable.
10.2 If the sample is not acidified at the time of collection, 20 mL of concentrated HCl or HNO should be added per 1000 mL
of sample. After acidification of the sample, the sample should be allowed to sit overnight prior to analysis.
11. Calibration
11.1 The reference standard for both iron isotopes will contain 5 mg iron carrier. Add 6 drops of concentrated phosphoric acid
to the carrier solution and heat on a hot plate until it clears. This will drive off any excess hydrochloric acid and water (to less than
0.5 mL but do not allow to bake dry). Add 1 mL of water and swirl in the glass vial. This final carrier solution should be colorless.
Cool the vial to room temperature. Spike with the appropriate isotope and add 15 mL of scintillation cocktail. Cap and shake until
the mixture is clear; this step ensures that the proper sample volume to scintillation cocktail volume ratio is obtained for a clear,
homogeneous solution. The volume of the reference standard should be such that its addition to the sample does not cause
additional quench.
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11.2 Prepare a series of quenched Fe standards and a series of quenched Fe standards using various weights of iron carrier
or concentration or volumes, or both, of acid. Use the least quenched standards in each set to optimize the liquid scintillation
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