ASTM D8026-16

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D8026 − 16
Standard Practice for
Determination of Tc-99 in Water by Inductively Coupled
Plasma Mass Spectrometry (ICP-MS)
This standard is issued under the fixed designation D8026; 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.
1. Scope 3. Terminology
1.1 Technetium is separated and concentrated from a water
3.1 Definitions:
sample by extraction chromatography using its chemical
3.1.1 For definitions of terms used in this standard, refer to
analog,rhenium,asatracer.Theratiooftechnetiumtorhenium
Terminologies D1129 and D7902.
is measured by inductively coupled plasma mass spectrometry
(ICP-MS) to then quantify the Tc concentration.
4. Summary of Practice
1.1.1 This practice is provided as an alternative to Test
4.1 Aknown quantity of Re is added to a known volume of
Method D7168 which provides for a different separation media
afilteredwatersample.Thesampleisheatedinthepresenceof
geometry and measurement by liquid scintillation spectrom-
peroxide to ensure the Tc and Re are in the oxidized form. The
etry. Similar detection limits should be attainable by this
Tc and Re are then extracted from the sample using an
method.
3, 4
extraction chromatography resin loaded in a column. The
1.2 The values stated in SI units are to be regarded as
resin is rinsed of some co-retained elements and then the Tc
standard. No other units of measurement are included in this
and Re are co-eluted from the resin.
standard.
4.2 An ICP-MS is used to determine the ratio of Tc relative
1.3 This standard does not purport to address all of the
to the Re tracer; the Re is used as an internal standard to
safety concerns, if any, associated with its use. It is the
monitor instrument response as well as to correct for chemical
responsibility of the user of this standard to establish appro-
yield of the Tc through the column separation.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents 5.1 Technetium-99 is produced by the fission of uranium
and plutonium, and has been released to the environment via
2.1 ASTM Standards:
nuclear weapons testing and nuclear materials processing. In
C1387 Guide for the Determination of Technetium-99 in
an oxidizing environment, it exists as the very mobile pertech-
Soil
–
netate ion, TcO , which is an analog to nitrate and can be
D1129 Terminology Relating to Water
taken up by living organisms. Monitoring of Tc in waters
D1193 Specification for Reagent Water
around nuclear processing facilities is part of a complete
D2777 Practice for Determination of Precision and Bias of
environmental monitoring program.
Applicable Test Methods of Committee D19 on Water
D5847 Practice for Writing Quality Control Specifications
5.2 Technetium-99 is a long-lived (half-life 2.1E+5years),
for Standard Test Methods for Water Analysis
weak beta (maximum beta energy of 293 keV) emitting
D7168 Test Method for Tc in Water by Solid Phase Extrac-
radioisotope. There are no stable isotopes of Tc. Thus the
tion Disk
determination of its activity concentration presents unique
D7902 Terminology for Radiochemical Analyses
challenges to traditional radiochemical determination methods.
This method provides an alternative to the spiked/unspiked
replicate method of Method D7168 and uses options presented
This practice is under the jurisdiction ofASTM Committee D19 on Water and
in Guide C1387 for the determination of Tc in soil.
is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemical
Analysis.
Current edition approved Feb. 15, 2016. Published March 2016. DOI: 10.1520/
D8026-16.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Tagami, K., and Uchida, S., Analytica Chimica Acta, Vol 405, 2000, pp.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 227–229.
Standards volume information, refer to the standard’s Document Summary page on Kabai, E., Beyermann, M., Seeger, J., Savkin, B. T., Stanglmaier, S., and
the ASTM website. Hiersche, L., Applied Radiation and Isotopes, Vol 81, 2013, pp. 6–41.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8026 − 16
6. Interferences 8.3 Extraction chromatography resin, an aliphatic quater-
nary amine which is mainly used for Tc analysis as well as for
6.1 Any element with a mass-to-charge ratio (m/z) of 99
6, 7
the separation of tetravalent actinides.
(that is, naturally occurring isotope of Ru, or other artificially
NOTE 1—If using the purchased prepared resin, the large particle size
produced elements of sufficient half-life with similar m/z) can
should be used; back extraction from the small particle resin may not be
interfere when using mass spectrometry for quantification of
equivalent for the Tc and the Re.
the Tc activity.Any element with the same m/z as the isotope
8.4 Prefilter Resin, anonionic acrylic ester polymer resin
used as an isotope dilution tracer or internal standard, that is,
used to remove residual organic matter prior to the extraction
m/z of 185 or 187, will cause a bias in the yield correction.
chromatography resin column.
Corrections should be included in the mass spectrometry data
8.5 Hydrogen Peroxide, 30 %.
reduction for known interferences.
8.6 Nitric Acid (16M HNO ), concentrated, specific gravity
6.2 High levels of nitrate in the sample could lead to
1.42, high purity.
saturating the active sites on the resin and cause low recovery
8.7 1M Nitric Acid—Add 63 mL of HNO (8.6) to 900 mL
of the Tc and Re. They should be equally affected by this and
of water, dilute to a final volume of 1 L.
therefore observed as a low signal for the Re in the ICP-MS
analysis.
8.8 8M Nitric Acid—Add 500 mLof HNO (8.6) to 400 mL
of water, dilute to a final volume of 1 L.
6.3 Most other elements will not be retained by the extrac-
tion resin at the low acidity suggested in this practice.The user 8.9 Rhenium tracer solution, commercially available as a
mass spectrometry solution standard, diluted to a known
should determine if any elements exist at high enough concen-
volume to provide the desired mass to the test sample in a
trationtoaffecttheretentionoftheTcandRe,andiftheycause
convenient delivery volume.
a bias in the effective retention of the two elements of interest.
8.10 Technetium-99 standard solution, traceable solution,
7. Apparatus
dilutedtoausefulactivityconcentration,formethodvalidation
and instrument calibration.Available from commercial suppli-
7.1 Extraction column, a standard geometry column to hold
ers of radioactive materials.
~2 mL of resin and allow connection to an extension funnel.
9. Hazards
7.2 Column extension funnels, that can be added to the
extraction column such that a few hundred mL of solution can
9.1 Use extreme caution when handling all acids. They are
be added to the column at one time.
extremely corrosive, and skin contact could result in severe
burns.
7.3 Column rack, holds columns such that several extrac-
9.2 When diluting concentrated acids, always use safety
tions can be performed simultaneously.
glasses and protective clothing, and add the acid to the water.
7.4 Vacuum pump, vacuum box, or other vacuum filtration
apparatus (optional)—to facilitate the flow through the col-
10. Procedure
umn.
10.1 The following steps are provided as guidance for
performing this Practice. The laboratory should define finite
7.5 Inductively Coupled–Plasma Mass Spectrometer, with
values when performing method validation and sample testing.
all associated hardware and software for sample analysis.
10.1.1 Collect a water sample according to prescribed
methods. The sample should be analyzed within a few days of
8. Reagents
collectionorpreservedbyrefrigerationatlessthan6°C,butnot
8.1 Purity of Reagents—All chemicals should, at a
freezing, until analysis. The sample should be filtered prior to
minimum, be of reagent grade and should conform to the
analysis to remove debris that could adversely impact the
specifications of the Committee on Analytical Reagents of the
column flow.
American Chemical Society where such specifications are
10.1.2 Transfer a known volume of water, up to 1 L, to a
available. High Purity reagents are suggested when mass
large glass beaker. Add a known amount of Re as the tracer,
spectrometry is the detection method.
nominally 10 ng, to the beaker. Add ~10 mL of hydrogen
peroxide and heat the sample to ~80°C with stirring for a few
8.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water, as defined
by Type III of Specification D1193.
The sole source in the United States of the Eichrom TEVA resin known to the
committeeatthistimeisEichromTechnologies,LLC,inLisle,IL,60532,anditcan
be purchased from the appropriate vender based on international location. If you are
aware of alternative suppliers, please provide this information to ASTM Interna-
Reagent Chemicals, American Chemical Society Specifications, American tional Headquarters.Your comments will receive careful consideration at a meeting
Chemical Society, Washington, DC. For suggestions on the testing of reagents not of the responsible technical committee
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