ASTM C1387-23

Standard Guide for the Determination of Technetium-99 in Soil

SIGNIFICANCE AND USE
5.1 This guide offers several options for the determination of 99Tc in soil samples. Sample sizes of up to 200 g are possible, depending on the method chosen to extract Tc from the soil matrix. It is up to the user to determine if it is appropriate for the intended use of the final data.
SCOPE
1.1 This guide is intended to serve as a reference for laboratories wishing to perform 99Tc analyses in soil. Several options are given for selection of a tracer and for the method of extracting the Tc from the soil matrix. Separation of Tc from the sample matrix is performed using an extraction chromatography resin. Options are then given for the determination of the 99Tc activity in the original sample. It is up to the user to determine which options are appropriate for use, and to generate acceptance data to support the chosen procedure.  
1.2 Due to the various extraction methods available, various tracers used, variable detection methods used, and lack of certified reference materials for 99Tc in soil, there is insufficient data to support a single method written as a standard method.  
1.3 The values stated in SI units are to be regarded as standard, except where the non-SI unit of molar, M, is used for the concentration of chemicals and reagents. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

General Information

• Status: Published
• Publication Date: 31-Dec-2022
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C998-17 - Standard Practice for Sampling Surface Soil for Radionuclides
• Effective Date: 01-Jun-2017
• Refers: ASTM C999-17 - Standard Practice for Soil Sample Preparation for the Determination of Radionuclides
• Effective Date: 01-Jun-2017
• Refers: ASTM D8026-16 - Standard Practice for Determination of Tc-99 in Water by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
• Effective Date: 15-Feb-2016
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jan-2014
• Refers: ASTM E11-13 - Standard Specification for Woven Wire Test Sieve Cloth and Test Sieves
• Effective Date: 01-Oct-2013
• Refers: ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jun-2013
• Refers: ASTM C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013
• Refers: ASTM D7168-11e1 - Standard Test Method for ⁹⁹Tc in Water by Solid Phase Extraction Disk
• Effective Date: 15-May-2011
• Refers: ASTM D7168-11 - Standard Test Method for ⁹⁹Tc in Water by Solid Phase Extraction Disk
• Effective Date: 15-May-2011
• Refers: ASTM C859-10b - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Nov-2010
• Refers: ASTM C859-10a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Aug-2010
• Refers: ASTM C999-05(2010)e1 - Standard Practice for Soil Sample Preparation for the Determination of Radionuclides
• Effective Date: 01-Jun-2010
• Refers: ASTM C998-05(2010)e1 - Standard Practice for Sampling Surface Soil for Radionuclides
• Effective Date: 01-Jun-2010

Overview

ASTM C1387-23, "Standard Guide for the Determination of Technetium-99 in Soil," provides comprehensive guidance for laboratories analyzing technetium-99 (^99Tc) in soil samples. Developed by ASTM International, this guide addresses multiple methods for extracting, purifying, and quantifying ^99Tc, a long-lived, mobile radionuclide produced through uranium and plutonium fission. The standard outlines procedures suited for various analytical objectives and emphasizes user responsibility in selecting appropriate methods and generating validation data for project-specific requirements.

This guide is essential for laboratories, remediation specialists, and environmental monitoring professionals seeking reliable, standardized approaches for ^99Tc soil analysis.

Key Topics

ASTM C1387-23 covers the following critical topics:

• Sample Preparation: Procedures for collecting, drying, homogenizing, and preparing soil samples, including optional steps such as ashing to remove organic matter.
• Extraction Methods: Detailed options for extracting technetium from soil matrices, including acid leaching, soil fusion, and microwave digestion. Each method allows for flexibility in sample size (up to 200 grams) and reagents.
• Purification: Use of extraction chromatography resin columns to separate ^99Tc from soil extracts. Pre-filtering is recommended for samples with significant organic content.
• Quantification Techniques: Instructions for determining ^99Tc activity by liquid scintillation spectrometry (LSC) and inductively coupled plasma mass spectrometry (ICP-MS). The guide highlights common challenges such as interferences and the lack of certified reference materials.
• Tracer Selection: Guidance on selecting suitable yield monitors, including radioisotope tracers (^95mTc, ^99mTc, ^97Tc) and rhenium as an internal standard for ICP-MS procedures.
• Interference Management: Strategies for identifying and correcting for analytical interferences due to similar radionuclides or mass-to-charge overlaps in mass spectrometric analyses.
• Safety and Compliance: Reminders that users are responsible for maintaining safety, health, and environmental practices and ensuring regulatory compliance.

Applications

The practical applications of ASTM C1387-23 include:

• Environmental Monitoring: Measurement of technetium-99 in soils for environmental risk assessment near nuclear facilities or areas impacted by nuclear waste.
• Remediation Projects: Supporting soil cleanup and remediation efforts by accurately documenting ^99Tc contamination levels.
• Nuclear Decommissioning: Used in site characterization and ongoing monitoring during the decommissioning of nuclear plants.
• Research and Development: Provides a reference for academic and industrial laboratories conducting studies related to radioactive contamination in soils.
• Regulatory Compliance: Assists organizations in meeting government or international requirements for radiological site assessments.

Related Standards

ASTM C1387-23 references several other standards, enhancing its value in integrated laboratory workflows:

• ASTM C859 - Terminology Relating to Nuclear Materials
• ASTM C998 - Practice for Sampling Surface Soil for Radionuclides
• ASTM C999 - Practice for Soil Sample Preparation for the Determination of Radionuclides
• ASTM D1193 - Specification for Reagent Water
• ASTM D7168 - Test Method for ^99Tc in Water by Solid Phase Extraction Disk
• ASTM D8026 - Practice for Determination of ^99Tc in Water by ICP-MS
• ASTM E11 - Specification for Woven Wire Test Sieve Cloth and Test Sieves

These related standards support quality assurance, procedural consistency, and accurate reporting for radionuclide analysis in complex environmental matrices.

---

Keywords: technetium-99, ASTM C1387-23, soil analysis, extraction chromatography, liquid scintillation spectrometry, mass spectrometry, environmental monitoring, radionuclide determination, nuclear site remediation, sample preparation

Standards Content (Sample)

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: C1387 − 23
Standard Guide for
the Determination of Technetium-99 in Soil
This standard is issued under the fixed designation C1387; 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 C998 Practice for Sampling Surface Soil for Radionuclides
C999 Practice for Soil Sample Preparation for the Determi-
1.1 This guide is intended to serve as a reference for
99 nation of Radionuclides
laboratories wishing to perform Tc analyses in soil. Several
D1193 Specification for Reagent Water
options are given for selection of a tracer and for the method of
D7168 Test Method for Tc in Water by Solid Phase Extrac-
extracting the Tc from the soil matrix. Separation of Tc from
tion Disk
the sample matrix is performed using an extraction chroma-
D8026 Practice for Determination of Tc-99 in Water by
tography resin. Options are then given for the determination of
99 Inductively Coupled Plasma Mass Spectrometry (ICP-
the Tc activity in the original sample. It is up to the user to
MS)
determine which options are appropriate for use, and to
E11 Specification for Woven Wire Test Sieve Cloth and Test
generate acceptance data to support the chosen procedure.
Sieves
1.2 Due to the various extraction methods available, various
tracers used, variable detection methods used, and lack of
3. Terminology
certified reference materials for Tc in soil, there is insufficient
3.1 For definitions of terms in this guide, refer to Terminol-
data to support a single method written as a standard method.
ogy C859.
1.3 The values stated in SI units are to be regarded as
standard, except where the non-SI unit of molar, M, is used for
4. Summary of Guide
the concentration of chemicals and reagents. The values given
4.1 There are no stable isotopes of technetium.
in parentheses after SI units are provided for information only
Technetium-99 is produced by the fission of uranium and
and are not considered standard.
plutonium, and has been released to the environment via
1.4 This standard does not purport to address all of the
nuclear weapons testing and nuclear materials processing. In
safety concerns, if any, associated with its use. It is the
an oxidizing environment, it exists as the very mobile pertech-
responsibility of the user of this standard to establish appro- –
netate ion, TcO . Technetium-99 is a long-lived (half-life of
priate safety, health, and environmental practices and deter-
2.1 E+5 years), weak beta (maximum beta energy of 293 keV)
mine the applicability of regulatory limitations prior to use.
emitting radioisotope.
1.5 This international standard was developed in accor-
4.2 For the analysis of Tc in soil, a tracer is added to the
dance with internationally recognized principles on standard-
sample matrix, or spiked duplicate samples are prepared, and
ization established in the Decision on Principles for the
then the Tc is extracted from the soil matrix by one of several
Development of International Standards, Guides and Recom-
methods, including acid leaching or one of various fusion
mendations issued by the World Trade Organization Technical
methods. The resulting solution is passed through an extraction
Barriers to Trade (TBT) Committee.
chromatography column. Technetium is known to be retained
by the extraction chromatography material while most other
2. Referenced Documents
2 elements pass through the column. The column is washed with
2.1 ASTM Standards:
dilute acid to remove any remaining interferents. The resin
C859 Terminology Relating to Nuclear Materials
may then be counted directly by adding it to a liquid scintil-
lation cocktail and counting by liquid scintillation
This guide is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel spectrometry, or the Tc may be eluted from the resin for
Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
alternative counting or mass spectrometric techniques.
Current edition approved Jan. 1, 2023. Published March 2023. Originally
approved in 1998. Last previous edition approved in 2014 as C1387 – 14. DOI:
5. Significance and Use
10.1520/C1387-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.1 This guide offers several options for the determination
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
of Tc in soil samples. Sample sizes of up to 200 g are
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. possible, depending on the method chosen to extract Tc from
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1387 − 23
the soil matrix. It is up to the user to determine if it is 8.2 Purity of Water—Unless otherwise indicated, references
appropriate for the intended use of the final data. to water shall be understood to mean reagent water, as defined
by Type I of Specification D1193.
6. Interferences
8.3 Tracer:
6.1 Any radionuclide not completely removed by the ex-
8.3.1 Isotope Dilution Yield Determination:
traction chromatography column that has a beta decay energy
95m 99m 4
8.3.1.1 Radiometric Yield Determination— Tc or Tc
similar to or higher than Tc will interfere when counting
have been used to monitor the chemical yield of the extraction
techniques are used for quantification of the Tc activity.
and purification of Tc prior to quantification. [Example: Add
99m
6.2 Any elements with a mass-to-charge ratio (m/z) of 99
370 Bq (10 nCi) of Tc as a yield tracer when determining
(that is, naturally occurring isotope of Ru or other artificially
yield by gamma spectrometry.]
produced elements of sufficient half-life with similar m/z) can
8.3.1.2 Mass Spectrometric Yield Determination— Tc may
interfere when using mass spectrometry for quantification of
be produced in a nuclear reactor in very limited quantities to be
the Tc mass activity. Any element with the same m/z as the
used as an isotope dilution tracer for the mass spectrometric
isotope used as an isotope dilution tracer or internal standard 99 5 97
determination of Tc (1). [Example: Add 1 ng of Tc as a
will cause a bias in the yield correction. Corrections should be
yield tracer for mass spectrometry.]
included in the mass spectrometry data reduction for known
8.3.1.3 Rhenium as a Mass Spectrometric Yield Monitor—
interferences.
The chemical behavior of Re and Tc are similar enough on the
6.3 Additional interferences may be encountered, depend-
extraction resin that Re may be used as a tracer for Tc when
ing on the tracer and measurement technique chosen. It is up to
using ICP-MS as a detection method (2). Practice D8026
the user to determine and correct for any additional interfer-
provides additional information on this option.
ences.
8.3.2 Duplicate Sample Analysis to Monitor Chemical
Yield:
7. Apparatus
8.3.2.1 Duplicate samples may be analyzed, one spiked with
7.1 Apparatus for the Extraction of Tc from Sample Matrix:
a known amount of Tc and one unspiked. The chemical
7.1.1 See the individual extraction method descriptions to
recovery of the spiked sample is then used to correct the
compile a list of the equipment needed for the chosen extrac-
unspiked sample to obtain the original sample activity. (See
tion method.
Test Method D7168 for an example of this method.)
7.2 Apparatus for the Purification of Tc from the Soil 99
8.4 Reagents for the Extraction of Tc from Sample Matrix:
Extract:
8.4.1 See the individual extraction method descriptions to
7.2.1 Extraction column—with a bed volume of several
compile a list of the reagents needed for the chosen extraction
milliliters for the extraction chromatography resin.
method.
7.2.2 Column extension funnels—that can be added to the
8.5 Reagents for the Purification of Tc from the Sample
extraction column such that a few hundred milliliters of
Matrix:
solution can be added to the column at one time.
8.5.1 Extraction Chromatrography Resin—TEVA Resin.
7.2.3 Column rack—holds columns such that several extrac-
tions can be performed simultaneously.
8.5.2 Prefilter Resin—a nonionic acrylic ester polymer resin
used to remove residual organic matter prior to the extraction
7.3 Apparatus for the Quantification of Tc:
chromatography resin column.
7.3.1 See the individual detection method descriptions to
8.5.3 Hydrogen Peroxide—30 %.
compile a list of the equipment needed for the chosen detection
8.5.4 Nitric Acid—(16 M HNO ) concentrated, specific
method.
gravity 1.42.
8. Reagents
8.5.5 1 M Nitric Acid—Add 64 mL of concentrated HNO
(15.7 M, mass fraction of 70.0 %) to 900 mL of water, dilute to
8.1 Purity of Reagents—All chemicals should, at a
a final volume of 1 L.
minimum, be of reagent grade and should conform to the
specifications of the Committee on Analytical Reagents of the 8.5.6 4 M Nitric Acid—Add 255 mL of concentrated HNO
American Chemical Society where such specifications are
(15.7 M, mass fraction of 70.0 %) to 600 mL of water, dilute to
available. High Purity reagents are suggested if mass spec- a final volume of 1 L.
trometry is chosen as the detection method. Other grades of
8.6 Reagents for the Quantification of Tc:
reagents may be used provided it is first determined that the
8.6.1 See the individual detection method descriptions to
reagent is of sufficient purity to permit its use without lessening
compile a list of the reagents needed for the chosen detection
the accuracy of the determination.
method.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
4 99m
DC. For suggestions on the testing of reagents not listed by the American Chemical Tc may be obtained from a local medical pharmacy supplier or other suitable
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, supplier.
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma- The boldface numbers in parentheses refer to the list of references at the end of
copeial Convention, Inc. (USPC), Rockville, MD. this standard.
C1387 − 23
9. Procedure 9.3.2 Soil Fusion—The following two methods have been
used for Tc.
9.1 Collect samples in accordance with Specification C998.
9.3.2.1 Weigh out four grams of sample. Add the desired
9.2 Soil or Sediment Preparation:
yield monitor and ash using step 9.2.2. When cool, transfer the
9.2.1 Oven dry samples at a temperature not to exceed
sample to a nickel crucible. Add 20 grams of the flux mixture
105 °C and homogenize in accordance with Specification
(Na CO , K CO and NaNO in a 3.92:5.08:1.00 weight ratio;
2 3 2 3 3
C999.
the flux-to-sample ratio should be 5:1). Start the fusion by
9.2.2 Optional—Samples may be placed in a muffle oven to
heating the crucible with the sample over a burner at high heat.
decompose organic matter prior to the extraction of Tc. The
When no further reaction is visible, cover the crucible and
muffling techniques reported vary significantly (3-5). If
place in a muffle over set at 900 °C for 30 minutes. Remove the
desired, weigh 5 g to 10 g of the sample and place in a high
sample from the oven and cool. Cover the crucible with a
temperature crucible. Add the chosen yield monitor and mix
watch glass and add about 25 mL of water to the crucible to
the sample. Wet the sample with concentrated ammonium
start dissolving the cake. Transfer the solution to a beaker and
hydroxide and mix, then dry under a heat lamp. It has been
continue rinsing the crucible with water until all the cake is
found that ammonium hydroxide will prevent the loss of the
rinsed into the beaker. Cover the beaker and warm slightly if
volatile Tc at higher temperatures. Place the sample in a muffle
needed to complete the dissolution. Dilute with water to a final
oven for 24 hours at 500 °C (5), or for 30 minutes to 60
volume of about 200 mL to 250 mL (11).
minutes at 600 °C followed by the addition of a few grams of
9.3.2.2 It is suggested that the sample be ground to pass
ammonium nitrate and 10 more minutes of heating if traces of
through a 45 micrometer standard test sieve as defined in
carbon remain (3).
Specification E11. This will result in a homogeneous sample
9.3 Tc Extraction—These discussions are summaries from
with a particle size that can be attacked by the fusion
available literature. The user must read the primary reference
procedure. Weigh out 0.25 gram of sample to a zirconium
for a complete discussion of the method prior to its use.
crucible. Add the desired yield monitor. Add 2.25 gram of
9.3.1 Acid Leaching—There are many reported acid leach-
sodium peroxide and mix well. Place the crucible in a muffle
ing techniques in the literature (3, 4, 6-10); however, only those
oven preheated to 470 °C. Heat for 30 minutes. Remove from
that are easily coupled to the extraction chromatography
the oven. When cool, add about 40 mL of water. Allow the
purificat
...

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.
Designation: C1387 − 14 C1387 − 23
Standard Guide for
the Determination of Technetium-99 in Soil
This standard is issued under the fixed designation C1387; 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
1.1 This guide is intended to serve as a reference for laboratories wishing to perform Tc analyses in soil. Several options are
given for selection of a tracer and for the method of extracting the Tc from the soil matrix. Separation of Tc from the sample matrix
is performed using an extraction chromatography resin. Options are then given for the determination of the Tc activity in the
original sample. It is up to the user to determine which options are appropriate for use, and to generate acceptance data to support
the chosen procedure.
1.2 Due to the various extraction methods available, various tracers used, variable detection methods used, and lack of certified
reference materials for Tc in soil, there is insufficient data to support a single method written as a standard method.
1.3 The values stated in SI units are to be regarded as standard. No other standard, except where the non-SI unit of molar, M,units
of measurement are included in this is used for the concentration of chemicals and reagents. The values given in parentheses after
SI units are provided for information only and are not considered standard.
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.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
C859 Terminology Relating to Nuclear Materials
C998 Practice for Sampling Surface Soil for Radionuclides
C999 Practice for Soil Sample Preparation for the Determination of Radionuclides
D1193 Specification for Reagent Water
D7168 Test Method for Tc in Water by Solid Phase Extraction Disk
This guide is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved Jan. 1, 2014Jan. 1, 2023. Published February 2014March 2023. Originally approved in 1998. Last previous edition approved in 20082014 as
C1387 – 08.C1387 – 14. DOI: 10.1520/C1387-14.10.1520/C1387-23.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1387 − 23
D8026 Practice for Determination of Tc-99 in Water by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 For definitions of terms in this guide, refer to Terminology C859.
4. Summary of Guide
4.1 There are no stable isotopes of technetium. Technetium-99 is produced by the fission of uranium and plutonium, and has been
released to the environment via nuclear weapons testing and nuclear materials processing. In an oxidizing environment, it exists
–
as the very mobile pertechnetate ion, TcO . Technetium-99 is a long-lived (half-life of 2.1 E 5 E+5 years), weak beta (maximum
beta energy of 293 keV) emitting radioisotope.
4.2 For the analysis of Tc in soil, a tracer is added to the sample matrix, or spiked duplicate samples are prepared, and then the
Tc is extracted from the soil matrix by one of several methods, including acid leaching or one of various fusion methods. The
resulting solution is passed through an extraction chromatography column. Technetium is known to be retained by the extraction
chromatography material while most other elements pass through the column. The column is washed with dilute acid to remove
any remaining interferents. The resin may then be counted directly by adding it to a liquid scintillation cocktail and counting by
liquid scintillation spectrometry, or the Tc may be eluted from the resin for alternative counting or mass spectrometric techniques.
5. Significance and Use
5.1 This guide offers several options for the determination of Tc in soil samples. Sample sizes of up to 200 g are possible,
depending on the method chosen to extract Tc from the soil matrix. It is up to the user to determine if it is appropriate for the
intended use of the final data.
6. Interferences
6.1 Any radionuclide not completely removed by the extraction chromatography column that has a beta decay energy similar to
99 99
or higher than Tc will interfere when counting techniques are used for quantification of the Tc activity.
6.2 Any elements with a mass-to-charge ratio (m/z) of 99 (that is, naturally occurring isotope of Ru or other artificially produced
elements of sufficient half-life with similar m/z) can interfere when using mass spectrometry for quantification of the Tc mass
activity. Any element with the same m/z as the isotope used as an isotope dilution tracer or internal standard will cause a bias in
the yield correction. Corrections should be included in the mass spectrometry data reduction for known interferences.
6.3 Additional interferences may be encountered, depending on the tracer and measurement technique chosen. It is up to the user
to determine and correct for any additional interferences.
7. Apparatus
7.1 Apparatus for the Extraction of Tc from Sample Matrix:
7.1.1 See the individual extraction method descriptions to compile a list of the equipment needed for the chosen extraction method.
7.2 Apparatus for the Purification of Tc from the Soil Extract:
7.2.1 Extraction column—with a bed volume of several milliliters for the extraction chromatography resin.
7.2.2 Column extension funnels—that can be added to the extraction column such that a few hundred milliliters of solution can
be added to the column at one time.
7.2.3 Column rack—holds columns such that several extractions can be performed simultaneously.
7.3 Apparatus for the Quantification of Tc:
C1387 − 23
7.3.1 See the individual detection method descriptions to compile a list of the equipment needed for the chosen detection method.
8. Reagents
8.1 Purity of Reagents—All chemicals should, at a minimum, be of reagent grade and should conform to the specifications of the
Committee on Analytical Reagents of the American Chemical Society where such specifications are available. High Purity
reagents are suggested if mass spectrometry is chosen as the detection method. Other grades of reagents may be used provided it
is first determined that the reagent is of sufficient 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, as defined by Type
I of Specification D1193.
8.3 Tracer:
8.3.1 Isotope Dilution Yield Determination:
95m 99m 4
8.3.1.1 Radiometric Yield Determination— Tc or Tc have been used to monitor the chemical yield of the extraction and
99 99m
purification of Tc prior to quantification. [Example: Add 10 nCi 370 Bq (10 nCi) of Tc as a yield tracer when determining
yield by gamma spectrometry.]
8.3.1.2 Mass Spectrometric Yield Determination— Tc may be produced in a nuclear reactor in very limited quantities to be used
99 5 97
as an isotope dilution tracer for the mass spectrometric determination of Tc (1). [Example: Add 1 ng of Tc as a yield tracer
for mass spectrometry.]
8.3.1.3 Rhenium as a Mass Spectrometric Yield Monitor—The chemical behavior of Re and Tc are similar enough on the extraction
resin that Re may be used as a tracer for Tc when using ICP-MS as a detection method (2). Practice D8026 provides additional
information on this option.
8.3.2 Duplicate Sample Analysis to Monitor Chemical Yield:
8.3.2.1 Duplicate samples may be analyzed, one spiked with a known amount of Tc and one unspiked. The chemical recovery
of the spiked sample is then used to correct the unspiked sample to obtain the original sample activity. (See Test Method D7168
for an example of this method.)
8.4 Reagents for the Extraction of Tc from Sample Matrix:
8.4.1 See the individual extraction method descriptions to compile a list of the reagents needed for the chosen extraction method.
8.5 Reagents for the Purification of Tc from the Sample Matrix:
8.5.1 Extraction Chromatrography Resin—TEVA Resin.
8.5.2 Prefilter Resin—a nonionic acrylic ester polymer resin used to remove residual organic matter prior to the extraction
chromatography resin column.
8.5.3 Hydrogen Peroxide—30 %.
8.5.4 Nitric Acid—(16 M HNO ) concentrated, specific gravity 1.42.
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, American Chemical Society, Washington, D. C. DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards
for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U. K., U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc.
(USPC), Rockville, MD.
99m
Tc may be obtained from a local medical pharmacy supplier or other suitable supplier.
The boldface numbers in parentheses refer to the list of references at the end of this standard.
C1387 − 23
8.5.5 1M1 M Nitric Acid—Add 6364 mL of concentrated HNO (15.7 M, mass fraction of 70.0 %) to 900 mL of DI water, dilute
to a final volume of 1 liter.1 L.
8.5.6 4M4 M Nitric Acid—Add 250255 mL of concentrated HNO (15.7 M, mass fraction of 70.0 %) to 600 mL of DI water, dilute
to a final volume of 1 liter.L.
8.6 Reagents for the Quantification of Tc:
8.6.1 See the individual detection method descriptions to compile a list of the reagents needed for the chosen detection method.
9. Procedure
9.1 Collect samples in accordance with Specification C998.
9.2 Soil or Sediment Preparation:
9.2.1 Oven dry samples at a temperature not to exceed 105°C105 °C and homogenize in accordance with Specification C999.
9.2.2 Optional—Samples may be placed in a muffle oven to decompose organic matter prior to the extraction of Tc. The muffling
techniques reported vary significantly (3-5). If desired, weigh 5–10 5 g to 10 g of the sample and place in a high temperature
crucible. Add the chosen yield monitor and mix the sample. Wet the sample with concentrated ammonium hydroxide and mix, then
dry under a heat lamp. It has been found that ammonium hydroxide will prevent the loss of the volatile Tc at higher temperatures.
Place the sample in a muffle oven for 24 hours at 500°C500 °C (5), or for 30–60 minutes at 600°C30 minutes to 60 minutes at
600 °C followed by the addition of a few grams of ammonium nitrate and 10 more minutes of heating if traces of carbon remain
(3).
9.3 Tc Extraction—These discussions are summaries from available literature. The user must read the primary reference for a
complete discussion of the method prior to its use.
9.3.1 Acid Leaching—There are many reported acid leaching techniques in the literature (3, 4, 6-10); however, only those that are
easily coupled to the extraction chromatography purification are described in 9.3.1.1 – 9.3.1.4. These methods are summarized in
the following four sectionssections:
9.3.1.1 Weigh out up to 10 grams of soil to a 250 mL glass beaker along with the desired yield monitor. Cover and heat the sample
in the presence of 1M1 M nitric acid. After cooling, remove residual solid matter from the sample by centrifugation. Add hydrogen
peroxide and sodium vanadate to each sample to destroy residual organic matter. Finally, reduce the acidity of the sample to less
than 0.5M0.5 M using ammonium hydroxide (dilute with water to a final sample volume of approximately 500 mL) (6).
9.3.1.2 Add the desired yield monitor to 5–10 5 g to 10 g of sample, which is then ashed using step 9.2.2. Leach the sample twice
with hot 8M8 M nitric acid and hydrogen peroxide, combining the leachates. Adjust the pH to 7 with sodium hydroxide and filter
the solution through a glass fiber filter. Dilute the filtrate to approximately 500 mL (7).
9.3.1.3 Weigh out up to 200 grams of sample. Add the desired yield monitor. Ash using step 9.2.2. Transfer the sample to a
decomposition vessel. Add 6M6 M nitric acid. Decompose the sample at 100–120°C 100 °C to 120 °C for one hour. Filter the
sample through a glass fiber filter then dilute with water until the acid concentration is less than 0.5M0.5 M nitric acid (at least
500 mL) (8).
9.3.1.4 Weigh out one gram of the dried, unashed sample to a 250 mL conical flask. Add the desired yield monitor. Add
concentrated nitric acid and fit into a reflux condenser. Reflux the sample until the brown fumes cease and all the organic matter
is dissolved. Cool the flask and pour the solution into water. Neutralize the solution with sodium hydroxide, filter out any
undissolved residue, and dilute with water until the acid concentration is less than 0.5M0.5 M nitric acid and to a final volume of
250–500 250 mL to 500 mL (9).
9.3.2 Soil Fusion—The following two methods have been used for Tc-99.Tc.
9.3.2.1 Weigh out four grams of sample. Add the desired yield monitor and ash using step 9.2.2. When cool, transfer the sample
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