ASTM C1109-10(2015)
(Practice)Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectroscopy
Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectroscopy
SIGNIFICANCE AND USE
5.1 This practice may be used to determine concentrations of elements leached from nuclear waste materials (glasses, ceramics, cements) using an aqueous leachant. If the nuclear waste material is radioactive, a suitably contained and shielded ICP-AES spectrometer system with a filtered exit-gas system must be used, but no other changes in the practice are required. The leachant may be deionized water or any aqueous solution containing less than 1 % total solids.
5.2 This practice as written is for the analysis of solutions containing 1 % (v/v) nitric acid. It can be modified to specify the use of the same or another mineral acid at the same or higher concentration. In such cases, the only change needed in this practice is to substitute the preferred acid and concentration value whenever 1 % nitric acid appears here. It is important that the acid type and content of the reference and check solutions closely match the leachate solutions to be analyzed.
5.3 This practice can be used to analyze leachates from static leach testing of waste forms using Test Method C1220.
SCOPE
1.1 This practice is applicable to the determination of low concentration and trace elements in aqueous leachate solutions produced by the leaching of nuclear waste materials, using inductively coupled plasma-atomic emission spectroscopy (ICP-AES).
1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioactive waste material.
1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1 % total dissolved solids.
1.4 This practice should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction.
1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.
1.6 This practice contains notes that are explanatory and are not part of the mandatory requirements of the method.
1.7 The values stated in SI units are to be regarded as the standard.
1.8 This standard does not purport to address all of the safety problems, 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.
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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: C1109 − 10 (Reapproved 2015)
Standard Practice for
Analysis of Aqueous Leachates from Nuclear Waste
Materials Using Inductively Coupled Plasma-Atomic
Emission Spectroscopy
This standard is issued under the fixed designation C1109; 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This practice is applicable to the determination of low
C859 Terminology Relating to Nuclear Materials
concentration and trace elements in aqueous leachate solutions
C1009 Guide for Establishing and Maintaining a Quality
produced by the leaching of nuclear waste materials, using
AssuranceProgramforAnalyticalLaboratoriesWithinthe
inductively coupled plasma-atomic emission spectroscopy
Nuclear Industry
(ICP-AES).
C1220 Test Method for Static Leaching of MonolithicWaste
1.2 The nuclear waste material may be a simulated (non-
Forms for Disposal of Radioactive Waste
radioactive) solid waste form or an actual solid radioactive
D1193 Specification for Reagent Water
waste material.
D7035 Test Method for Determination of Metals and Met-
1.3 The leachate may be deionized water or any natural or
alloids in Airborne Particulate Matter by Inductively
simulated leachate solution containing less than 1 % total
Coupled Plasma Atomic Emission Spectrometry (ICP-
dissolved solids.
AES)
E135 Terminology Relating to Analytical Chemistry for
1.4 This practice should be used by analysts experienced in
Metals, Ores, and Related Materials
the use of ICP-AES, the interpretation of spectral and non-
E177 Practice for Use of the Terms Precision and Bias in
spectral interferences, and procedures for their correction.
ASTM Test Methods
1.5 No detailed operating instructions are provided because 3
2.2 ISO and European Standards:
of differences among various makes and models of suitable
ISO 1042 Laboratory Glassware—One-mark Volumetric
ICP-AES instruments. Instead, the analyst shall follow the
Flasks
instructions provided by the manufacturer of the particular
ISO 3585 Borosilicate Glass 3.3—Properties
instrument. This test method does not address comparative
ISO 8655 Piston-Operated Volumetric Instruments (6 parts)
accuracy of different devices or the precision between instru-
ments of the same make and model.
3. Terminology
1.6 This practice contains notes that are explanatory and are
3.1 For definitions of pertinent terms not listed here, see
not part of the mandatory requirements of the method.
Terminology C859.
1.7 The values stated in SI units are to be regarded as the 3.2 Definitions:
standard.
3.2.1 atomic emission—characteristic radiation emitted by
an electronically excited atomic species. D7035
1.8 This standard does not purport to address all of the
3.2.1.1 Discussion—In atomic (or optical) emission
safety problems, if any, associated with its use. It is the
spectrometry, a very high-temperature environment, such as a
responsibility of the user of this standard to establish appro-
plasma, is used to create excited state atoms. For analytical
priate safety and health practices and determine the applica-
purposes,characteristicemissionsignalsfromelementsintheir
bility of regulatory limitations prior to use.
excited states are then measured at specific wavelengths.
1 2
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2015. Published June 2015. Originally the ASTM website.
approved in 1988. Last previous edition approved in 2010 as C1109 – 10. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/C1109-10R15. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1109 − 10 (2015)
3.2.2 background correction—process of correcting the in- 3.2.14 linearity check solution(s)—solution(s) containing
tensity at an analytical wavelength for the intensity due to the the elements to be determined at concentrations that cover a
underlying spectral background of a blank. D7035 range that is two to ten times higher and lower than the
3.2.2.1 Discussion—During sample analysis, measurements concentration of these elements in the calibration reference
aremadeofthebackgroundintensitynearthepeakwavelength solutions. These solutions also contain 1 % (v/v) nitric acid.
of the analytical lines. Correction of the analytical line peak
3.2.15 non-spectral interference—changes in the apparent
intensity to yield the net line intensity can be made by
net signal intensity from the analyte due to physical or
subtraction of either (a) a single intensity measurement per-
chemicalprocessesthataffectthetransportoftheanalytetothe
formed on the high or low wavelength side of the analytical
plasma and its vaporization, atomization, or excitation in the
line (single-point background correction), or (b) an interpo-
plasma.
lated background intensity from background measurements
3.2.16 sensitivity—the slope of the linear dynamic range.
acquired on both the high and low wavelength sides of the
analytical line (double-point background correction).
3.2.17 spectral interference—an interference caused by the
emission from a species other than the analyte of interest.
3.2.3 bias—between the expectation of the test results and
D7035
an accepted reference value. E177
3.2.17.1 Discussion—Sources of spectral interference in-
3.2.4 calibration—the process by which the relationship
clude spectral line overlaps, broadened wings of intense
between net signal intensity and elemental concentration is
spectral lines, ion-atom recombination continuum emission,
determined for a specific element analysis.
molecular band emission, and stray (scattered) light effects.
3.2.5 calibration blank solution—calibration solution pre-
pared without the addition of any reference solutions. D7035
4. Summary of Practice
3.2.6 calibration curve—plot of net signal intensity versus
4.1 Aqueous leachates are prepared, using Test Method
elemental concentration using data obtained during calibration.
C1220, for analysis using this practice.
3.2.7 calibration reference solution(s)—solutions contain-
4.2 The general principles of emission spectrometric analy-
ingknownconcentrationsofoneormoreelementsin1 %(v/v)
sis are given in Ref (3). In this practice, elemental constituents
nitric acid for instrument calibration.
ofaqueousleachatesolutionsaredeterminedsimultaneouslyor
3.2.8 critical limit (L )—minimum significant value of an
C
sequentially by inductively coupled plasma-atomic emission
estimated net signal or concentration, applied as a discrimina-
spectroscopy (ICP-AES).
tor against background noise. (1)
4.3 Samples are prepared by filtration if needed to remove
3.2.9 inductively coupled plasma (ICP)—a high-
particulates and acidification to match calibration reference
temperature discharge generated by a flowing conductive gas,
solutions. Filtration should be the last resort to clarify a
normallyargon,throughamagneticfieldinducedbyaloadcoil
solution since leach studies are designed to determine the
that surrounds the tubes carrying the gas. D7035
absolute amount of material removed from a waste form by
3.2.10 instrument check solution(s)—solution(s) containing
aqueous leaching.
all the elements to be determined at concentration levels
4.4 Additional general guidelines are provided in Guide
approximating the concentrations in the samples. These solu-
C1009, Specification D1193, Terminology C859, and Termi-
tions must also contain 1 % (v/v) nitric acid.
nology E135.
3.2.11 interelement correction—a spectral interference cor-
rection technique in which emission contributions from inter-
5. Significance and Use
fering elements that emit radiation at the analyte wavelength
are subtracted from the apparent analyte emission after mea- 5.1 This practice may be used to determine concentrations
suring the interfering element concentrations at other
of elements leached from nuclear waste materials (glasses,
wavelengths. D7035 ceramics, cements) using an aqueous leachant. If the nuclear
waste material is radioactive, a suitably contained and shielded
3.2.12 limit of detection (L )—value for which the false
D
ICP-AES spectrometer system with a filtered exit-gas system
negative error is B using a given critical limit. (1)
must be used, but no other changes in the practice are required.
3.2.12.1 Discussion—If the analytical standard deviation is
The leachant may be deionized water or any aqueous solution
constant with respect to concentration, this can be computed as
containing less than 1 % total solids.
3.7 times the standard deviation of the analytical results from
ten matrix blank samples spiked at approximately the antici-
5.2 This practice as written is for the analysis of solutions
pated detection limit; otherwise, see references (1, 2) for
containing 1 % (v/v) nitric acid. It can be modified to specify
additional guidance.
the use of the same or another mineral acid at the same or
3.2.13 linear dynamic range—the elemental concentration higher concentration. In such cases, the only change needed in
range over which the calibration curve remains linear to within this practice is to substitute the preferred acid and concentra-
the precision of the analytical method. tion value whenever 1 % nitric acid appears here. It is
important that the acid type and content of the reference and
check solutions closely match the leachate solutions to be
The boldface numbers in parentheses refer to the list of references at the end
of this standard. analyzed.
C1109 − 10 (2015)
5.3 This practice can be used to analyze leachates from contaminants. The acid may be prepared by sub-boiling distil-
static leach testing of waste forms using Test Method C1220. lation (4), or purchased from commercial sources.
7.5 Stock Solutions—May be purchased or prepared from
6. Apparatus
metals or metal salts of known purity. Stock solutions should
contain known concentrations of the element of interest rang-
6.1 Ordinary laboratory apparatus are not listed, but are
assumed to be present. ing from 100 to 10 000 mg/L.
7.6 Calibration Blank Solution, 1 % (v/v) HNO .
6.2 Glassware, volumetric flasks complying with the re-
quirements of ISO 1042, made of borosilicate glass complying
7.7 Calibration Reference Solutions, Instrument Check
with the requirements of ISO 3585. Glassware should be
Solutions, and Linearity Check Solutions:
cleaned before use by soaking in nitric acid and then rinsing
7.7.1 Prepare single-element or multielement calibration
thoroughly with water.
reference solutions by combining appropriate volumes of the
6.3 Filters, inert membrane, having pore size of 0.45 µm or stock solutions in acid-rinsed volumetric flasks. To establish
smaller. the calibration slope accurately, provide at least one solution
with element concentration that is a minimum of 100 times the
6.4 Piston-operated Volumetric Pipettors and Dispensers,
L foreachelement.Addsufficientnitricacidtobringthefinal
D
complying with the requirements of ISO 8655, for pipetting
solution to 1 % HNO . Prior to preparing the multielement
and dispensing of solutions, acids, and so forth.
solutions, analyze each stock solution separately to check for
6.5 Bottles, tetrafluoroethylene or polyethylene, for storage
strong spectral interference and the presence of impurities (5).
of calibration and check solutions.
Take care when preparing the multielement solutions to verify
that the components are compatible and stable (they do not
6.6 Disposable Gloves, impermeable, for protection from
interact to cause precipitation) and that none of the elements
corrosive substances. Polyvinyl chloride (PVC) gloves are
present exhibit mutual spectral interference. Transfer the cali-
suitable.
bration reference solutions to acid-leached FEP TFE-
6.7 Inductively Coupled Plasma-Atomic Emission
fluorocarbon or polyethylene bottles for storage. Calibration
Spectrometer, computer controlled, with a spectral bandpass of
reference solutions must be verified initially using a quality
0.05 nm or less, is required to provide the necessary spectral
control sample and monitored periodically for stability.
resolution.
NOTE 3—Solutions in polyethylene bottles are subject to transpiration
NOTE1—Thespectrometermaybeofthesimultaneousmultielementor
losses that may affect the assigned concentration values.
sequential scanning type. The spectrometer may be of the air-path, inert
gas-path,orvacuumtype,withspectrallinesselectedappropriatelyforuse
7.7.2 Prepare the instrument check solution(s) and linearity
with the specific instrument.
check solutions in a similar manner.
NOTE 2—An autosampler having a flowing rinse is recommended.
7.7.3 Fresh solutions should be prepared as needed with the
realization that concentrations can change over time. The
7. Reagents and Materials
recommended maximum shelf life for calibration reference
7.1 Purity of Reagents—Reagent grade chemicals shall be
solutions, instrument check solutions, and linearity check
used in all tests. Unless otherwise indicated, it is intended that solutions is one month.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
8. Sample Preparation
such specifications are available. Other grades may be used,
8.1 If necessary to remove solids or suspended colloids,
provided it is first ascertained that the reagent is of sufficiently
filter the leachate through a clean filter, using an inert filter
high purity to permit its use without lessening the accuracy of
support (avoid the use of fritted glass supports). Examine the
the determination.
filtered leachate to verify the absence of visible solids or
7.2 Purity of Water—Unless otherwise indicated, references
suspended colloids. The deposit on the filter may be analyzed
to water shall be understood to mean reagent water as defined
separately if required.
by Type I of Specification D1193 or water exceeding these
8.2 Prepare filtered and unfiltere
...
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: C1109 − 10 (Reapproved 2015)
Standard Practice for
Analysis of Aqueous Leachates from Nuclear Waste
Materials Using Inductively Coupled Plasma-Atomic
Emission Spectroscopy
This standard is issued under the fixed designation C1109; 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This practice is applicable to the determination of low
C859 Terminology Relating to Nuclear Materials
concentration and trace elements in aqueous leachate solutions
C1009 Guide for Establishing and Maintaining a Quality
produced by the leaching of nuclear waste materials, using
Assurance Program for Analytical Laboratories Within the
inductively coupled plasma-atomic emission spectroscopy
Nuclear Industry
(ICP-AES).
C1220 Test Method for Static Leaching of Monolithic Waste
1.2 The nuclear waste material may be a simulated (non-
Forms for Disposal of Radioactive Waste
radioactive) solid waste form or an actual solid radioactive
D1193 Specification for Reagent Water
waste material.
D7035 Test Method for Determination of Metals and Met-
1.3 The leachate may be deionized water or any natural or
alloids in Airborne Particulate Matter by Inductively
simulated leachate solution containing less than 1 % total
Coupled Plasma Atomic Emission Spectrometry (ICP-
dissolved solids.
AES)
E135 Terminology Relating to Analytical Chemistry for
1.4 This practice should be used by analysts experienced in
Metals, Ores, and Related Materials
the use of ICP-AES, the interpretation of spectral and non-
E177 Practice for Use of the Terms Precision and Bias in
spectral interferences, and procedures for their correction.
ASTM Test Methods
1.5 No detailed operating instructions are provided because 3
2.2 ISO and European Standards:
of differences among various makes and models of suitable
ISO 1042 Laboratory Glassware—One-mark Volumetric
ICP-AES instruments. Instead, the analyst shall follow the
Flasks
instructions provided by the manufacturer of the particular
ISO 3585 Borosilicate Glass 3.3—Properties
instrument. This test method does not address comparative
ISO 8655 Piston-Operated Volumetric Instruments (6 parts)
accuracy of different devices or the precision between instru-
ments of the same make and model.
3. Terminology
1.6 This practice contains notes that are explanatory and are
3.1 For definitions of pertinent terms not listed here, see
not part of the mandatory requirements of the method.
Terminology C859.
1.7 The values stated in SI units are to be regarded as the
3.2 Definitions:
standard. 3.2.1 atomic emission—characteristic radiation emitted by
an electronically excited atomic species. D7035
1.8 This standard does not purport to address all of the
3.2.1.1 Discussion—In atomic (or optical) emission
safety problems, if any, associated with its use. It is the
spectrometry, a very high-temperature environment, such as a
responsibility of the user of this standard to establish appro-
plasma, is used to create excited state atoms. For analytical
priate safety and health practices and determine the applica-
purposes, characteristic emission signals from elements in their
bility of regulatory limitations prior to use.
excited states are then measured at specific wavelengths.
1 2
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2015. Published June 2015. Originally the ASTM website.
approved in 1988. Last previous edition approved in 2010 as C1109 – 10. DOI: Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/C1109-10R15. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1109 − 10 (2015)
3.2.2 background correction—process of correcting the in- 3.2.14 linearity check solution(s)—solution(s) containing
tensity at an analytical wavelength for the intensity due to the the elements to be determined at concentrations that cover a
underlying spectral background of a blank. D7035 range that is two to ten times higher and lower than the
3.2.2.1 Discussion—During sample analysis, measurements concentration of these elements in the calibration reference
are made of the background intensity near the peak wavelength solutions. These solutions also contain 1 % (v/v) nitric acid.
of the analytical lines. Correction of the analytical line peak
3.2.15 non-spectral interference—changes in the apparent
intensity to yield the net line intensity can be made by
net signal intensity from the analyte due to physical or
subtraction of either (a) a single intensity measurement per-
chemical processes that affect the transport of the analyte to the
formed on the high or low wavelength side of the analytical
plasma and its vaporization, atomization, or excitation in the
line (single-point background correction), or (b) an interpo-
plasma.
lated background intensity from background measurements
3.2.16 sensitivity—the slope of the linear dynamic range.
acquired on both the high and low wavelength sides of the
analytical line (double-point background correction). 3.2.17 spectral interference—an interference caused by the
emission from a species other than the analyte of interest.
3.2.3 bias—between the expectation of the test results and
D7035
an accepted reference value. E177
3.2.17.1 Discussion—Sources of spectral interference in-
3.2.4 calibration—the process by which the relationship
clude spectral line overlaps, broadened wings of intense
between net signal intensity and elemental concentration is
spectral lines, ion-atom recombination continuum emission,
determined for a specific element analysis.
molecular band emission, and stray (scattered) light effects.
3.2.5 calibration blank solution—calibration solution pre-
pared without the addition of any reference solutions. D7035
4. Summary of Practice
3.2.6 calibration curve—plot of net signal intensity versus
4.1 Aqueous leachates are prepared, using Test Method
elemental concentration using data obtained during calibration.
C1220, for analysis using this practice.
3.2.7 calibration reference solution(s)—solutions contain-
4.2 The general principles of emission spectrometric analy-
ing known concentrations of one or more elements in 1 % (v/v)
sis are given in Ref (3). In this practice, elemental constituents
nitric acid for instrument calibration.
of aqueous leachate solutions are determined simultaneously or
3.2.8 critical limit (L )—minimum significant value of an
C
sequentially by inductively coupled plasma-atomic emission
estimated net signal or concentration, applied as a discrimina-
spectroscopy (ICP-AES).
tor against background noise. (1)
4.3 Samples are prepared by filtration if needed to remove
3.2.9 inductively coupled plasma (ICP)—a high-
particulates and acidification to match calibration reference
temperature discharge generated by a flowing conductive gas,
solutions. Filtration should be the last resort to clarify a
normally argon, through a magnetic field induced by a load coil
solution since leach studies are designed to determine the
that surrounds the tubes carrying the gas. D7035
absolute amount of material removed from a waste form by
3.2.10 instrument check solution(s)—solution(s) containing
aqueous leaching.
all the elements to be determined at concentration levels
4.4 Additional general guidelines are provided in Guide
approximating the concentrations in the samples. These solu-
C1009, Specification D1193, Terminology C859, and Termi-
tions must also contain 1 % (v/v) nitric acid.
nology E135.
3.2.11 interelement correction—a spectral interference cor-
rection technique in which emission contributions from inter-
5. Significance and Use
fering elements that emit radiation at the analyte wavelength
are subtracted from the apparent analyte emission after mea-
5.1 This practice may be used to determine concentrations
suring the interfering element concentrations at other of elements leached from nuclear waste materials (glasses,
wavelengths. D7035
ceramics, cements) using an aqueous leachant. If the nuclear
waste material is radioactive, a suitably contained and shielded
3.2.12 limit of detection (L )—value for which the false
D
ICP-AES spectrometer system with a filtered exit-gas system
negative error is B using a given critical limit. (1)
must be used, but no other changes in the practice are required.
3.2.12.1 Discussion—If the analytical standard deviation is
The leachant may be deionized water or any aqueous solution
constant with respect to concentration, this can be computed as
containing less than 1 % total solids.
3.7 times the standard deviation of the analytical results from
ten matrix blank samples spiked at approximately the antici-
5.2 This practice as written is for the analysis of solutions
pated detection limit; otherwise, see references (1, 2) for
containing 1 % (v/v) nitric acid. It can be modified to specify
additional guidance.
the use of the same or another mineral acid at the same or
3.2.13 linear dynamic range—the elemental concentration higher concentration. In such cases, the only change needed in
range over which the calibration curve remains linear to within this practice is to substitute the preferred acid and concentra-
the precision of the analytical method. tion value whenever 1 % nitric acid appears here. It is
important that the acid type and content of the reference and
4 check solutions closely match the leachate solutions to be
The boldface numbers in parentheses refer to the list of references at the end
of this standard. analyzed.
C1109 − 10 (2015)
5.3 This practice can be used to analyze leachates from contaminants. The acid may be prepared by sub-boiling distil-
static leach testing of waste forms using Test Method C1220. lation (4), or purchased from commercial sources.
7.5 Stock Solutions—May be purchased or prepared from
6. Apparatus
metals or metal salts of known purity. Stock solutions should
6.1 Ordinary laboratory apparatus are not listed, but are contain known concentrations of the element of interest rang-
ing from 100 to 10 000 mg/L.
assumed to be present.
6.2 Glassware, volumetric flasks complying with the re- 7.6 Calibration Blank Solution, 1 % (v/v) HNO .
quirements of ISO 1042, made of borosilicate glass complying
7.7 Calibration Reference Solutions, Instrument Check
with the requirements of ISO 3585. Glassware should be
Solutions, and Linearity Check Solutions:
cleaned before use by soaking in nitric acid and then rinsing
7.7.1 Prepare single-element or multielement calibration
thoroughly with water.
reference solutions by combining appropriate volumes of the
6.3 Filters, inert membrane, having pore size of 0.45 µm or stock solutions in acid-rinsed volumetric flasks. To establish
the calibration slope accurately, provide at least one solution
smaller.
with element concentration that is a minimum of 100 times the
6.4 Piston-operated Volumetric Pipettors and Dispensers,
L for each element. Add sufficient nitric acid to bring the final
D
complying with the requirements of ISO 8655, for pipetting
solution to 1 % HNO . Prior to preparing the multielement
and dispensing of solutions, acids, and so forth.
solutions, analyze each stock solution separately to check for
6.5 Bottles, tetrafluoroethylene or polyethylene, for storage
strong spectral interference and the presence of impurities (5).
of calibration and check solutions.
Take care when preparing the multielement solutions to verify
that the components are compatible and stable (they do not
6.6 Disposable Gloves, impermeable, for protection from
interact to cause precipitation) and that none of the elements
corrosive substances. Polyvinyl chloride (PVC) gloves are
present exhibit mutual spectral interference. Transfer the cali-
suitable.
bration reference solutions to acid-leached FEP TFE-
6.7 Inductively Coupled Plasma-Atomic Emission
fluorocarbon or polyethylene bottles for storage. Calibration
Spectrometer, computer controlled, with a spectral bandpass of
reference solutions must be verified initially using a quality
0.05 nm or less, is required to provide the necessary spectral
control sample and monitored periodically for stability.
resolution.
NOTE 3—Solutions in polyethylene bottles are subject to transpiration
NOTE 1—The spectrometer may be of the simultaneous multielement or
losses that may affect the assigned concentration values.
sequential scanning type. The spectrometer may be of the air-path, inert
gas-path, or vacuum type, with spectral lines selected appropriately for use 7.7.2 Prepare the instrument check solution(s) and linearity
with the specific instrument.
check solutions in a similar manner.
NOTE 2—An autosampler having a flowing rinse is recommended.
7.7.3 Fresh solutions should be prepared as needed with the
realization that concentrations can change over time. The
7. Reagents and Materials
recommended maximum shelf life for calibration reference
7.1 Purity of Reagents—Reagent grade chemicals shall be solutions, instrument check solutions, and linearity check
used in all tests. Unless otherwise indicated, it is intended that
solutions is one month.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
8. Sample Preparation
such specifications are available. Other grades may be used,
8.1 If necessary to remove solids or suspended colloids,
provided it is first ascertained that the reagent is of sufficiently
filter the leachate through a clean filter, using an inert filter
high purity to permit its use without lessening the accuracy of
support (avoid the use of fritted glass supports). Examine the
the determination.
filtered leachate to verify the absence of visible solids or
7.2 Purity of Water—Unless otherwise indicated, references
suspended colloids. The deposit on the filter may be analyzed
to water shall be understood to mean reagent water as defined
separately if required.
by Type I of Specification D1193 or water exceeding these
8.2 Prepare filtered and unfiltered aliquots of a calibration
spec
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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: C1109 − 10 C1109 − 10 (Reapproved 2015)
Standard Practice for
Analysis of Aqueous Leachates from Nuclear Waste
Materials Using Inductively Coupled Plasma-Atomic
Emission Spectroscopy
This standard is issued under the fixed designation C1109; 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 practice is applicable to the determination of low concentration and trace elements in aqueous leachate solutions
produced by the leaching of nuclear waste materials, using inductively coupled plasma-atomic emission spectroscopy (ICP-AES).
1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioactive waste
material.
1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1 % total dissolved
solids.
1.4 This practice should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral
interferences, and procedures for their correction.
1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable
ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument.
This test method does not address comparative accuracy of different devices or the precision between instruments of the same make
and model.
1.6 This practice contains notes that are explanatory and are not part of the mandatory requirements of the method.
1.7 The values stated in SI units are to be regarded as the standard.
1.8 This standard does not purport to address all of the safety problems, 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.
2. Referenced Documents
2.1 ASTM Standards:
C859 Terminology Relating to Nuclear Materials
C1009 Guide for Establishing and Maintaining a Quality Assurance Program for Analytical Laboratories Within the Nuclear
Industry
C1220 Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive Waste
D1193 Specification for Reagent Water
D7035 Test Method for Determination of Metals and Metalloids in Airborne Particulate Matter by Inductively Coupled Plasma
Atomic Emission Spectrometry (ICP-AES)
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
2.2 ISO and European Standards:
ISO 1042 Laboratory Glassware—One-mark Volumetric Flasks
ISO 3585 Borosilicate Glass 3.3—Properties
This practice 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 Oct. 1, 2010June 1, 2015. Published December 2010June 2015. Originally approved in 1988. Last previous edition approved in 20042010 as
C1109 – 04.C1109 – 10. DOI: 10.1520/C1109-10.10.1520/C1109-10R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1109 − 10 (2015)
ISO 8655 Piston-Operated Volumetric Instruments (6 parts)
3. Terminology
3.1 For definitions of pertinent terms not listed here, see Terminology C859.
3.2 Definitions:
3.2.1 atomic emission—characteristic radiation emitted by an electronically excited atomic species. D7035
3.2.1.1 Discussion—
In atomic (or optical) emission spectrometry, a very high-temperature environment, such as a plasma, is used to create excited state
atoms. For analytical purposes, characteristic emission signals from elements in their excited states are then measured at specific
wavelengths.
3.2.2 background correction—process of correcting the intensity at an analytical wavelength for the intensity due to the
underlying spectral background of a blank. D7035
3.2.2.1 Discussion—
During sample analysis, measurements are made of the background intensity near the peak wavelength of the analytical lines.
Correction of the analytical line peak intensity to yield the net line intensity can be made by subtraction of either (a) a single
intensity measurement performed on the high or low wavelength side of the analytical line (single-point background correction),
or (b) an interpolated background intensity from background measurements acquired on both the high and low wavelength sides
of the analytical line (double-point background correction).
3.2.3 bias—between the expectation of the test results and an accepted reference value. E177
3.2.4 calibration—the process by which the relationship between net signal intensity and elemental concentration is determined
for a specific element analysis.
3.2.5 calibration blank solution—calibration solution prepared without the addition of any reference solutions. D7035
3.2.6 calibration curve—plot of net signal intensity versus elemental concentration using data obtained during calibration.
3.2.7 calibration reference solution(s)—solutions containing known concentrations of one or more elements in 1 % (v/v) nitric
acid for instrument calibration.
3.2.8 critical limit (L )—minimum significant value of an estimated net signal or concentration, applied as a discriminator
C
against background noise. (1)
3.2.9 inductively coupled plasma (ICP)—a high-temperature discharge generated by a flowing conductive gas, normally argon,
through a magnetic field induced by a load coil that surrounds the tubes carrying the gas. D7035
3.2.10 instrument check solution(s)—solution(s) containing all the elements to be determined at concentration levels
approximating the concentrations in the samples. These solutions must also contain 1 % (v/v) nitric acid.
3.2.11 interelement correction—a spectral interference correction technique in which emission contributions from interfering
elements that emit radiation at the analyte wavelength are subtracted from the apparent analyte emission after measuring the
interfering element concentrations at other wavelengths. D7035
3.2.12 limit of detection (L )—value for which the false negative error is B using a given critical limit. (1)
D
3.2.12.1 Discussion—
If the analytical standard deviation is constant with respect to concentration, this can be computed as 3.7 times the standard
deviation of the analytical results from ten matrix blank samples spiked at approximately the anticipated detection limit; otherwise,
see references (1, 2) for additional guidance.
3.2.13 linear dynamic range—the elemental concentration range over which the calibration curve remains linear to within the
precision of the analytical method.
3.2.14 linearity check solution(s)—solution(s) containing the elements to be determined at concentrations that cover a range that
is two to ten times higher and lower than the concentration of these elements in the calibration reference solutions. These solutions
also contain 1 % (v/v) nitric acid.
3.2.15 non-spectral interference—changes in the apparent net signal intensity from the analyte due to physical or chemical
processes that affect the transport of the analyte to the plasma and its vaporization, atomization, or excitation in the plasma.
The boldface numbers in parentheses refer to the list of references at the end of this standard.
C1109 − 10 (2015)
3.2.16 sensitivity—the slope of the linear dynamic range.
3.2.17 spectral interference—an interference caused by the emission from a species other than the analyte of interest. D7035
3.2.17.1 Discussion—
Sources of spectral interference include spectral line overlaps, broadened wings of intense spectral lines, ion-atom recombination
continuum emission, molecular band emission, and stray (scattered) light effects.
4. Summary of Practice
4.1 Aqueous leachates are prepared, using Test Method C1220, for analysis using this practice.
4.2 The general principles of emission spectrometric analysis are given in Ref (3). In this practice, elemental constituents of
aqueous leachate solutions are determined simultaneously or sequentially by inductively coupled plasma-atomic emission
spectroscopy (ICP-AES).
4.3 Samples are prepared by filtration if needed to remove particulates and acidification to match calibration reference solutions.
Filtration should be the last resort to clarify a solution since leach studies are designed to determine the absolute amount of material
removed from a waste form by aqueous leaching.
4.4 Additional general guidelines are provided in Guide C1009, Specification D1193, Terminology C859, and Terminology
E135.
5. Significance and Use
5.1 This practice may be used to determine concentrations of elements leached from nuclear waste materials (glasses, ceramics,
cements) using an aqueous leachant. If the nuclear waste material is radioactive, a suitably contained and shielded ICP-AES
spectrometer system with a filtered exit-gas system must be used, but no other changes in the practice are required. The leachant
may be deionized water or any aqueous solution containing less than 1 % total solids.
5.2 This practice as written is for the analysis of solutions containing 1 % (v/v) nitric acid. It can be modified to specify the use
of the same or another mineral acid at the same or higher concentration. In such cases, the only change needed in this practice is
to substitute the preferred acid and concentration value whenever 1 % nitric acid appears here. It is important that the acid type
and content of the reference and check solutions closely match the leachate solutions to be analyzed.
5.3 This practice can be used to analyze leachates from static leach testing of waste forms using Test Method C1220.
6. Apparatus
6.1 Ordinary laboratory apparatus are not listed, but are assumed to be present.
6.2 Glassware, volumetric flasks complying with the requirements of ISO 1042, made of borosilicate glass complying with the
requirements of ISO 3585. Glassware should be cleaned before use by soaking in nitric acid and then rinsing thoroughly with
water.
6.3 Filters, inert membrane, having pore size of 0.45 μm or smaller.
6.4 Piston-operated Volumetric Pipettors and Dispensers, complying with the requirements of ISO 8655, for pipetting and
dispensing of solutions, acids, and so forth.
6.5 Bottles, tetrafluoroethylene or polyethylene, for storage of calibration and check solutions.
6.6 Disposable Gloves, impermeable, for protection from corrosive substances. Polyvinyl chloride (PVC) gloves are suitable.
6.7 Inductively Coupled Plasma-Atomic Emission Spectrometer, computer controlled, with a spectral bandpass of 0.05 nm or
less, is required to provide the necessary spectral resolution.
NOTE 1—The spectrometer may be of the simultaneous multielement or sequential scanning type. The spectrometer may be of the air-path, inert
gas-path, or vacuum type, with spectral lines selected appropriately for use with the specific instrument.
NOTE 2—An autosampler having a flowing rinse is recommended.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents 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.
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 Analar 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.
C1109 − 10 (2015)
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type I of Specification D1193 or water exceeding these specifications.
7.3 Nitric Acid (specific gravity 1.42)—Concentrated nitric acid (HNO ).
7.4 Nitric Acid, High-Purity—Nitric acid of higher purity than reagent grade, specially prepared to be low in metallic
contaminants. The acid may be prepared by sub-boiling distillation (4), or purchased from commercial sources.
7.5 Stock Solutions—May be purchased or prepared from metals or metal salts of known purity. Stock solutions should contain
known concentrations of the element of interest ranging from 100 to 10 000 mg/L.
7.6 Calibration Blank Solution, 1 % (v/v) HNO .
7.7 Calibration Reference Solutions, Instrument Check Solutions, and Linearity Check Solutions:
7.7.1 Prepare single-element or multielement calibration reference solutions by combining appropriate volumes of the stock
solutions in acid-rinsed volumetric flasks. To establish the calibration slope accurately, provide at least one solution with element
concentration that is a minimum of 100 times the L for each element. Add sufficient nitric acid to bring the final solution to 1 %
D
HNO . Prior to preparing the multielement solutions, analyze each stock solution separately to check for strong spectral
interference and the presence of impurities (5). Take care when preparing the multielement solutions to verify that the components
are compatible and stable (they do not interact to cause precipitation) and that none of the elements present exhibit mutual spectral
interference. Transfer the calibration reference solutions to acid-leached FEP TFE-fluorocarbon or polyethylene bottles for storage.
Calibration reference solutions must be verified initially using a quality control sampl
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