ASTM C1109-23

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 % 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 standard. No other units of measurement are included in this standard.  
1.8 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.  
1.9 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: 30-Nov-2023
• ICS: 13.030.30 - Special wastes
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1109-10(2015) - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectroscopy
• Effective Date: 01-Dec-2023
• Refers: ASTM E438-92(2024) - Standard Specification for Glasses in Laboratory Apparatus
• Effective Date: 01-Feb-2024
• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C859-23 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Feb-2023
• Refers: ASTM E438-92(2018) - Standard Specification for Glasses in Laboratory Apparatus
• Effective Date: 01-Jan-2018
• Referred By: ASTM D5185-18 - Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Dec-2023
• Referred By: ASTM D7691-23 - Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Dec-2023
• Referred By: ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Dec-2023
• Referred By: ASTM C1463-19 - Standard Practices for Dissolving Glass Containing Radioactive and Mixed Waste for Chemical and Radiochemical Analysis
• Effective Date: 01-Dec-2023
• Referred By: ASTM D8088-16(2022) - Standard Practice for Determination of the Six Major Rare Earth Elements in Fluid Catalytic Cracking Catalysts, Zeolites, Additives, and Related Materials by Inductively Coupled Plasma Optical Emission Spectroscopy
• Effective Date: 01-Dec-2023
• Referred By: ASTM C1111-10(2020) - Standard Test Method for Determining Elements in Waste Streams by Inductively Coupled Plasma-Atomic Emission Spectroscopy
• Effective Date: 01-Dec-2023
• Referred By: ASTM C1220-21 - Standard Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive Waste
• Effective Date: 01-Dec-2023
• Referred By: ASTM C1285-21 - Standard Test Methods for Determining Chemical Durability of Nuclear, Hazardous, and Mixed Waste Glasses and Multiphase Glass Ceramics: The Product Consistency Test (PCT)
• Effective Date: 01-Dec-2023
• Referred By: ASTM D7151-15(2023) - Standard Test Method for Determination of Elements in Insulating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Dec-2023
• Referred By: ASTM C1662-18 - Standard Practice for Measurement of the Glass Dissolution Rate Using the Single-Pass Flow-Through Test Method
• Effective Date: 01-Dec-2023

Overview

ASTM C1109-23 outlines the standard practice for the analysis of aqueous leachates from nuclear waste materials using Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES). This standard enables laboratories to accurately determine low concentrations and trace elements that leach from various nuclear waste forms, such as glasses, ceramics, and cements, into aqueous solutions. The practice applies to both simulated (non-radioactive) waste and solid radioactive waste materials. This method is essential for compliance with regulatory guidelines and for ensuring environmental and operational safety in the nuclear industry.

Key Topics

• ICP-AES Analysis: The standard describes the use of ICP-AES, a sensitive and robust analytical technique, for detecting trace metals and other elements in leachates resulting from nuclear waste materials.
• Sample Type and Preparation:
  • Applicable to leachates produced using deionized water or other aqueous solutions containing less than 1% dissolved solids.
  • Guidance on preparing calibration, check, and sample solutions, emphasizing the need for acid concentrations and matrix matching.
• Radioactive and Non-Radioactive Waste:
  • Offers specific considerations for handling radioactive samples, such as the use of shielded and contained ICP-AES systems with filtered exhaust.
• Quality Control and Calibration:
  • Details on calibration procedures, use of calibration blanks, reference solutions, check solutions, and control limits based on standard deviation.
  • Emphasizes routine instrument checks and methods for drift and interference correction (both spectral and non-spectral).
• Data Interpretation and Correction:
  • Addresses background correction, spectral interference, non-spectral interference, and the method of standard additions for accurate quantification.
• Precision and Bias:
  • Discusses factors influencing analytical precision and bias, including instrument performance, calibration accuracy, and interference management.

Applications

The ASTM C1109-23 standard practice has critical applications in the nuclear fuel cycle and waste management sectors. Key uses include:

• Environmental Monitoring: Determination of trace element release from nuclear waste forms, contributing to environmental safety assessments.
• Regulatory Compliance: Supports compliance with international and national regulations regarding nuclear waste disposal and storage.
• Quality Assurance in Analytical Laboratories: Ensures reliable and repeatable results, maintaining laboratory accreditation and adherence to industry best practices.
• Research and Development: Applicable in studies focused on the behavior of nuclear waste materials and the integrity of waste form barriers over time.
• Supporting Waste Form Testing: Directly supports practices such as the static leach testing method (ASTM C1220) for evaluating nuclear waste forms.

Related Standards

• ASTM C1220: Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive Waste.
• ASTM C1009: Guide for Quality Assurance in Analytical Laboratories within the Nuclear Industry.
• ASTM D1193: Specification for Reagent Water.
• ASTM D7035: Test Method for Determination of Metals and Metalloids in Airborne Particulate Matter by ICP-AES.
• ASTM E135/E177: Analytical chemistry and measurement practices for precision and bias.
• ISO 1042 / ISO 3585 / ISO 8655: International standards for laboratory glassware, borosilicate glass properties, and piston-operated volumetric instruments.

Practical Value

Adopting ASTM C1109-23 for ICP-AES analysis of nuclear waste leachates ensures:

• Sensitive, reliable detection of trace contaminants.
• Consistency in analytical methods, promoting comparability across facilities and over time.
• Comprehensive data for decision-makers regarding nuclear waste storage, transport, and disposal safety.

By following this standard, laboratories and organizations enhance their analytical integrity and support the long-term stewardship of nuclear materials.

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: C1109 − 23
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 1.9 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This practice is applicable to the determination of low
ization established in the Decision on Principles for the
concentration and trace elements in aqueous leachate solutions
Development of International Standards, Guides and Recom-
produced by the leaching of nuclear waste materials, using
mendations issued by the World Trade Organization Technical
inductively coupled plasma-atomic emission spectroscopy
Barriers to Trade (TBT) Committee.
(ICP-AES).
1.2 The nuclear waste material may be a simulated (non-
2. Referenced Documents
radioactive) solid waste form or an actual solid radioactive
2.1 ASTM Standards:
waste material.
C859 Terminology Relating to Nuclear Materials
1.3 The leachate may be deionized water or any natural or
C1009 Guide for Establishing and Maintaining a Quality
simulated leachate solution containing less than 1 % total
Assurance Program for Analytical Laboratories Within the
dissolved solids.
Nuclear Industry
C1220 Test Method for Static Leaching of Monolithic Waste
1.4 This practice should be used by analysts experienced in
Forms for Disposal of Radioactive Waste
the use of ICP-AES, the interpretation of spectral and non-
D1193 Specification for Reagent Water
spectral interferences, and procedures for their correction.
D7035 Test Method for Determination of Metals and Met-
1.5 No detailed operating instructions are provided because
alloids in Airborne Particulate Matter by Inductively
of differences among various makes and models of suitable
Coupled Plasma Atomic Emission Spectrometry (ICP-
ICP-AES instruments. Instead, the analyst shall follow the
AES)
instructions provided by the manufacturer of the particular
E135 Terminology Relating to Analytical Chemistry for
instrument. This test method does not address comparative
Metals, Ores, and Related Materials
accuracy of different devices or the precision between instru-
E177 Practice for Use of the Terms Precision and Bias in
ments of the same make and model.
ASTM Test Methods
1.6 This practice contains notes that are explanatory and are
E288 Specification for Laboratory Glass Volumetric Flasks
not part of the mandatory requirements of the method.
E438 Specification for Glasses in Laboratory Apparatus
E1154 Specification for Piston or Plunger Operated Volu-
1.7 The values stated in SI units are to be regarded as
metric Apparatus and Operator Qualification
standard. No other units of measurement are included in this
standard.
3. Terminology
1.8 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.1 For definitions of pertinent terms not listed here, see
Terminology C859.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
3.2 Definitions:
mine the applicability of regulatory limitations prior to use.
3.2.1 atomic emission—characteristic radiation emitted by
an electronically excited atomic species. D7035
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. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2023. Published January 2024. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1988. Last previous edition approved in 2015 as C1109 – 10 (2015). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/C1109-23. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1109 − 23
3.2.1.1 Discussion—In atomic (or optical) emission 3.2.12 linear dynamic range—the elemental concentration
spectrometry, a very high-temperature environment, such as a range over which the calibration curve remains linear to within
plasma, is used to create excited state atoms. For analytical the precision of the analytical method.
purposes, characteristic emission signals from elements in their
3.2.13 linearity check solution(s)—solution(s) of nitric acid
excited states are then measured at specific wavelengths.
with a volume fraction concentration of 1 % containing the
3.2.2 background correction—process of correcting the in- elements to be determined at concentrations that cover a range
tensity at an analytical wavelength for the intensity due to the
that is two to ten times higher and lower than the concentration
underlying spectral background of a blank. D7035 of these elements in the calibration reference solutions.
3.2.2.1 Discussion—During sample analysis, measurements
3.2.14 non-spectral interference—changes in the apparent
are made of the background intensity near the peak wavelength
net signal intensity from the analyte due to physical or
of the analytical lines. Correction of the analytical line peak
chemical processes that affect the transport of the analyte to the
intensity to yield the net line intensity can be made by
plasma and its vaporization, atomization, or excitation in the
subtraction of either (a) a single intensity measurement per-
plasma.
formed on the high or low wavelength side of the analytical
3.2.15 sensitivity—the slope of the linear dynamic range.
line (single-point background correction), or (b) an interpo-
lated background intensity from background measurements 3.2.16 spectral interference—an interference caused by the
acquired on both the high and low wavelength sides of the emission from a species other than the analyte of interest.
analytical line (double-point background correction). D7035
3.2.16.1 Discussion—Sources of spectral interference in-
3.2.3 bias—difference between the expectation of the test
clude spectral line overlaps, broadened wings of intense
results and an accepted reference value. E177
spectral lines, ion-atom recombination continuum emission,
3.2.4 calibration blank solution—calibration solution pre-
molecular band emission, and stray (scattered) light effects.
pared without the addition of any reference solutions. D7035
3.2.5 calibration curve—plot of net signal intensity versus
4. Summary of Practice
elemental concentration using data obtained during calibration.
4.1 Aqueous leachates are prepared, using Test Method
3.2.6 calibration reference solution(s)—solutions contain-
C1220, for analysis using this practice.
ing known concentrations of one or more elements in 1 %
4.2 The general principles of emission spectrometric analy-
nitric acid for instrument calibration.
sis are given in Ref (3). In this practice, elemental constituents
3.2.7 critical limit (L )—minimum significant value of an
C
of aqueous leachate solutions are determined simultaneously or
estimated net signal or concentration, applied as a discrimina-
sequentially by inductively coupled plasma-atomic emission
tor against background noise. (1)
spectroscopy (ICP-AES).
3.2.8 inductively coupled plasma (ICP)—a high-
4.3 Samples are prepared by filtration if needed to remove
temperature discharge generated by a flowing conductive gas,
particulates and acidification to match calibration reference
normally argon, through a magnetic field induced by a load coil
solutions. Filtration should be the last resort to clarify a
that surrounds the tubes carrying the gas. D7035
solution since leach studies are designed to determine the
3.2.9 instrument check solution(s)—solution(s) containing
absolute amount of material removed from a waste form by
all the elements to be determined at concentration levels
aqueous leaching.
approximating the concentrations in the samples. These solu-
4.4 Additional general guidelines are provided in Guide
tions must also contain 1 % nitric acid.
C1009, Specification D1193, Terminology C859, and Termi-
3.2.10 interelement correction—a spectral interference cor-
nology E135.
rection technique in which emission contributions from inter-
fering elements that emit radiation at the analyte wavelength
5. Significance and Use
are subtracted from the apparent analyte emission after mea-
suring the interfering element concentrations at other 5.1 This practice may be used to determine concentrations
wavelengths. D7035
of elements leached from nuclear waste materials (glasses,
ceramics, cements) using an aqueous leachant. If the nuclear
3.2.11 limit of detection (L )—value for which the false
D
waste material is radioactive, a suitably contained and shielded
negative error is B using a given critical limit. (1)
ICP-AES spectrometer system with a filtered exit-gas system
3.2.11.1 Discussion—If the analytical standard deviation is
must be used, but no other changes in the practice are required.
constant with respect to concentration, this can be computed as
The leachant may be deionized water or any aqueous solution
3.7 times the standard deviation of the analytical results from
containing less than 1 % total solids.
ten matrix blank samples spiked at approximately the antici-
pated detection limit; otherwise, see references (1, 2) for
5.2 This practice as written is for the analysis of solutions
additional guidance.
containing 1 % 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
The boldface numbers in parentheses refer to the list of references at the end
of this standard. value whenever 1 % nitric acid appears here. It is important
C1109 − 23
that the acid type and content of the reference and check 7.4 Nitric Acid, Volume Fraction 1 %—Volumetrically di-
solutions closely match the leachate solutions to be analyzed. lute 10 mL of concentrated HNO (7.3) to 1000 mL with water.
5.3 This practice can be used to analyze leachates from
NOTE 3—The volume fraction can be up to 5 % provided the same
volume fraction is used in all calibration blank, calibration reference, and
static leach testing of waste forms using Test Method C1220.
check solutions.
6. Apparatus
7.5 Stock Solutions—May be purchased or prepared from
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-
assumed to be present.
ing from 100 mg ⁄L to 10 000 mg ⁄L.
6.2 Glassware, volumetric flasks complying with the re-
7.6 Calibration Blank Solution, 1 % HNO .
quirements of Specification E288, made of borosilicate glass 3
complying with the requirements of Specification E438. Glass-
7.7 Calibration Reference Solutions, Instrument Check
ware should be cleaned before use by soaking in nitric acid and
Solutions, and Linearity Check Solutions:
then rinsing thoroughly with water.
7.7.1 Prepare single-element or multielement calibration
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
6.4 Piston-operated Volumetric Pipettors and Dispensers,
with element concentration that is a minimum of 100 times the
complying with the requirements of Specification E1154, for
L for each element. Add sufficient concentrated HNO to
D 3
pipetting and dispensing of solutions, acids, and so forth.
bring the final solution to 1 % HNO . Prior to preparing the
6.5 Bottles, tetrafluoroethylene or polyethylene, for storage
multielement solutions, analyze each stock solution separately
of calibration and check solutions.
to check for strong spectral interference and the presence of
impurities (4). Take care when preparing the multielement
6.6 Disposable Gloves, impermeable, for protection from
solutions to verify that the components are compatible and
corrosive substances. Polyvinyl chloride (PVC) gloves are
stable (they do not interact to cause precipitation) and that none
suitable.
of the elements present exhibit mutual spectral interference.
6.7 Inductively Coupled Plasma-Atomic Emission
Transfer the calibration reference solutions to acid-leached
Spectrometer, computer controlled, with a spectral bandpass of
FEP TFE-fluorocarbon or polyethylene bottles for storage.
0.05 nm or less, is required to provide the necessary spectral
Calibration reference solutions must be verified initially using
resolution.
a quality control sample and monitored periodically for stabil-
NOTE 1—The spectrometer may be of the simultaneous multielement or ity.
sequential scanning type. The spectrometer may be of the air-path, inert
NOTE 4—Solutions in polyethylene bottles are subject to transpiration
gas-path, or vacuum type, with spectral lines selected appropriately for use
losses that may affect the assigned concentration values.
with the specific instrument.
NOTE 2—An autosampler having a flowing rinse is recommended.
7.7.2 Prepare the instrument check solution(s) and linearity
check solutions in a similar manner.
7. Reagents and Materials
7.7.3 Fresh solutions should be prepared as needed with the
7.1 Purity of Reagents—Reagent grade chemicals shall be
realization that concentrations can change over time. The
used in all tests. Unless otherwise indicated, it is intended that
recommended maximum shelf life for calibration reference
all reagents conform to the specifications of the Committee on
solutions, instrument check solutions, and linearity check
Analytical Reagents of the American Chemical Society where
solutions is one month.
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
8. Sample Preparation
high purity to permit its use without lessening the accuracy of
8.1 If necessary to remove solids or suspended colloids,
the determination.
filter the leachate through a clean filter, using an inert filter
7.2 Purity of Water—Unless otherwise indicated, references
support (avoid the use of fritted glass supports). Examine the
to water shall be understood to mean reagent water as defined
filtered leachate to verify the absence of visible solids or
by Type I of Specification D1193 or water exceeding these
suspended colloids. The deposit on the filter may be analyzed
specifications.
separately if required.
7.3 Nitric Acid (Specific Gravity 1.42)—Concentrated nitric
8.2 Prepare filtered and unfiltered aliquots of a calibration
acid (HNO ) of sufficiently high purity to permit its use
3 blank solution, and compare the results of these aliquots to
without lessening the accuracy of the determination.
determine whether the filter membrane contributes to the blank
level of the filtered solution.
NOTE 5—Step 8.2 may be omitted if none of the samples requires
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
filtration.
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical
8.3 Add sufficient high-purity concentrated HNO to bring
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
the leachate sample solution to volume in 1 % HNO . If the
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma- 3
copeial Convention, Inc. (USPC), Rockville, MD. leachate is known to be a chloride solution, or HNO is
C1109 − 23
undesirable for other experimental reasons, concentrated hy- 9.2.1 The lowest attainable L ,
D
drochloric or other mineral acid may be used instead. The acid 9.2.2 The acceptable linear dynamic range,
conditions of the calibration and check solutions used in the 9.2.3 Avoidance or minimization of spectral and non-
analytical procedure must match those of the leachate sample. spectral interference, and
It is necessary that quantities of acid and sample be carefully 9.2.4 Best attainable precision.
measured during acidification to allow correction of results to
9.3 Follow the spectrometer manufacturer’s recommenda-
account for dilution.
tion wherever possible in establishing operating conditions.
For simultaneous multielement systems, the optimum plasma
9. Analytical Conditions
viewing position and set of operating conditions is usually a
9.1 Analytical Lines—Suggested analytical lines for typical
compromise (14). The combination of conditions selected must
elements are given in Table 1. Additional lines for these and
be used in all subsequent ICP operations, including determi-
other elements of interest, and information about possible
nation of L , calibrations, sample analyses, and performance
D
interfering lines, can be found in compilations of analytical
checks. Systematic use of an appropriate method such as
lines for ICP-AES (5-13).
reference to an atom-to-ion emission intensity ratio (4) to
ensure reproducible conditions is recommended.
9.2 Selection of Analytical Conditions—Select an optimum
combination of analytical lines, background correction
9.4 Perform at least ten consecutive measurements of a
methods, plasma viewing position, and plasma/spectrometer
matrix blank and calculate L as described in 3.2.11.1.
D
operating conditions to obtain the following for each element:
9.5 Perform experiments to determine the linear dynamic
range for each element of interest. Use L and the linear
D
TABLE 1 Suggested Analytical Wavelengths of Typical Elements
dynamic range as a guide in the preparation of calibration
A
for ICP-AES
reference solutions and linearity check solut
...

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 (Reapproved 2015) C1109 − 23
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. No other units of measurement are included in this standard.
1.8 This standard does not purport to address all of the safety problems,concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and healthsafety, health, and environmental practices and
determine the applicability of regulatory limitations prior to use.
1.9 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.
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 June 1, 2015Dec. 1, 2023. Published June 2015January 2024. Originally approved in 1988. Last previous edition approved in 20102015 as
C1109 – 10.C1109 – 10 (2015). DOI: 10.1520/C1109-10R15.10.1520/C1109-23.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1109 − 23
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
E288 Specification for Laboratory Glass Volumetric Flasks
E438 Specification for Glasses in Laboratory Apparatus
E1154 Specification for Piston or Plunger Operated Volumetric Apparatus and Operator Qualification
2.2 ISO and European Standards:
ISO 1042 Laboratory Glassware—One-mark Volumetric Flasks
ISO 3585 Borosilicate Glass 3.3—Properties
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—difference 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.
3.2.4 calibration blank solution—calibration solution prepared without the addition of any reference solutions. D7035
3.2.5 calibration curve—plot of net signal intensity versus elemental concentration using data obtained during calibration.
3.2.6 calibration reference solution(s)—solutions containing known concentrations of one or more elements in 1 % (v/v) nitric
acid for instrument calibration.
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.
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3.2.7 critical limit (L )—minimum significant value of an estimated net signal or concentration, applied as a discriminator against
C
background noise. (1)
3.2.8 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
3.2.9 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.
3.2.10 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
3.2.11 limit of detection (L )—value for which the false negative error is B using a given critical limit. (1)
D
3.2.11.1 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.
3.2.12 linear dynamic range—the elemental concentration range over which the calibration curve remains linear to within the
precision of the analytical method.
3.2.13 linearity check solution(s)—solution(s) of nitric acid with a volume fraction concentration of 1 % 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.
3.2.14 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.
3.2.15 sensitivity—the slope of the linear dynamic range.
3.2.16 spectral interference—an interference caused by the emission from a species other than the analyte of interest. D7035
3.2.16.1 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.
The boldface numbers in parentheses refer to the list of references at the end of this standard.
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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 ISOSpecification E2881042,, made of borosilicate glass
complying with the requirements of ISOSpecification E4383585. 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 ISOSpecification E11548655,, 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.
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(Specific Gravity 1.42)—Concentrated nitric acid (HNO ).) of sufficiently high purity to permit its
use without lessening the accuracy of the determination.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society,ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, 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.
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7.4 Nitric Acid, High-Purity—Volume Fraction 1 %—Nitric acid of higher purityVolumetrically dilute 10 mL of concentrated
HNO than reagent grade, specially prepared to be low in metallic contaminants. The acid may be prepared by sub-boiling
distillation (47.3),) or purchased from commercial sources.to 1000 mL with water.
NOTE 3—The volume fraction can be up to 5 % provided the same volume fraction is used in all calibration blank, calibration reference, and check
solutions.
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 100100 mg ⁄L to 10 000 mg/L.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 acidconcentrated HNO to bring the
D 3
final solution to 1 % HNO . Prior to preparing the multielement solutions, analyze each stock solution separately to check for
strong spectral interference and the presence of impurities (54). 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 sample and monitored
periodically for stability.
NOTE 4—Solutions in polyethylene bottles are subject to transpiration losses that may affect the assigned concentration values.
7.7.2 Prepare the instrument check solution(s) and linearity check solutions in a similar manner.
7.7.3 Fresh solutions should be prepared as needed with the realization that concentrations can change over time. The
recommended maximum shelf life for calibration reference solutions, instrument check solutions, and linearity check solutions is
one month.
8. Sample Preparation
8.1 If necessary to remove solids or suspended colloids, filter the leachate through a clean filter, using an inert filter support (avoid
the use of fritted glass supports). Examine the filtered leachate to verify the absence of visible solids or suspended colloids. The
deposit on the filter may be analyzed separately if required.
8.2 Prepare filtered and unfiltered aliquots of a calibration blank solution, and compare the results of these aliquots to determine
whether the filter membrane contributes to the blank level of the filtered solution.
NOTE 5—Step 8.2 may be omitted if none of the samples requires filtration.
8.3 Add sufficient high-purity concentrated nitricHNO acid to bring the leachate sample solution to volume in 1 % HNO . If the
3 3
leachate is known to be a chloride solution, or nitricHNO acid is undesirable for other experimental reasons, concentrated
hydrochloric or other mineral acid may be used instead. The acid conditions of the calibration and check solutions used in the
analytical procedure must match those of the leachate sample. It is necessary that quantities of acid and sample be carefully
measured during acidification to allow correction of results to account for dilution.
NOTE 5—It is necessary that quantities of acid and sample be carefully measured during acidification to allow correction of results to account for dilution.
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9. Analytical Conditions
9.1 Analytical Lines—Suggested analytical lines for typical elements are given in Table 1. Additional lines for these and other
elements of interest, and information about possible interfering lines, can be found in compilations of analytical lines for ICP-AES
(6-5-1413).
9.2 Selection of Analytical Conditions—Select an optimum combination of analytical lines, background correction methods,
plasma viewing position, and plasma/spectrometer operating conditions to obtain the following for each element:
9.2.1 The lowest attainable L ,
D
9.2.2 The acceptable linear dynamic range,
9.2.3 Avoidance or minimization of spectral and non-spectral interference, and
9.2.4 Best attainable precision.
TABLE 1 Suggested Analytical Wavelengths of Typical Elements
A
for ICP-AES
Suggested Estimated Alternative Estimated
Element Wavelength, Detection Wavelength, Detection
nm Limit, mg/L nm Limit, mg/L
Aluminum 308.22 0.04 237.32 0.03
Americium 283.23 0.01 292.06 >0.01
B
Arsenic 193.70 0.05 189.04 0.01
Barium 493.41 0.002 455.40 0.001
Beryllium 234.86 0.0003 313.04 0.0003
Boron 249.77 0.005 249.68 0.005
Cadmium 214.44 0.002 . .
Calcium 317.93 0.01 393.37 0.0002
Cerium 418.66 0.05 413.76 0.05
Chromium 267.72 0.007 205.55 0.006
Dyspr
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