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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.

General Information

Status
Historical
Publication Date
31-May-2015
ICS
13.030.30 - Special wastes
Technical Committee
C26 - Nuclear Fuel Cycle
Drafting Committee
C26.05 - Methods of Test
Current Stage
Ref Project

Relations

Replaces
ASTM C1109-10 - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry
Effective Date
01-Jun-2015
Refers
ASTM E135-20 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
01-Jan-2020
Refers
ASTM E135-19 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
15-May-2019
Refers
ASTM E135-16 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
15-May-2016
Refers
ASTM E135-15a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
01-Jul-2015
Refers
ASTM E135-15 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
15-May-2015
Refers
ASTM E135-14b - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
15-Aug-2014
Refers
ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
Effective Date
15-Jun-2014
Refers
ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
Effective Date
01-May-2014
Refers
ASTM E135-14a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
01-Apr-2014
Refers
ASTM E135-14 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
15-Feb-2014
Refers
ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
Effective Date
15-Jan-2014
Refers
ASTM E135-13a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
Effective Date
01-Dec-2013
Refers
ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
Effective Date
01-Jun-2013
Refers
ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
Effective Date
01-May-2013

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ASTM C1109-10(2015) - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission SpectroscopyASTM C1109-10(2015) - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectroscopy
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ASTM C1109-10(2015) - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectroscopy
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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 − 10 (Reapproved 2015)
Standard Practice for
Analysis of Aqueous Leachates from Nuclear Waste
Materials Using Inductively Coupled Plasma-Atomic
1
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
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.
3
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
1

---------------------- Page: 1 ----------------------
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 blan
...

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5.1 This test method is useful for the determination of concentrations of metals in many waste streams from various nuclear and non-nuclear manufacturing processes. The test method is useful for characterizing liquid wastes and liquid wastes containing undissolved solids prior to treatment, storage, or stabilization. It has the capability for the simultaneous determination of up to 26 elements.  
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1.4 This test method has been used successfully for treatment of a large variety of waste solutions and industrial process liquids. The composition of such samples is highly variable, both between waste stream types and within a single waste stream. As a result of this variability, a single acid digestion scheme may not be expected to succeed with all sample matrices. Certain elements may be recovered on a semi-quantitative basis, while most results will be highly quantitative.  
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5.1.1 U.S. Public Law 97–425, the Nuclear Waste Policy Act of 1982, provides for the deep geologic disposal of high-level radioactive waste through a system of multiple barriers. These barriers include engineered barriers designed to prevent the migration of radionuclides out of the engineered system, and the geologic host medium that provides an additional transport barrier between the engineered system and biosphere. The regulations of the U.S. Nuclear Regulatory Commission for geologic disposal require a performance confirmation program to provide data through tests and analyses, where practicable, that demonstrate engineered systems and components that are designed or assumed to act as barriers after permanent closure are functioning as intended and anticipated.  
5.1.2 IAEA Safety Requirements specify that engineered barriers shall be designed and the host environment shall be selected to provide containment of the radionuclides associated with the wastes.  
5.1.3 The Swedish Regulatory Authority has provided general advice to the repository developer that the application of best available technique be followed in connection with disposal, which means that the siting, design, construction, and operation of the repository and appurtenant syste...
SCOPE
1.1 This guide addresses how various test methods and data analyses can be used to develop models for the evaluation of the long-term alteration behavior of materials used in an engineered barrier system (EBS) for the disposal of spent nuclear fuel (SNF) and other high-level nuclear waste in a geologic repository. The alteration behavior of waste forms and EBS materials is important because it affects the retention of radionuclides within the disposal system either directly, as in the case of waste forms in which the radionuclides are initially immobilized, or indirectly, as in the case of EBS containment materials that restrict the ingress of groundwater or the egress of radionuclides that are released as the waste forms degrade.  
1.2 The purpose of this guide is to provide a scientifically-based strategy for developing models that can be used to estimate material alteration behavior after a repository is permanently closed (that is, in the post-closure period). Because the timescale involved with geological disposal precludes direct validation of predictions, mechanistic understanding of the processes based on detailed data and models and consideration of the range of uncertainty are recommended.  
1.3 This guide addresses the scientific bases and uncertainties in material behavior models and the impact on the confidence in the EBS design criteria and repository performance assessments using those models. This includes the identification and use of conservative assumptions to address uncertainty in the long-term performance of materials.  
1.3.1 Steps involved in evaluating the performance of waste forms and EBS materials include problem definition, laboratory and field testing, modeling of individual and coupled processes, and model confirmation.  
1.3.2 The estimates of waste form and EBS material performance are based on models derived from theoretical considerations, expert judgments, and interpretations of d...

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ASTM
ASTM C1718-10(2019)(Test Method)
Standard Test Method for Nondestructive Assay of Radioactive Material by Tomographic Gamma Scanning

SIGNIFICANCE AND USE
5.1 The TGS provides a nondestructive means of mapping the attenuation characteristics and the distribution of the radionuclide content of items on a voxel by voxel basis. Typically in a TGS analysis a vertical layer (or segment) of an item will be divided into a number of voxels. By comparison, a segmented gamma scanner (SGS) can determine matrix attenuation and radionuclide concentrations only on a segment by segment basis.  
5.2 It has been successfully used to quantify  238Pu, 239Pu, and 235U. SNM loadings from 0.5 g to 200 g of 239Pu (5, 6), from 1 g to 25 g of 235U (7), and from 0.1 to 1 g of 238Pu have been successfully measured. The TGS technique has also been applied to assaying radioactive waste generated by nuclear power plants (NPP). Radioactive waste from NPP is dominated by activation products (for example, 54Mn, 58Co, 60Co,  110mAg) and fission products (for example, 137Cs,  134Cs). The radionuclide activities measured in NPP waste is in the range from 3.7E+04 Bq to 1.0E+07 Bq. Some results of TGS application to non-SNM radionuclides can be found in the literature  (8).  
5.3 The TGS technique is well suited for assaying items that have heterogeneous matrices and that contain a non-uniform radionuclide distribution.  
5.4 Since the analysis results are obtained on a voxel by voxel basis, the TGS technique can in many situations yield more accurate results when compared to other gamma ray techniques such as SGS.  
5.5 In determining the radionuclide distribution inside an item, the TGS analysis explicitly takes into account the cross talk between various vertical layers of the item.  
5.6 The TGS analysis technique uses a material basis set method that does not require the user to select a mass attenuation curve apriori, provided the transmission source has at least 2 gamma lines that span the energy range of interest.  
5.7 A commercially available TGS system consists of building blocks that can easily be configured to operate the system in the ...
SCOPE
1.1 This test method describes the nondestructive assay (NDA) of gamma ray emitting radionuclides inside containers using tomographic gamma scanning (TGS). High resolution gamma ray spectroscopy is used to detect and quantify the radionuclides of interest. The attenuation of an external gamma ray transmission source is used to correct the measurement of the emission gamma rays from radionuclides to arrive at a quantitative determination of the radionuclides present in the item.  
1.2 The TGS technique covered by the test method may be used to assay scrap or waste material in cans or drums in the 1 to 500 litre volume range. Other items may be assayed as well.  
1.3 The test method will cover two implementations of the TGS procedure: (1) Isotope Specific Calibration that uses standards of known radionuclide masses (or activities) to determine system response in a mass (or activity) versus corrected count rate calibration, that applies to only those specific radionuclides for which it is calibrated, and (2) Response Curve Calibration that uses gamma ray standards to determine system response as a function of gamma ray energy and thereby establishes calibration for all gamma emitting radionuclides of interest.  
1.4 This test method will also include a technique to extend the range of calibration above and below the extremes of the measured calibration data.  
1.5 The assay technique covered by the test method is applicable to a wide range of item sizes, and for a wide range of matrix attenuation. The matrix attenuation is a function of the matrix composition, photon energy, and the matrix density. The matrix types that can be assayed range from light combustibles to cemented sludge or concrete. It is particularly well suited for items that have heterogeneous matrix material and non-uniform radioisotope distributions. Measured transmission values should be available to permit valid attenuation corrections, but are not n...

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ASTM
ASTM C1463-19(Practice)
Standard Practices for Dissolving Glass Containing Radioactive and Mixed Waste for Chemical and Radiochemical Analysis

ABSTRACT
These practices cover three standard technique for dissolving glass samples containing radioactive, nuclear, and mixed wastes. These techniques used together or independently will produce solutions that can be analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), atomic absorption spectrometry (AAS), radiochemical methods and wet chemical techniques for major components, minor components and radionuclides. The practices for dissolving silicate matrix samples each require the sample to be initially dried and ground to a fine powder. The first practice involves the mixing and fusion of the sample with sodium tetraborate (Na2B4O7) and sodium carbonate (Na2CO4) in a muffle for a given amount of time and temperature. The sample is then cooled, dissolved in hydrochloric acid, and diluted to appropriate volume for analyses. The second practice, on the other hand, involves the fusion of the sample with potassium hydroxide (KOH) or sodium peroxide (Na2O2) using an electric bunsen burner, dissolving the fused sample in water and dilute HCl, and making to volume for analyses. Finally, the third practice involves the dissolution of the sample using a microwave oven. The ground sample is digested in a microwave oven using a mixture of hydrofluoric (HF) and nitric (HNO3) acids. Boric acid is added to the resulting solution to complex excess fluoride ions.
SCOPE
1.1 These practices cover techniques suitable for dissolving glass samples that may contain nuclear wastes. These techniques used together or independently will produce solutions that can be analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), atomic absorption spectrometry (AAS), radiochemical methods and wet chemical techniques for major components, minor components and radionuclides.  
1.2 One of the fusion practices and the microwave practice can be used in hot cells and shielded hoods after modification to meet local operational requirements.  
1.3 The user of these practices must follow radiation protection guidelines in place for their specific laboratories.  
1.4 Additional information relating to safety is included in the text.  
1.5 The dissolution techniques described in these practices can be used for quality control of the feed materials and the product of plants vitrifying nuclear waste materials in glass.  
1.6 These practices are introduced to provide the user with an alternative means to Test Methods C169 for dissolution of waste containing glass in shielded facilities. Test Methods C169 is not practical for use in such facilities and with radioactive materials.  
1.7 The ICP-AES methods in Test Methods C1109 and C1111 can be used to analyze the dissolved sample with additional sample preparation as necessary and with matrix effect considerations. Additional information as to other analytical methods can be found in Test Method C169.  
1.8 Solutions from this practice may be suitable for analysis using ICP-MS after establishing laboratory performance criteria and verification that the criteria can be met. For example, Test Methods C1287 or C1637 may be used with additional sample preparation as necessary and appropriate matrix effect considerations.  
1.9 The values stated in SI units are to be regarded as standard. Units in parentheses are for information only.  
1.10 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. Specific precautionary statements are given in Sections 10, 20, and 30.  
1.11 This international standard was developed in accordance with internationally recognized principles on standardization established in the De...

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ASTM
ASTM C1133/C1133M-10(2018)(Test Method)
Standard Test Method for Nondestructive Assay of Special Nuclear Material in Low-Density Scrap and Waste by Segmented Passive Gamma-Ray Scanning

SIGNIFICANCE AND USE
5.1 Segmented gamma-ray scanning provides a nondestructive means of measuring the nuclide content of scrap and waste where the specific nature of the matrix and the chemical form and relationship between the nuclide and matrix may be unknown.  
5.2 The procedure can serve as a diagnostic tool that provides a vertical profile of transmission and nuclide concentration within the item.  
5.3 Item preparation is generally limited to good waste/scrap segregation practices that produce relatively homogeneous items that are required for any successful waste/inventory management and assay scheme, regardless of the measurement method used. Also, process knowledge should be used, when available, as part of a waste management program to complement information on item parameters, container properties, and the appropriateness of calibration factors.  
5.4 To obtain the lowest detection levels, a two-pass assay should be used. The two-pass assay also reduces problems related to potential interferences between transmission peaks and assay peaks. For items with higher activities, a single-pass assay may be used to increase throughput.
SCOPE
1.1 This test method covers the transmission-corrected nondestructive assay (NDA) of gamma-ray emitting special nuclear materials (SNMs), most commonly 235U, 239Pu, and 241Am, in low-density scrap or waste, packaged in cylindrical containers. The method can also be applied to NDA of other gamma-emitting nuclides including fission products. High-resolution gamma-ray spectroscopy is used to detect and measure the nuclides of interest and to measure and correct for gamma-ray attenuation in a series of horizontal segments (collimated gamma detector views) of the container. Corrections are also made for counting losses occasioned by signal processing limitations  (1-3).2  
1.2 There are currently several systems in use or under development for determining the attenuation corrections for NDA of radioisotopic materials (4-8). A related technique, tomographic gamma-ray scanning (TGS), is not included in this test method (9, 10, 11).  
1.2.1 This test method will cover two implementations of the Segmented Gamma Scanning (SGS) procedure: (1) Isotope Specific (Mass) Calibration, the original SGS procedure, uses standards of known radionuclide masses to determine detector response in a mass versus corrected count rate calibration that applies only to those specific radionuclides for which it is calibrated, and (2) Efficiency Curve Calibration, an alternative method, typically uses non-SNM radionuclide sources to determine system detection efficiency vs. gamma energy and thereby calibrate for all gamma-emitting radionuclides of interest (12).  
1.2.1.1 Efficiency Curve Calibration, over the energy range for which the efficiency is defined, has the advantage of providing calibration for many gamma-emitting nuclides for which half-life and gamma emission intensity data are available.  
1.3 The assay technique may be applicable to loadings up to several hundred grams of nuclide in a 208-L [55-gal] drum, with more restricted ranges to be applicable depending on specific packaging and counting equipment considerations.  
1.4 Measured transmission values must be available for use in calculation of segment-specific attenuation corrections at the energies of analysis.  
1.5 A related method, SGS with calculated correction factors based on item content and density, is not included in this standard.  
1.6 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.  
1.7 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 esta...

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