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ASTM C1109-04

(Practice)

Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry

Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry

SIGNIFICANCE AND USE
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.
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.
This practice can be used to analyze leachates from static leach testing of waste forms using C 1220.
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.
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 The analysis must be conducted with an inductively coupled plasma-atomic emission spectrometer.
1.5 The values stated in SI units are to be regarded as the standard.
1.6 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-2004
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 C1109-98 - Standard Test Method for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry
Effective Date
01-Jun-2004
Replaced By
ASTM C1109-10 - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry
Effective Date
01-Oct-2010
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-Jun-2004
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-Jun-2004
Referred By
ASTM C1220-21 - Standard Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive Waste
Effective Date
01-Jun-2004
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-Jun-2004
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-Jun-2004
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-Jun-2004
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-Jun-2004
Referred By
ASTM D7151-15 - Standard Test Method for Determination of Elements in Insulating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
Effective Date
01-Jun-2004
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-Jun-2004
Referred By
ASTM C1463-19 - Standard Practices for Dissolving Glass Containing Radioactive and Mixed Waste for Chemical and Radiochemical Analysis
Effective Date
01-Jun-2004

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ASTM C1109-04 - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission SpectrometryASTM C1109-04 - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry
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ASTM C1109-04 - Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry
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Standards Content (Sample)

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:C1109–04
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 3. Terminology
1.1 This practice is applicable to the determination of low 3.1 Definitions:
concentration and trace elements in aqueous leachate solutions 3.1.1 Inductively Coupled Plama Emission Spectroscopy
produced by the leaching of nuclear waste materials. (ICP-AES)—refer to Terminology E135.
1.2 The nuclear waste material may be a simulated (non- 3.1.2 water— refer to Terminology D1129.
radioactive) solid waste form or an actual solid radioactive 3.2 Definitions of Terms Specific to This Standard:
waste material. 3.2.1 analytical curve—the plot of net signal intensity
1.3 The leachate may be deionized water or any natural or versus elemental concentration using data obtained during
simulated leachate solution containing less than 1 % total calibration.
dissolved solids. 3.2.2 calibration—the process by which the relationship
1.4 The analysis must be conducted with an inductively between net signal intensity and elemental concentration is
coupled plasma-atomic emission spectrometer. determined for a specific element analysis.
1.5 The values stated in SI units are to be regarded as the 3.2.3 calibration blank—a 1 % (v/v) solution of nitric acid
standard. in deionized water.
1.6 This standard does not purport to address all of the 3.2.4 calibration reference solution(s)—solutions contain-
safety problems, if any, associated with its use. It is the ingknownconcentrationsofoneormoreelementsin1 %(v/v)
responsibility of the user of this standard to establish appro- nitric acid for instrument calibration.
priate safety and health practices and determine the applica- 3.2.5 detection limits (DL)—the concentration of the ana-
bility of regulatory limitations prior to use. lyte element equivalent to three times the standard deviation of
ten replicate measurements of the matrix blank.
2. Referenced Documents
3.2.6 instrument check solution(s)—solution(s) containing
2
2.1 ASTM Standards:
all the elements to be determined at concentration levels
C1009 Guide for Establishing a QualityAssurance Program approximating the concentrations in the specimens. These
for Analytical Chemistry Laboratories Within the Nuclear
solutions must also contain 1 % (v/v) nitric acid.
Industry 3.2.7 linear dynamic range—the elemental concentration
C1220 Test Method for Static Leaching of Monolithic
range over which the analytical curve remains linear to within
Waste Forms for Disposal of Radioactive Waste the precision of the analytical method.
D1129 Terminology Relating to Water
3.2.8 linearity check solution(s)—solution(s) containing the
D1193 Specification for Reagent Water elements to be determined at concentrations that cover a range
E135 Terminology Relating to Analytical Chemistry for
that is two to ten times higher and lower than the concentration
Metals, Ores, and Related Materials of these elements in the calibration reference solutions. These
solutions also contain 1 % (v/v) nitric acid.
3.2.9 non-spectral interference—changes in the apparent
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
net signal intensity from the analyte due to physical or
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
chemicalprocessesthataffectthetransportoftheanalytetothe
Test.
plasma and its vaporization, atomization, or excitation in the
CurrenteditionapprovedJune1,2004.PublishedJuly2004.Originallyapproved
plasma.
in 1988. Last previous edition approved in 1998 as C1109 – 98. DOI: 10.1520/
C1109-04.
3.2.10 off-peak background correction—during specimen
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
analysis, measurements are made of the background intensity
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
near the peak wavelength of the analytical lines. Correction of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the analytical line peak intensity to yield the net line intensity
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C1109–04
can be made by subtraction of either (a) a single intensity 6. Apparatus
measurement performed on the high or low wavelength side of
6.1 Inductively
...

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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 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 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 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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