ASTM C1254-18

Standard Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence

SIGNIFICANCE AND USE
5.1 This test method is applicable to aqueous solutions of uranium containing 0.05 to 20 g uranium per litre of solution presented to the spectrometer.  
5.2 Either wavelength-dispersive or energy-dispersive X-ray fluorescence systems may be used provided the software accompanying the system is able to accommodate the use of internal standards.
SCOPE
1.1 This test method covers the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of mineral acid solutions containing uranium.  
1.2 This test method is valid for those solutions containing 0.05 to 20 g uranium/L as presented to the spectrometer. Higher concentrations may be covered by appropriate dilutions.  
1.3 The values stated in SI units are to be regarded as the standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9 and Note 1.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Sep-2018
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1254-13 - Standard Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence
• Effective Date: 01-Oct-2018
• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• 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 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 C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013

Overview

ASTM C1254-18 is the Standard Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence (XRF), published by ASTM International. This standard outlines consistent procedures for the preparation and analysis of mineral acid solutions containing uranium concentrations from 0.05 to 20 grams per liter, using both wavelength-dispersive and energy-dispersive XRF systems equipped to handle internal standards. It provides an efficient, reliable approach for laboratories and industries to analyze uranium content with a focus on safety, accuracy, and reproducibility.

Key Topics

• Uranium Analysis in Mineral Acids: Establishes validated procedures for accurate quantification of uranium in aqueous solutions of mineral acids using XRF technology.
• Applicability: Suitable for samples containing between 0.05 and 20 g uranium per liter. Higher concentrations may be measured by implementing appropriate sample dilutions.
• Instrumentation: Compatible with a broad range of X-ray fluorescence spectrometers, including both wavelength-dispersive (WDXRF) and energy-dispersive (EDXRF) systems, provided the software supports the use of internal standards.
• Sample Preparation: Details procedures for safe sample handling, solution preparation, and dilution to ensure the integrity of the analytical process.
• Calibration and Standardization: Specifies methods for preparing internal standards, including commonly used elements such as yttrium or strontium, and emphasizes the importance of calibration curves for robust uranium quantification.
• Interference Management: Outlines precautions regarding potential interferences and the selection of appropriate internal standards or scatter lines.
• Safety and Environmental Considerations: The standard requires users to observe stringent safety, health, and environmental practices due to the use of ionizing radiation and corrosive mineral acids.

Applications

ASTM C1254-18 is crucial for any industry or laboratory involved in uranium processing or assessment, including:

• Nuclear Fuel Cycle: Quality control and validation of uranium content in chemical processing streams, essential for nuclear fuel production, reprocessing, and waste management.
• Environmental Monitoring: Analyzing uranium concentrations in mining effluents and environmental samples to ensure regulatory compliance and environmental protection.
• Research and Development: Accurate uranium quantification in mineral acid solutions supports scientific studies in radiochemistry, nuclear chemistry, and material sciences.
• Industrial Safety Compliance: Provides a standardized framework to help meet international and governmental safety regulations for uranium handling and analysis.

Using the XRF method defined in ASTM C1254-18 delivers significant advantages:

• Non-destructive Analysis: Preserves samples and reduces hazardous waste.
• Rapid Results: Compared to wet chemical assays, XRF allows for faster throughput in routine uranium determinations.
• Reduced Sample Handling: Streamlined sample preparation lowers risk of contamination and exposure.

Related Standards

ASTM C1254-18 is often used in conjunction with other standards for XRF analysis and laboratory safety:

• ASTM C859: Terminology Relating to Nuclear Materials.
• ASTM D1193: Specification for Reagent Water, ensuring purity in analytical procedures.
• ASTM E135: Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials.
• ANSI/HPS N43.2: Radiation Safety for X-ray Diffraction and Fluorescence Analysis Equipment.

Keywords: uranium analysis, X-ray fluorescence, mineral acids, ASTM C1254-18, uranium determination, XRF, internal standards, nuclear fuel, environmental monitoring.

By following ASTM C1254-18, laboratories and industrial operations benefit from a proven, internationally recognized approach for the accurate determination of uranium in mineral acid matrices, supporting safe practices, regulatory compliance, and operational efficiency.

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: C1254 − 18
Standard Test Method for
Determination of Uranium in Mineral Acids by X-Ray
Fluorescence
This standard is issued under the fixed designation C1254; 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 2.2 Other Document:
ANSI/HPS N43.2–2001 Radiation Safety for X-ray Diffrac-
1.1 This test method covers the steps necessary for the
tion and Fluorescence Analysis Equipment
preparation and analysis by X-ray fluorescence (XRF) of
mineral acid solutions containing uranium.
3. Terminology
1.2 This test method is valid for those solutions containing
3.1 Definitions:
0.05 to 20 g uranium/L as presented to the spectrometer.
3.1.1 See Terminologies E135 and C859 for definitions of
Higher concentrations may be covered by appropriate dilu-
terms applicable to this test method.
tions.
4. Summary of Test Method
1.3 The values stated in SI units are to be regarded as the
4.1 Solutionstandardscontaining0.025guranium/Lto20g
standard.
uranium/L and an appropriate internal standard (usually either
1.4 This standard does not purport to address all of the
yttriumorstrontium),unlessascatterlineisusedinlieuof,are
safety concerns, if any, associated with its use. It is the
placed in a liquid sample holder of an X-ray spectrometer and
responsibility of the user of this standard to establish appro-
exposed to an X-ray beam capable of exciting the uranium
priate safety, health, and environmental practices and deter-
L-alpha emission line and the appropriate emission line for the
mine the applicability of regulatory limitations prior to use.
internal standard (usually the K-alpha line). The intensities
Specific precautionary statements are given in Section 9 and
generated are measured by an appropriate detector. The inten-
Note 1.
sity ratio values obtained from this data are used to calibrate
1.5 This international standard was developed in accor-
the X-ray analyzer.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5. Significance and Use
Development of International Standards, Guides and Recom-
5.1 This test method is applicable to aqueous solutions of
mendations issued by the World Trade Organization Technical
uranium containing 0.05 to 20 g uranium per litre of solution
Barriers to Trade (TBT) Committee.
presented to the spectrometer.
5.2 Either wavelength-dispersive or energy-dispersive
2. Referenced Documents
X-ray fluorescence systems may be used provided the software
2.1 ASTM Standards:
accompanying the system is able to accommodate the use of
C859 Terminology Relating to Nuclear Materials
internal standards.
D1193 Specification for Reagent Water
E135 Terminology Relating to Analytical Chemistry for
6. Interferences
Metals, Ores, and Related Materials
6.1 This test method requires the use of an appropriate
internal standard. Care must be taken to ascertain that samples
analyzed by this test method do not contain the internal
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
standard element or that this contamination has been corrected
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
for mathematically whenever present. Such corrections are not
Test.
addressed in this test method.
Current edition approved Oct. 1, 2018. Published November 2018. Originally
approved in 1993. Last previous edition approved in 2013 as C1254 – 13. DOI:
6.2 Alternatively a scatter line may be used as internal
10.1520/C1254-18.
standard in which case the preparation of internal standard
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. Available from the Health Physics Society, McLean, Virginia, 22101.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1254 − 18
solutions and subsequent doping of samples and calibration 8.7 Yttrium Oxide, Y O .
2 3
standards is unnecessary.
9. Technical Precautions
6.3 Sample must not contain significant concentration of
9.1 XRF equipment analyzes by the interaction of ionizing
anyelementsthathavemassabsorptionedgesthatfallbetween
radiation with the sample. Applicable safety regulations and
the energies of the uranium L-alpha line and the internal
standard operating procedures must be reviewed prior to the
standard line.
use of such equipment. All modern XRF spectrometers are
6.4 Care must also be taken that the choice of internal
equipped with safety interlocks to prevent accidental penetra-
standardandsamplemediumarecompatible;thatis,donotuse
tion of the X-ray beam by the user. Do NOT override these
yttrium with solutions containing HF or strontium with those
interlocks without proper training, or a second knowledgeable
having H SO .
2 4
person present during such operation. (See ANSI/HPS
N43.2–2001.)
7. Apparatus
9.2 Instrument performance may be influenced by environ-
7.1 X-RaySpectrometer—Thistestmethodisvalidforeither
mental factors such as heat, vibration, humidity, dust, stray
energy-dispersive or wavelength-dispersive systems.
electronic noise, and line voltage stability. These factors and
7.2 Sample Cups:
performance characteristics should be reviewed prior to use of
7.2.1 Prepare liquid sample cups for the X-ray spectrometer
this standard.
as described by the manufacturer. Vented, disposable sample
cups with snap-on caps are satisfactory for most such analyses;
10. Preparation of Apparatus
such cups decrease the likelihood of contamination between
10.1 Chamber Environment—The standards and samples
samples.
used in this test method are corrosive liquids. Some fumes will
7.2.2 Polyester, polyethylene, and polypropylene films have
be emitted from the sample cups. These fumes may be
been used successfully as the film window for such cups. Tests
detrimental to the spectrometer chamber. It is desirable to flush
shouldbeperformedtodeterminetheserviceabilityofanyfilm
this chamber with an appropriate gas (for example, helium and
chosen before insertion into the instrument.
nitrogen) before and during analysis. Some X-ray spectrom-
7.3 Solution Dispenser—The dispenser for the internal stan-
eters control the change of sample chamber atmosphere (air,
dard solution should be capable of reproducibly dispensing the
vacuum, helium, nitrogen) automatically through the software;
internal standard to a level of 0.5 % relative standard deviation
in others, it must be done manually. Follow the instrument
of the volume dispensed.
manufacturer’s recommendations to achieve the inert gas
environment.
8. Reagents and Materials
NOTE 1—Caution: Allow sufficient stabilization time before analysis.
8.1 Purity of Reagents—Reagent grade chemicals shall be
Care must be taken to ensure that a vacuum environment is not chosen
used in all tests. Unless otherwise indicated, it is intended that with liquid samples.
all reagents conform to the specifications of the Committee of
10.2 X-Ray Power Supply—If the power to the X-ray tube is
Analytical Reagents of the American Chemical Society where
not controlled by the instrument software, set the proper
such specifications are available. Other grades may be used
combination of voltage and current for the instrument in use.
provided it is first ascertained that the reagent is of sufficiently
These settings must be determined by the user for his instru-
high purity to permit its use without lessening the accuracy of
ment and choice of X-ray tube. Allow sufficient stabilization
the determination.
time prior to analysis.
8.2 Purity of Water—Unless otherwise indicated, references
11. Calibration and Standardization
to water shall mean reagent water conforming to Specification
D1193.
11.1 Internal Standard Solution (25.0 g/L):
11.1.1 Weigh 25 g of the chosen internal standard com-
8.3 Ferric Nitrate, Fe(NO ) ·9H O.
3 3 2
pound into an 800-mL beaker. Cover with water. Add concen-
8.4 Nitric Acid, HNO , concentrated (70 %).
trated nitric acid slowly. For yttrium oxide the reaction will be
8.5 Strontium Carbonate, SrCO .
3 slow and may require heating. For strontium carbonate, the
reaction will be vigorous.
8.6 Uranium Oxide, U O , NBLCRM-129 (or equivalent).
3 8
11.1.2 Heat on a hot plate if necessary to complete the
dissolution.
11.1.3 Cool the solution to room temperature, and transfer
Andermann,George,andKemp,J.W.,“ScatteredX-RaysasInternalStandards
to a 1000-mL volumetric flask. (Filter the solution if neces-
in X-Ray Spectroscopy,” Analytical Chemistry, Vol. 20(8), 1958.
Reagent Chemicals, American Chemical Society Specifications, American
sary.) Dilute to volume with water and mix thoroughly.
Chemical Society, Washington, DC. For suggestions o
...

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: C1254 − 13 C1254 − 18
Standard Test Method for
Determination of Uranium in Mineral Acids by X-Ray
Fluorescence
This standard is issued under the fixed designation C1254; 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 test method covers the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of mineral acid
solutions containing uranium.
1.2 This test method is valid for those solutions containing 0.05 to 20 g uranium/L as presented to the spectrometer. Higher
concentrations may be covered by appropriate dilutions.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9 and Note 1.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
C859 Terminology Relating to Nuclear Materials
C982 Guide for Selecting Components for Energy-Dispersive X-Ray Fluorescence (XRF) Systems (Withdrawn 2008)
C1118 Guide for Selecting Components for Wavelength-Dispersive X-Ray Fluorescence (XRF) Systems (Withdrawn 2011)
D1193 Specification for Reagent Water
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
2.2 Other Document:
ANSI/HPS N43.2–2001 Radiation Safety for X-ray Diffraction and Fluorescence Analysis Equipment
3. Terminology
3.1 Definitions:
3.1.1 See Terminologies E135 and C859 for definitions of terms applicable to this test method.
4. Summary of Test Method
4.1 Solution standards containing 0.025 g uranium/L to 20 g uranium/L and an appropriate internal standard (usually either
yttrium or strontium), unless a scatter line is used in lieu of, are placed in a liquid sample holder of an X-ray spectrometer and
exposed to an X-ray beam capable of exciting the uranium L-alpha emission line and the appropriate emission line for the internal
standard (usually the K-alpha line). The intensities generated are measured by an appropriate detector. The intensity ratio values
obtained from this data are used to calibrate the X-ray analyzer.
5. Significance and Use
5.1 This test method is applicable to aqueous solutions of uranium containing 0.05 to 20 g uranium per litre of solution
presented to the spectrometer.
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved Jan. 1, 2013Oct. 1, 2018. Published January 2013November 2018. Originally approved in 1993. Last previous edition approved in 19992013
as C1254 – 99 (2005).C1254 – 13. DOI: 10.1520/C1254-13.10.1520/C1254-18.
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.
Available from the Health Physics Society, McLean, Virginia, 22101.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1254 − 18
5.2 Either wavelength-dispersive or energy-dispersive X-ray fluorescence systems may be used provided the software
accompanying the system is able to accommodate the use of internal standards.
6. Interferences
6.1 This test method requires the use of an appropriate internal standard. Care must be taken to ascertain that samples analyzed
by this test method do not contain the internal standard element or that this contamination has been corrected for mathematically
whenever present. Such corrections are not addressed in this test method.
6.2 Alternatively a scatter line may be used as internal standard in which case the preparation of internal standard solutions and
subsequent doping of samples and calibration standards is unnecessary.
6.3 Sample must not contain significant concentration of any elements that have mass absorption edges that fall between the
energies of the uranium L-alpha line and the internal standard line.
6.4 Care must also be taken that the choice of internal standard and sample medium are compatible; that is, do not use yttrium
with solutions containing HF or strontium with those having H SO .
2 4
7. Apparatus
7.1 X-Ray Spectrometer—See Guide C982 or Guide C1118 for the selection of the X-ray spectrometer. This test method is valid
for either energy-dispersive or wavelength-dispersive systems.
7.2 Sample Cups:
7.2.1 Prepare liquid sample cups for the X-ray spectrometer as described by the manufacturer. Vented, disposable sample cups
with snap-on caps are satisfactory for most such analyses; such cups decrease the likelihood of contamination between samples.
7.2.2 Polyester, polyethylene, and polypropylene films have been used successfully as the film window for such cups. Tests
should be performed to determine the serviceability of any film chosen before insertion into the instrument.
7.3 Solution Dispenser—The dispenser for the internal standard solution should be capable of reproducibly dispensing the
internal standard to a level of 0.5 % relative standard deviation of the volume dispensed.
8. Reagents and Materials
8.1 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 of 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.
8.2 Purity of Water—Unless otherwise indicated, references to water shall mean reagent water conforming to Specification
D1193.
8.3 Ferric Nitrate, Fe(NO ) ·9H O.
3 3 2
8.4 Nitric Acid, HNO , concentrated (70 %).
8.5 Strontium Carbonate, SrCO .
8.6 Uranium Oxide, U O , NBL CRM-129 (or equivalent).
3 8
8.7 Yttrium Oxide, Y O .
2 3
9. Technical Precautions
9.1 XRF equipment analyzes by the interaction of ionizing radiation with the sample. Applicable safety regulations and standard
operating procedures must be reviewed prior to the use of such equipment. All modern XRF spectrometers are equipped with safety
interlocks to prevent accidental penetration of the X-ray beam by the user. Do NOT override these interlocks without proper
training, or a second knowledgeable person present during such operation. (See ANSI/HPS N43.2–2001.)
9.2 Instrument performance may be influenced by environmental factors such as heat, vibration, humidity, dust, stray electronic
noise, and line voltage stability. These factors and performance characteristics should be reviewed prior to use of this standard.
10. Preparation of Apparatus
10.1 Chamber Environment—The standards and samples used in this test method are corrosive liquids. Some fumes will be
emitted from the sample cups. These fumes may be detrimental to the spectrometer chamber. It is desirable to flush this chamber
Andermann, George, and Kemp, J. W., “Scattered X-Rays as Internal Standards in X-Ray Spectroscopy,” Analytical Chemistry, Vol. 20(8), 1958.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Available from the U.S. Department of Energy, New Brunswick Laboratory, D350, 9800 South Cass Avenue, Argonne, IL 60439, Attn: Reference Material Sales.
C1254 − 18
with an appropriate gas (for example, helium and nitrogen) before and during analysis. Some X-ray spectrometers control the
change of sample chamber atmosphere (air, vacuum, helium, nitrogen) automatically through the software; in others, it must be
done manually. Follow the instrument manufacturer’s recommendations to achieve the inert gas environment.
NOTE 1—Caution: Allow sufficient stabilization time before analysis. Care must be taken to ensure that a vacuum environment is not chosen with liquid
samples.
10.2 X-Ray Power Supply—If the power to the X-ray tube is not controlled by the instrument software, set the proper
combination of voltage and current for the instrument in use. These settings must be determined by the user for his instrument
...