ASTM C1474-19
(Test Method)Standard Test Method for Analysis of Isotopic Composition of Uranium in Nuclear-Grade Fuel Material by Quadrupole Inductively Coupled Plasma-Mass Spectrometry
Standard Test Method for Analysis of Isotopic Composition of Uranium in Nuclear-Grade Fuel Material by Quadrupole Inductively Coupled Plasma-Mass Spectrometry
SIGNIFICANCE AND USE
5.1 Nuclear-grade reactor fuel material must meet certain criteria, such as those described in Specifications C753, C776, C778, and C833. Included in these criteria is the uranium isotopic composition. This test method is designed to demonstrate whether or not a given material meets an isotopic requirement and whether the effective fissile content is in compliance with the purchaser's specifications.
SCOPE
1.1 This test method is applicable to the determination of the isotopic composition of uranium (U) in nuclear-grade fuel material. The following isotopic weight percentages are determined using a quadrupole inductively coupled plasma-mass spectrometer (Q-ICP-MS): 233U, 234U, 235U, 236U, and 238U. The analysis can be performed on various material matrices after acid dissolution and sample dilution into water or dilute nitric (HNO3) acid. These materials include: fuel product, uranium oxide, uranium oxide alloys, uranyl nitrate (UNH) crystals, and solutions. The sample preparation discussed in this test method focuses on fuel product material but may be used for uranium oxide or a uranium oxide alloy. Other preparation techniques may be used and some references are given. Purification of the uranium by anion-exchange extraction is not required for this test method, as it is required by other test methods such as radiochemistry and thermal ionization mass spectroscopy (TIMS). This test method is also described in ASTM STP 13442.
1.2 The 233U isotope is primarily measured as a qualitative measure of its presence by comparing the 233U peak intensity to a background point since it is not normally found present in materials. The example data presented in this test method do not contain any 233U data. A 233U enriched standard is given in Section 8, and it may be used as a quantitative spike addition to the other standard materials listed.
1.3 A single standard calibration technique is used. Optimal accuracy (or a low bias) is achieved through the use of a single standard that is closely matched to the enrichment of the samples. The intensity or concentration is also adjusted to within a certain tolerance range to provide good statistical counting precision for the low-abundance isotopes while maintaining a low bias for the high-abundance isotopes, resulting from high-intensity dead time effects. No blank subtraction or background correction is utilized. Depending upon the standards chosen, enrichments between depleted and 97 % can be quantified. The calibration and measurements are made by measuring the intensity ratios of each low-abundance isotope to the intensity sum of 233U, 234U, 235U, 236U, and 238U. The high-abundance isotope is obtained by difference.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only. The instrument is calibrated and the samples measured in units of isotopic weight percent (Wt %). For example, the 235U enrichment may be stated as Wt % 235U or as g 235U/100 g of U. Statements regarding dilutions, particularly for μg/g concentrations or lower, are given assuming a solution density of 1.0 since the uranium concentration of a solution is not important when making isotopic ratio measurements other than to maintain a reasonably consistent intensity within a tolerance range.
1.5 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.
1.6 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 ...
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1474 − 19
Standard Test Method for
Analysis of Isotopic Composition of Uranium in Nuclear-
Grade Fuel Material by Quadrupole Inductively Coupled
1
Plasma-Mass Spectrometry
This standard is issued under the fixed designation C1474; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope countingprecisionforthelow-abundanceisotopeswhilemain-
taining a low bias for the high-abundance isotopes, resulting
1.1 This test method is applicable to the determination of
from high-intensity dead time effects. No blank subtraction or
the isotopic composition of uranium (U) in nuclear-grade fuel
background correction is utilized. Depending upon the stan-
material. The following isotopic weight percentages are deter-
dards chosen, enrichments between depleted and 97% can be
mined using a quadrupole inductively coupled plasma-mass
233 234 235 236 238 quantified. The calibration and measurements are made by
spectrometer (Q-ICP-MS): U, U, U, U, and U.
measuring the intensity ratios of each low-abundance isotope
The analysis can be performed on various material matrices
233 234 235 236 238
to the intensity sum of U, U, U, U, and U. The
after acid dissolution and sample dilution into water or dilute
high-abundance isotope is obtained by difference.
nitric (HNO ) acid. These materials include: fuel product,
3
uranium oxide, uranium oxide alloys, uranyl nitrate (UNH) 1.4 The values stated in SI units are to be regarded as the
crystals, and solutions. The sample preparation discussed in standard. The values given in parentheses are for information
this test method focuses on fuel product material but may be only.Theinstrumentiscalibratedandthesamplesmeasuredin
235
used for uranium oxide or a uranium oxide alloy. Other unitsofisotopicweightpercent(Wt%).Forexample,the U
235 235
preparation techniques may be used and some references are enrichment may be stated as Wt% Uorasg U/100 g of
given. Purification of the uranium by anion-exchange extrac- U. Statements regarding dilutions, particularly for µg/g con-
tion is not required for this test method, as it is required by centrations or lower, are given assuming a solution density of
other test methods such as radiochemistry and thermal ioniza- 1.0 since the uranium concentration of a solution is not
tion mass spectroscopy (TIMS). This test method is also importantwhenmakingisotopicratiomeasurementsotherthan
2
described in ASTM STP 1344 . tomaintainareasonablyconsistentintensitywithinatolerance
233 range.
1.2 The U isotope is primarily measured as a qualitative
233
1.5 This standard does not purport to address all of the
measure of its presence by comparing the U peak intensity
safety concerns, if any, associated with its use. It is the
to a background point since it is not normally found present in
responsibility of the user of this standard to establish appro-
materials. The example data presented in this test method do
233 233
priate safety, health, and environmental practices and deter-
notcontainany Udata.A Uenrichedstandardisgivenin
mine the applicability of regulatory limitations prior to use.
Section 8, and it may be used as a quantitative spike addition
Specific precautionary statements are given in Section 9.
to the other standard materials listed.
1.6 This international standard was developed in accor-
1.3 Asingle standard calibration technique is used. Optimal
dance with internationally recognized principles on standard-
accuracy(oralowbias)isachievedthroughtheuseofasingle
ization established in the Decision on Principles for the
standard that is closely matched to the enrichment of the
Development of International Standards, Guides and Recom-
samples. The intensity or concentration is also adjusted to
mendations issued by the World Trade Organization Technical
within a certain tolerance range to provide good statistical
Barriers to Trade (TBT) Committee.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
2. Referenced Documents
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
3
2.1 ASTM Standards:
Test.
Current edition approved Feb. 1, 2019. Published February 2019. Originally
approved in 2000. Last previous edition approved in 2011 as C1474–00(2011).
DOI: 10.1520/C1474-19.
2 3
Policke,T.A.,Bolin,R.N.,andHarris,T.L.,“UraniumIsotopeMeasurements For referenced ASTM standards, visit the ASTM website, www.astm.org, or
by Quqdrupole ICP-MS for Process Monitorin
...
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: C1474 − 00 (Reapproved 2011) C1474 − 19
Standard Test Method for
Analysis of Isotopic Composition of Uranium in Nuclear-
Grade Fuel Material by Quadrupole Inductively Coupled
1
Plasma-Mass Spectrometry
This standard is issued under the fixed designation C1474; 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 is applicable to the determination of the isotopic composition of uranium (U) in nuclear-grade fuel
material. The following isotopic weight percentages are determined using a quadrupole inductively coupled plasma-mass
233 234 235 236 238
spectrometer (Q-ICP-MS): U, U, U, U, and U. The analysis can be performed on various material matrices after acid
dissolution and sample dilution into water or dilute nitric (HNO ) acid. These materials include: fuel product, uranium oxide,
3
uranium oxide alloys, uranyl nitrate (UNH) crystals, and solutions. The sample preparation discussed in this test method focuses
on fuel product material but may be used for uranium oxide or a uranium oxide alloy. Other preparation techniques may be used
and some references are given. Purification of the uranium by anion-exchange extraction is not required for this test method, as
it is required by other test methods such as radiochemistry and thermal ionization mass spectroscopy (TIMS). This test method
2
is also described in ASTM STP 1344 .
233 233
1.2 The U isotope is primarily measured as a qualitative measure of its presence by comparing the U peak intensity to a
background point since it is not normally found present in materials. The example data presented in this test method do not contain
233 233
any U data. A U enriched standard is given in Section 8, and it may be used as a quantitative spike addition to the other
standard materials listed.
1.3 A single standard calibration technique is used. Optimal accuracy (or a low bias) is achieved through the use of a single
standard that is closely matched to the enrichment of the samples. The intensity or concentration is also adjusted to within a certain
tolerance range to provide good statistical counting precision for the low-abundance isotopes while maintaining a low bias for the
high-abundance isotopes, resulting from high-intensity dead time effects. No blank subtraction or background correction is utilized.
Depending upon the standards chosen, enrichments between depleted and 97 % can be quantified. The calibration and
233 234 235
measurements are made by measuring the intensity ratios of each low-abundance isotope to the intensity sum of U, U, U,
236 238
U, and U. The high-abundance isotope is obtained by difference.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
235
The instrument is calibrated and the samples measured in units of isotopic weight percent (Wt %). For example, the U
235 235
enrichment may be stated as Wt % U or as g U/100 g of U. Statements regarding dilutions, particularly for ug/gμg/g
concentrations or lower, are given assuming a solution density of 1.0 since the uranium concentration of a solution is not important
when making isotopic ratio measurements other than to maintain a reasonably consistent intensity within a tolerance range.
1.5 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.
1.6 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.
1
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 June 1, 2011Feb. 1, 2019. Published June 2011February 2019. Originally approved in 2000. Last previous edition approved in 20062011 as
ε1
C1474 – 00 (20
...
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