ASTM C1477-08
(Test Method)Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry
Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry
SIGNIFICANCE AND USE
The test method is capable of measuring uranium isotopic abundances of 234U, 235U, 236U and 238U as required by Specifications C 787 and C 996.
SCOPE
1.1 This test method covers the isotopic abundance analysis of 234U, 235U, 236U and 238U in samples of hydrolysed uranium hexafluoride (UF6) by inductively coupled plasma source, multicollector, mass spectrometry (ICP-MC-MS). The method applies to material with 235U abundance in the range of 0.2 to 6 % mass. This test method is also described in ASTM STP 1344.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:C1477 −08
StandardTest Method for
Isotopic Abundance Analysis of Uranium Hexafluoride and
Uranyl Nitrate Solutions by Multi-Collector, Inductively
1
Coupled Plasma-Mass Spectrometry
This standard is issued under the fixed designation C1477; 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:
STP 1344 Applications of Inductively Coupled Plasma-
1.1 This test method covers the isotopic abundance analysis
234 235 236 238 Mass Spectrometry (ICP-MS) to Radionuclide Determi-
of U, U, U and U in samples of hydrolysed ura-
3
nations
nium hexafluoride (UF ) by inductively coupled plasma
6
source, multicollector, mass spectrometry (ICP-MC-MS). The
3. Terminology
235
methodappliestomaterialwith Uabundanceintherangeof
3.1 Acronyms:
0.2 to 6 % mass. This test method is also described in ASTM
3.1.1 amu—atomic mass unit
STP 1344.
3.1.2 ICP-MC-MS—Inductively Coupled Plasma Multi-
1.2 The values stated in SI units are to be regarded as
Collector Mass Spectrometer
standard. No other units of measurement are included in this
3.1.3 ICP-MS—Inductively Coupled Plasma Mass Spec-
standard.
trometer
1.3 This standard does not purport to address all of the
3.1.4 UIRM—Uranium Isotopic Reference Material
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4.1 Samples are received either in the form of uranium
hexafluoride (UF ) or aqueous uranic solution. The UF
6 6
2. Referenced Documents
samples are hydrolysed, diluted and acidified with nitric acid.
2
2.1 ASTM Standards:
Uranic solution samples are diluted and acidified with nitric
C761 Test Methods for Chemical, Mass Spectrometric,
acid. If required, an internal reference of thorium isotopes can
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
be subsequently added to each diluted sample. As detailed in
Uranium Hexafluoride
Section 8, isotope pairs of elements other than thorium could
C787 Specification for Uranium Hexafluoride for Enrich-
be used for an internal reference.
ment
4.2 The samples are contained in polypropylene tubes that
C996 Specification for Uranium Hexafluoride Enriched to
are inserted into the auto-sampler rack of the mass spectrom-
235
Less Than 5 % U
eter. Sample details are input to the computer and the instru-
D1193 Specification for Reagent Water
ment is prepared for measurement. The automatic measuring
sequence is initiated.
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
4.3 Uranium Isotopic Reference Materials (UIRMs) are
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
used to calibrate the instrument. Each UIRM is prepared in
Test.
Current edition approved June 1, 2008. Published August 2008. Originally aqueous solution (acidified with nitric acid) and if required
approved in 2000. Last previous edition approved in 2006 as C1477 – 06. DOI:
spiked with the same internal reference as the samples. This
10.1520/C1477-08.
calibration solution is measured and a mass bias parameter is
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
3
the ASTM website. Available from ASTM Headquarters.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1477−08
238
calculatedthatisstoredandsubsequentlyimportedintoeachof solution and measuring the background U ion beam. The
4
the sample measurements to correct the measured uranium sample introduction system should be periodically disas-
238
isotopic ratios. sembled and cleaned, to minimise the background U ion
beam.
4.4 Measurements of isotopic ratios in the calibration solu-
6.4.2 A background correction is performed during the
tion and the subsequent samples are initiated by customised
measurement run by monitoring the analyte signals of the 0.3
software. The mass bias factor is computed from the measured
M nitric acid rinse solution. The background correction is
isotopic ratios in the calibration solution. This parameter is
measured prior to the mass calibration and is re-measured
then exported to correct the measured isotopic ratios of the
before each subsequent sample.
samples for mass bias. The corrected isotopic abundan
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:C1477–06 Designation: C 1477 – 08
Standard Test Method for
Isotopic Abundance Analysis of Uranium Hexafluoride and
Uranyl Nitrate Solutions by Multi-Collector, Inductively
1
Coupled Plasma-Mass Spectrometry
This standard is issued under the fixed designation C 1477; 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
234 235 236 238
1.1 This test method covers the isotopic abundance analysis of U, U, U and U in samples of hydrolysed uranium
hexafluoride (UF ) by inductively coupled plasma source, multi-collector, mass spectrometry (ICP-MC-MS). The method applies
6
235
to material with U abundance in the range of 0.2 to 6 % mass. This test method is also described in ASTM STP 1344.
1.2
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
C 761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium
Hexafluoride
C 787 Specification for Uranium Hexafluoride for Enrichment
235
C 996 Specification for Uranium Hexafluoride Enriched to Less Than 5 % U
D 1193 Specification for Reagent Water
2.2 Other Document:
3
STP 1344 Applications of Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) to Radionuclide Determinations
3. Summary of Test Method
3.1Samples are received either in the form of uranium hexafluoride (UF
Terminology
3.1 Acronyms:
3.1.1 amu—atomic mass unit
3.1.2 ICP-MC-MS—Inductively Coupled Plasma Multi-Collector Mass Spectrometer
3.1.3 ICP-MS—Inductively Coupled Plasma Mass Spectrometer
3.1.4 UIRM—Uranium Isotopic Reference Material
4. Summary of Test Method
4.1 Samples are received either in the form of uranium hexafluoride (UF ) or aqueous uranic solution. The UF samples are
6
6
hydrolysed, diluted and acidified with nitric acid. Uranic solution samples are diluted and acidified with nitric acid. Subsequently,
If required, an internal reference of thorium isotopes is can be subsequently added to each diluted sample. As detailed in Section
8, isotope pairs of elements other than thorium could be used for an internal reference.
3.2The4.2 The samples are contained in polypropylene tubes that are inserted into the auto-sampler rack of the mass
spectrometer. Sample details are input to the computer and the instrument is prepared for measurement. The automatic measuring
sequence is initiated.
34.3 Uranium Isotopic Reference Materials (UIRMs) are used to calibrate the instrument. Each UIRM is prepared in aqueous
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test
.
Current edition approved JulyJune 1, 2006.2008. PublishedAugust 2006.2008. Originally approved in 2000. Last previous edition approved in 20002006 as C 1477 – 006.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from ASTM Headquarters.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
C1477–08
solution (acidified with nitric acid) and if required spiked with the same internal reference as the samples.This calibration solution
is measured and a mass bias parameter is calculated that is stored and subsequently imported into each of the sample
4
measurements to correct the measured uranium isotopic ratios.
3.4Measurements of isotopic ratios in the calibration solution and the subsequent samples are initiated by customised software.
230 232 234 238 235 238 236 238
Usingthe Th/ Thratios(thatareacquiredsimultaneouslytothe U/ U, U/ Uand U/ Uratios)andthemassbias
parameter imported from the calibration, the mass bias factor is computed. The mass bias factor is then used to correct the
2
...
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