ASTM C1771-13
(Test Method)Standard Test Method for Determination of Boron, Silicon, and Technetium in Hydrolyzed Uranium Hexafluoride by Inductively Coupled Plasma—Mass Spectrometer After Removal of Uranium by Solid Phase Extraction
Standard Test Method for Determination of Boron, Silicon, and Technetium in Hydrolyzed Uranium Hexafluoride by Inductively Coupled Plasma—Mass Spectrometer After Removal of Uranium by Solid Phase Extraction
SIGNIFICANCE AND USE
5.1 This method is capable of measuring the concentration of boron, silicon and technetium in UF6. Limits for these contaminants are set in Specifications C787 and C996.
SCOPE
1.1 This test method covers the determination of boron, silicon and technetium in hydrolyzed uranium hexafluoride (UF6) by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) after separation of the uranium by solid phase extraction.
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. Some specific hazards statements are given in Section 7 on Hazards.
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Designation:C1771 −13
Standard Test Method for
Determination of Boron, Silicon, and Technetium in
Hydrolyzed Uranium Hexafluoride by Inductively Coupled
Plasma—Mass Spectrometer After Removal of Uranium by
1
Solid Phase Extraction
This standard is issued under the fixed designation C1771; 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 3.2 Definitions:
3.2.1 internal reference solution, n—a solution containing
1.1 This test method covers the determination of boron,
non-analyte elements, the signal from which is used to correct
silicon and technetium in hydrolyzed uranium hexafluoride
for variation in the performance of a measuring instrument
(UF ) by Inductively Coupled Plasma Mass Spectrometry
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through the course of analyzing a batch of samples, thereby
(ICP-MS) after separation of the uranium by solid phase
improving precision.
extraction.
3.2.2 method blank, n—a solution which in so far as is
1.2 The values stated in SI units are to be regarded as
practical duplicates the sample to be analyzed and passes
standard. No other units of measurement are included in this
through the same measurement process but does not initially
standard.
contain significant quantities of any of the analytes to be
1.3 This standard does not purport to address all of the
measured.
safety concerns, if any, associated with its use. It is the
3.2.2.1 Discussion—The method blank does not initially
responsibility of the user of this standard to establish appro-
contain significant quantities of analyte, hence the value of any
priate safety and health practices and determine the applica-
analyte measured may be assumed to be due to interference,
bility of regulatory limitations prior to use. Some specific
matrix effects or contamination introduced as a consequence of
hazards statements are given in Section 7 on Hazards.
sample processing, The contribution of such factors to the
value measured on the genuine sample may therefore be
2. Referenced Documents
eliminated by subtracting the measured value for the method
2
2.1 ASTM Standards:
blank,typicallyprovidingabetterestimateforthetruevalueof
C787 Specification for Uranium Hexafluoride for Enrich-
the quantity of analyte in the sample.
ment
3.2.3 recovery correction, n—a factor applied to the mea-
C859 Terminology Relating to Nuclear Materials
sured value of the analyte in the sample to account for losses
C996 Specification for Uranium Hexafluoride Enriched to
of analyte during sample processing.
235
Less Than 5 % U
3.2.3.1 Discussion—Some of the analyte originally present
C1346 Practice for Dissolution of UF from P-10 Tubes
6
in a sample is likely to be lost during the process of preparing
C1689 Practice for Subsampling of Uranium Hexafluoride
the sample for instrumental measurement, so that the measured
D1193 Specification for Reagent Water
value will typically be subject to negative bias. The proportion
of analyte lost may be estimated by repeated measurement of
3. Terminology
a sample containing a known quantity of the analyte and a
3.1 Definitions—For definitions of other standard terms in
correction factor introduced to account for losses. Recovery
this test method, refer to Terminology C859.
correction is only required when analyte losses are significant
when compared with overall measurement uncertainty.
1
3.2.4 spike, n—a known quantity of analyte added to a
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
sample.
Test.
Current edition approved Jan. 1, 2013. Published February 2013. DOI: 10.1520/
4. Summary of Test Method
C1771-13
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 A4 % by weight solution of UF is initially prepared by
6
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
reacting a quantity of UF with water. Sub-sampling of UF
Standards volume information, refer to the standard’s Document Summary page on 6 6
the ASTM website. may be carried out as described in Practice C1689. Preparation
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C1771−13
NOTE 4—PFAcontainers may be used as an alternative and may help to
of the hydrolyzed solution may be carried out as described in
reduce silicon background levels.
Practice C1346. The laboratory may choose to adopt a simpli-
fied version of the standard practices, or to adopt other
7.1.7 Polyfluoroalkoxy fluorocarbon plastic (PFA) bottles,
p
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