ASTM C1502-16
(Test Method)Standard Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide
Standard Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide
SIGNIFICANCE AND USE
5.1 The method is designed to show whether or not the tested materials meet the specifications as given in either Specification C753, C776, C888 or C922.
SCOPE
1.1 This test method covers the determination of chlorine and fluorine in nuclear-grade uranium dioxide (UO2) powder and pellets, nuclear grade gadolinium oxide (Gd2O3 ) powder and gadolinium oxide-uranium oxide (Gd2O3-UO2) powder and pellets.
1.2 With a 2 gram UO2 sample size the detection limit of the method is 4 µg/g for chlorine and 2 µg/g for fluorine. The maximum concentration determined with a 2 gram sample is 500 µg/g for both chlorine and fluorine. The sample size used in this test method can vary from 1 to 10 grams resulting in a corresponding change in the detection limits and range.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 and health practices and determine the applicability of regulatory limitations prior to use.
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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: C1502 − 16
Standard Test Method for
Determination of Total Chlorine and Fluorine in Uranium
1
Dioxide and Gadolinium Oxide
This standard is issued under the fixed designation C1502; 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 test method covers the determination of chlorine 3.1 Definitions—Except as otherwise defined herein, defini-
and fluorine in nuclear-grade uranium dioxide (UO ) powder tions of terms are given in Terminology C859.
2
and pellets, nuclear grade gadolinium oxide (Gd O ) powder
2 3
3.2 Definitions of Terms Specific to This Standard:
and gadolinium oxide-uranium oxide (Gd O -UO ) powder
2 3 2
3.2.1 accelerator—a chemical compound or a flux that will
and pellets.
decrease the reaction time or prohydrolysis time.
1.2 Witha2gramUO samplesizethedetectionlimitofthe
2
4. Summary of Test Method
method is 4 µg/g for chlorine and 2 µg/g for fluorine. The
maximum concentration determined with a 2 gram sample is
4.1 The halogens are separated from the test materials by
500 µg/g for both chlorine and fluorine. The sample size used
pyrohydrolysis in a quartz reaction tube with a stream of wet
in this test method can vary from 1 to 10 grams resulting in a
oxygenorairatatemperatureof900to1000°C (1-4).Chloride
corresponding change in the detection limits and range.
and fluoride are volatilized simultaneously as acids, absorbed
inanabsorptionsolutionaschlorideandfluorideandmeasured
1.3 The values stated in SI units are to be regarded as
with ion selective electrodes (4-6).
standard. No other units of measurement are included in this
standard.
5. Significance and Use
1.4 This standard does not purport to address all of the
5.1 The method is designed to show whether or not the
safety concerns, if any, associated with its use. It is the
tested materials meet the specifications as given in either
responsibility of the user of this standard to establish appro-
Specification C753, C776, C888 or C922.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
6. Interferences
2. Referenced Documents 6.1 The absorption solution controls the pH of the measured
2
solutiontoavoidhydroxideioninterferenceortheformationof
2.1 ASTM Standards:
hydrogen complexes with fluoride.
C753 Specification for Nuclear-Grade, Sinterable Uranium
Dioxide Powder
6.2 Bromide, iodide, cyanide and sulfide, if present in the
C776 Specification for Sintered Uranium Dioxide Pellets condensate, interfere in the measurement of chloride with
C859 Terminology Relating to Nuclear Materials
ion-selective electrodes, but have very little effect upon the
C888 Specification for Nuclear-Grade Gadolinium Oxide measurement of fluoride with ion-selective electrodes.
(Gd O ) Powder
2 3
6.3 As the ionic activity of the chloride and fluoride ions is
C922 Specification for Sintered Gadolinium Oxide-Uranium
temperature dependent, the standard solutions and sample
Dioxide Pellets
solutions should be measured at the same temperature.
D1193 Specification for Reagent Water
7. Apparatus
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear 7.1 Pyrohydrolysis Equipment, the assembly of suitable
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
equipment is shown in Fig. 1.
Test.
Current edition approved Jan. 15, 2016. Published February 2016. Originally 7.2 Gas Flow Regulator and Flowmeter.
approved in 2001. Last previous edition approved in 2009 as C1502 – 09. DOI:
7.3 Hot Plate, used to warm the water saturating the sparge
10.1520/C1502-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or gas to 50 to 80°C.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7.4 Combustion Tube Furnace, having a bore of about 32
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. mm with a length of about 300 mm and the capability of
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1502 − 16
FIG. 1 Pyrohydrolysis Equipment
maintaining a temperature of 950 6 25°C. Combustion tube 7.7 Absorption Vessel, a 50-ml polyethylene graduate or
furnaces with different dimensions may be satisfactory. Tem- tube is satisfactory.
peratures between 900 and 1000°C have been found to be
7.8
...
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: C1502 − 09 C1502 − 16
Standard Test Method for
Determination of Total Chlorine and Fluorine in Uranium
1
Dioxide and Gadolinium Oxide
This standard is issued under the fixed designation C1502; 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 determination of chlorine and fluorine in nuclear-grade uranium dioxide (UO ) powder and
2
pellets, nuclear grade gadolinium oxide (Gd O ) powder and gadolinium oxide-uranium oxide (Gd O -UO ) powder and pellets.
2 3 2 3 2
1.2 With a 2 gram UO sample size the detection limit of the method is 4 μg/g for chlorine and 2 μg/g for fluorine. The maximum
2
concentration determined with a 2 gram sample is 500 μg/g for both chlorine and fluorine. The sample size used in this test method
can vary from 1 to 10 grams resulting in a corresponding change in the detection limits and range.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
C776 Specification for Sintered Uranium Dioxide Pellets
C859 Terminology Relating to Nuclear Materials
C888 Specification for Nuclear-Grade Gadolinium Oxide (Gd O ) Powder
2 3
C922 Specification for Sintered Gadolinium Oxide-Uranium Dioxide Pellets
D1193 Specification for Reagent Water
3. Terminology
3.1 Definitions—Except as otherwise defined herein, definitions of terms are given in Terminology C859.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 accelerator—a chemical compound or a flux that will decrease the reaction time or prohydrolysis time.
4. Summary of Test Method
4.1 The halogens are separated from the test materials by pyrohydrolysis in a quartz reaction tube with a stream of wet oxygen
or air at a temperature of 900 to 1000°C.1000°C (1-4)). Chloride and fluoride are volatilized simultaneously as acids, absorbed in
a bufferan absorption solution as chloride and fluoride and measured with ion selective electrodes (4-6).
5. Significance and Use
5.1 The method is designed to show whether or not the tested materials meet the specifications as given in either Specification
C753, C776, C888 or C922.
6. Interferences
6.1 The buffer absorption solution controls the pH of the measured solution to avoid hydroxide ion interference or the formation
of hydrogen complexes with fluoride.
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, 2009Jan. 15, 2016. Published July 2009February 2016. Originally approved in 2001. Last previous edition approved in 20012009 as
C1502 – 01.C1502 – 09. DOI: 10.1520/C1502-09.10.1520/C1502-16.
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 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1502 − 16
6.2 Bromide, iodide, cyanide and sulfide, if present in the condensate, interfere in the measurement of chloride with
ion-selective electrodes, but have very little effect upon the measurement of fluoride with ion-selective electrodes.
6.3 As the ionic activity of the chloride and fluoride ions is temperature dependent, the standard solutions and sample solutions
should be measured at the same temperature.
7. Apparatus
7.1 Pyrohydrolysis Equipment, the assembly of suitable equipment is shown in Fig. 1.
7.2 Gas Flow Regulator and Flowmeter.
7.3 Hot Plate, used to warm the water saturating the sparge gas to 50–80°C.50 to 80°C.
7.4 Combustion Tube Furnace, having a bore of about 32 mm with a length of about 300 mm and the capability of maintaining
a temperature of 950 6 25
...
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