ASTM C1502-09

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Designation: C1502 − 09
StandardTest 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. Summary of Test Method
1.1 This test method covers the determination of chlorine 3.1 The halogens are separated from the test materials by
and fluorine in nuclear-grade uranium dioxide (UO ) powder pyrohydrolysis in a quartz tube with a stream of wet oxygen or
2
and pellets, nuclear grade gadolinium oxide (Gd O ) powder air at a temperature of 900 to 1000°C. (1-4) Chloride and
2 3
and gadolinium oxide-uranium oxide (Gd O -UO ) powder fluoride are volatilized simultaneously as acids, absorbed in a
2 3 2
and pellets. buffer solution as chloride and fluoride and measured with ion
selective electrodes (4-6).
1.2 Witha2gramUO samplesizethedetectionlimitofthe
2
method is 4 µg/g for chlorine and 2 µg/g for fluorine. The
4. Significance and Use
maximum concentration determined with a 2 gram sample is
4.1 The method is designed to show whether or not the
500 µg/g for both chlorine and fluorine. The sample size used
tested materials meet the specifications as given in either
in this test method can vary from 1 to 10 grams resulting in a
Specification C753, C776, C888 or C922.
corresponding change in the detection limits and range.
1.3 The values stated in SI units are to be regarded as
5. Interferences
standard. No other units of measurement are included in this
5.1 The buffer controls the pH of the measured solution to
standard.
avoid hydroxide ion interference or the formation of hydrogen
1.4 This standard does not purport to address all of the
complexes with fluoride.
safety concerns, if any, associated with its use. It is the
5.2 Bromide, iodide, cyanide and sulfide, if present in the
responsibility of the user of this standard to establish appro-
condensate, interfere in the measurement of chloride with
priate safety and health practices and determine the applica-
ion-selective electrodes, but have very little effect upon the
bility of regulatory limitations prior to use.
measurement of fluoride with ion-selective electrodes.
2. Referenced Documents
5.3 As the ionic activity of the chloride and fluoride ions is
2
temperature dependent, the standard solutions and sample
2.1 ASTM Standards:
solutions should be measured at the same temperature.
C753 Specification for Nuclear-Grade, Sinterable Uranium
Dioxide Powder
6. Apparatus
C776 Specification for Sintered Uranium Dioxide Pellets
6.1 Pyrohydrolysis Equipment, the assembly of suitable
C888 Specification for Nuclear-Grade Gadolinium Oxide
equipment is shown in Fig. 1.
(Gd O ) Powder
2 3
C922 Specification for Sintered Gadolinium Oxide-Uranium
6.2 Gas Flow Regulator and Flowmeter.
Dioxide Pellets
6.3 Hot Plate, used to warm the water saturating the sparge
D1193 Specification for Reagent Water
gas to 50–80°C.
6.4 Combustion Tube Furnace, having a bore of about 32
mm with a length of about 300 mm and the capability of
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
maintaining a temperature of 950 6 25°C. Combustion tube
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
furnaces with different dimensions may be satisfactory. Tem-
CurrenteditionapprovedJune1,2009.PublishedJuly2009.Originallyapproved
peratures between 900 and 1000°C have been found to be
in 2001. Last previous edition approved in 2001 as C1502 – 01. DOI: 10.1520/
satisfactory.
C1502-09.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.5 Quartz Reaction Tube (Fig. 2)—The exit end should not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
extend more than 50 mm beyond the furnace with a ground
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. jointconnectingtothedeliverytube.Thedeliverytubeextends
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C1502 − 09
FIG. 1 Pyrohydrolysis Equipment
NOTE 1—All dimensions in millimetres.
FIG. 2 Quartz Reaction Tube
into a polyethylene or Pyrex absorption vessel with a tip 6.10 pH/mV Meter—The meter should have minimum reso-
capable of giving a stream of very fine bubbles. A second lution of 1 mV.
absorption vessel connected in series, may be necessary to
6.11 Magnetic Stirrer.
ensure complete collection of the fluorine and chlorine from
6.
...