ASTM D3443-00(2010)
(Test Method)Standard Test Method for Chloride in Trichlorotrifluoroethane
Standard Test Method for Chloride in Trichlorotrifluoroethane
SIGNIFICANCE AND USE
This test method determines ionizable chloride that can be aqueously extracted from trichlorotrifluoroethane.
This test method can be used to establish production and purchasing specifications.
SCOPE
1.1 This test method covers the determination of chloride in trichlorotrifluoroethane and other halocarbons that are liquid at room temperature.
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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3443 – 00 (Reapproved 2010)
Standard Test Method for
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Chloride in Trichlorotrifluoroethane
This standard is issued under the fixed designation D3443; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
1.1 This test method covers the determination of chloride in
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where such specifications are available. Other grades may be
trichlorotrifluoroethane and other halocarbons that are liquid at
used, provided it is first ascertained that the reagent is of
room temperature.
sufficiently high purity to permit its use without lessening the
1.2 The values stated in SI units are to be regarded as
accuracy of the determination.
standard. No other units of measurement are included in this
5.2 Purity of Water—Unless otherwise indicated, references
standard.
towatershallbeunderstoodtomeanhalide-freedistilledwater.
1.3 This standard does not purport to address all of the
5.3 s-Diphenylcarbazone Solution—Dissolve 0.5 g of
safety concerns, if any, associated with its use. It is the
s-diphenylcarbazone, in 100 mL of methanol.
responsibility of the user of this standard to establish appro-
5.4 Silver Nitrate Solution—Dissolve 8.5 g of silver nitrate
priate safety and health practices and determine the applica-
(AgNO ) in 500 mL of water.
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bility of regulatory limitations prior to use.
5.5 Standard Mercuric Acetate Solution—Dilute 40 mL of
2. Summary of Test Method stock mercuric acetate solution, reagent 2, to 1000 mL and
adjust the pH to 1.6 with nitric acid. Standardize as follows:
2.1 This test method is based on the determination of
5.5.1 Pipet 10.00 mL of standard sodium chloride solution
ionizable chloride by titration with mercuric acetate solution
into a 250-mL Erlenmeyer flask. Add 20 mL of chloride-free
using s-diphenylcarbazone as the indicator.
waterand5dropsof s-diphenylcarbazonesolution.Titratewith
3. Significance and Use
standard mercuric acetate solution to the faint purple end point.
Then:
3.1 This test method determines ionizable chloride that can
be aqueously extracted from trichlorotrifluoroethane.
mL NaCl 3 1.000
5 F 5 µg Cl/mL (1)
3.2 This test method can be used to establish production and mL mercuric acetate
purchasing specifications.
where
F = factor for the mercuric acetate solution (see 7.1).
4. Apparatus
5.6 Standard Sodium Chloride Solution—Dissolve 0.0660 g
4.1 Separatory Funnels, two 250-mL, with polytetra-
of sodium chloride in water and dilute to 1000 mL. Pipet 25
fluoroethylene stopcocks.
mL of this solution into a 1000-mL volumetric flask, dilute to
4.2 Erlenmeyer Flask, 125-mL.
volume, and mix. One millilitre of this solution contains 1.00
5. Reagents µg of chloride ion.
5.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
1 2
This test method is under the jurisdiction of ASTM Committee D26 on Reagent Chemicals, American Chemical Society Specifications , American
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct Chemical Society, Washington, DC. For suggestions on the testing of reagents not
responsibility of Subcommittee D26.04 on Test Methods. listed by the American Chemical Society, see Analar Standards for Laboratory
CurrenteditionapprovedJune1,2010.PublishedJuly2010.Originallyapproved Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
in 1975. Last previous edition approved in 2005 as D3443 – 00(2005). DOI: and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
10.1520/D3443-00R10. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D3443 – 00 (2010)
5.7 Stock Mercuric Acetate Solution—Dissolve 1.6 g of
where:
mercuricacetatein500mLofwatercontaining3.5mLofnitric
A = millilitres of mercuric acetate solution required for the
acid. Dilute to 1000 mL and mix.
titration,
F = factor for the solution (see 5.5.1),
6. Procedure
S = millilitres of sample, and
6.1 Wash all glassware with chloride-free water until 10 mL G = specific gravity of the sample.
of the washings show no trace of turbidity when 1 mLof silver
8. Precision and Bias
nitrate solution is added.
6.2 Transfer100mLofthesampleintoa250-mLseparatory
8.1 Repeatability (Single Analyst): The standard deviation
funnel, add 25 mL of chloride-free wate
...
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