ASTM D3443-00(2010)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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´1
Designation:D3443 −00(Reapproved2010)
Standard Test Method for
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.
´ NOTE—Added research report information to Section 8 editorially in September 2010.
1. Scope tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
1.1 This test method covers the determination of chloride in
used, provided it is first ascertained that the reagent is of
trichlorotrifluoroethane and other halocarbons that are liquid at
sufficiently high purity to permit its use without lessening the
room temperature.
accuracy of the determination.
1.2 The values stated in SI units are to be regarded as
5.2 Purity of Water—Unless otherwise indicated, references
standard. No other units of measurement are included in this
towatershallbeunderstoodtomeanhalide-freedistilledwater.
standard.
5.3 s-Diphenylcarbazone Solution—Dissolve 0.5 g of
1.3 This standard does not purport to address all of the
s-diphenylcarbazone, in 100 mL of methanol.
safety concerns, if any, associated with its use. It is the
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.
bility of regulatory limitations prior to use.
5.5 Standard Mercuric Acetate Solution—Dilute 40 mL of
stock mercuric acetate solution, reagent 2, to 1000 mL and
2. Summary of Test Method
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
standard mercuric acetate solution to the faint purple end point.
3. Significance and Use
Then:
3.1 This test method determines ionizable chloride that can
mL NaCl 31.000
be aqueously extracted from trichlorotrifluoroethane.
5 F 5µg Cl/mL (1)
mL mercuric acetate
3.2 This test method can be used to establish production and
where
purchasing specifications.
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
volume, and mix. One millilitre of this solution contains 1.00
4.2 Erlenmeyer Flask, 125-mL.
µg of chloride ion.
5. Reagents
5.7 Stock Mercuric Acetate Solution—Dissolve 1.6 g of
5.1 Purity of Reagents—Reagent grade chemicals shall be
mercuricacetatein500mLofwatercontaining3.5mLofnitric
used in all tests. Unless otherwise indicated, it is intended that
acid. Dilute to 1000 mL and mix.
all reagents shall conform to the specifications of the Commit-
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 Metho
...