ASTM D3443-00(2005)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3443 – 00 (Reapproved 2005)
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.
1. Scope where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
1.1 This test method covers the determination of chloride in
sufficiently high purity to permit its use without lessening the
trichlorotrifluoroethane and other halocarbons that are liquid at
accuracy of the determination.
room temperature.
5.2 Purity of Water—Unless otherwise indicated, references
1.2 This standard does not purport to address all of the
towatershallbeunderstoodtomeanhalide-freedistilledwater.
safety concerns, if any, associated with its use. It is the
5.3 s-Diphenylcarbazone Solution—Dissolve 0.5 g of
responsibility of the user of this standard to establish appro-
s-diphenylcarbazone, in 100 mL of methanol.
priate safety and health practices and determine the applica-
5.4 Silver Nitrate Solution—Dissolve 8.5 g of silver nitrate
bility of regulatory limitations prior to use.
(AgNO ) in 500 mL of water.
2. Summary of Test Method
5.5 Standard Mercuric Acetate Solution—Dilute 40 mL of
stock mercuric acetate solution, reagent 2, to 1000 mL and
2.1 This test method is based on the determination of
adjust the pH to 1.6 with nitric acid. Standardize as follows:
ionizable chloride by titration with mercuric acetate solution
5.5.1 Pipet 10.00 mL of standard sodium chloride solution
using s-diphenylcarbazone as the indicator.
into a 250-mL Erlenmeyer flask. Add 20 mL of chloride-free
3. Significance and Use
waterand5dropsof s-diphenylcarbazonesolution.Titratewith
standard mercuric acetate solution to the faint purple end point.
3.1 This test method determines ionizable chloride that can
Then:
be aqueously extracted from trichlorotrifluoroethane.
3.2 This test method can be used to establish production and mL NaCl 3 1.000
5 F 5 µg Cl/mL (1)
purchasing specifications. mL mercuric acetate
4. Apparatus where
F = factor for the mercuric acetate solution (see 7.1).
4.1 Separatory Funnels, two 250-mL, with polytetra-
5.6 Standard Sodium Chloride Solution—Dissolve 0.0660 g
fluoroethylene stopcocks.
of sodium chloride in water and dilute to 1000 mL. Pipet 25
4.2 Erlenmeyer Flask, 125-mL.
mL of this solution into a 1000-mL volumetric flask, dilute to
5. Reagents volume, and mix. One millilitre of this solution contains 1.00
µg of chloride ion.
5.1 Purity of Reagents—Reagent grade chemicals shall be
5.7 Stock Mercuric Acetate Solution—Dissolve 1.6 g of
used in all tests. Unless otherwise indicated, it is intended that
mercuricacetatein500mLofwatercontaining3.5mLofnitric
all reagents shall conform to the specifications of the Commit-
acid. Dilute to 1000 mL and mix.
tee onAnalytical Reagents of theAmerican Chemical Society,
6. Procedure
6.1 Wash all glassware with chloride-free water until 10 mL
of the washings show no trace of turbidity when 1 mLof silver
nitrate solution is added.
1 2
This test method is under the jurisdiction of ASTM Committee D26 on Reagent Chemicals, American Chemical Society Specifications, American
Halogenated Organic Solvent
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