ASTM D3444-00(2005)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3444 – 00 (Reapproved 2005)
Standard Test Method for
Total Acid Number of Trichlorotrifluoroethane
This standard is issued under the fixed designation D3444; 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 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 total
sufficiently high purity to permit its use without lessening the
acidity in trichlorotrifluoroethane and other halocarbons that
accuracy of the determination.
are liquid at 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 Isopropyl Alcohol.
responsibility of the user of this standard to establish appro-
5.4 Phenolphthalein Indicator Solution (0.05 g in 100 mL
priate safety and health practices and determine the applica-
of isopropyl alcohol).
bility of regulatory limitations prior to use. Specific precau-
5.5 Potassium Acid Phthalate, U.S. National Bureau of
tionary statements are given in Section 6.
Standards primary standard. Dry this chemical in a 120°C oven
2. Summary of Test Method for several hours prior to use. Store the dry chemical in a
desiccator.
2.1 The total acidity of the solvent is determined by titration
5.6 Potassium Hydroxide Pellets.
with standard alcoholic potassium hydroxide solution using
5.7 Potassium Hydroxide Solution in Isopropyl Alcohol
phenolphthalein solution as the indicator.
(0.01 N)—Add approximately1gof solid KOH to approxi-
3. Significance and Use
mately 1 Lof anhydrous isopropyl alcohol in a 2-LErlenmeyer
flask. Boil the mixture gently for 5 to 10 min, stirring to
3.1 This test method determines the total acidity of trichlo-
prevent the solids from forming a cake on the bottom. Add at
rotrifluoroethane by titration with alcoholic potassium hydrox-
least 2 g of barium hydroxide [Ba(OH) ] and boil again gently
ide using phenolphthalein for an indicator. 2
for 5 to 10 min. Cool to room temperature. Allow to stand for
3.2 This test method can be used to develop production and
several hours and filter the supernatant liquid through a fine
purchasing specifications.
sintered glass or porcelain filtering funnel. Avoid unnecessary
4. Apparatus
exposure to CO during filtration. Store the solution out of
contact with cork or rubber. Protect the solution from CO by
4.1 Buret, 2-mLin 0.01-mLsubdivisions, self-leveling, with
a guard tube containing Ascarite II. Standardize against pure
1000-mL reservoir.
potassium acid phthalate in about 25 mL of CO -free water
4.2 Vinyl Tubing.
using phenolphthalein to detect the end point.
4.3 Two Indicating Carbon Dioxide Absorbent Tubes, 30–50
mesh.
6. Hazards
5. Reagents
6.1 Trichlorotrifluoroethane removes natural oils from skin.
Avoid skin contact. The solvent is not flammable and has a
5.1 Purity of Reagents—Reagent grade chemicals shall be
threshold limit value of 1000 ppm by volume in air. See the
used in all tests. Unless otherwise indicated, it is intended that
manufacturer’s MSDS.
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chem-ical Society,
Reagent Chemicals, American Chemical Society Specifications, American
This test method is under the jurisdiction of ASTM Committee D26 on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct listed by the American Chemical Society, see Analar Standards for Laboratory
responsibility of Subcommittee D26.04 on Test Methods. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved June 1, 2005. Published June 2005. Originally and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
approved in 1975. Last previous edition approved in 2000 as D3444 – 00. DOI: MD.
10.1520/D3444-00R05. Ascarite II has been found satisfactory and is available from chemical supply
Tygon has been found satisfactory. An equivalent may be used. houses.
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D3444 – 00 (2005)
6.2 Isopropyl alcohol is flammable, and has a threshold 8. Calculation
limit value of 400 ppm by volume in air. See the manufactur-
8.1 Calcu
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