ASTM D3444-00(2010)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3444 −00(Reapproved 2010)
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.
ε NOTE—Section 5.1 was updated in June 2010.
1. Scope 5. Reagents
1.1 This test method covers the determination of total 5.1 Purity of Reagents—Reagent grade chemicals shall be
acidity in trichlorotrifluoroethane and other halocarbons that used in all tests. Unless otherwise indicated, it is intended that
are liquid at room temperature. all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
1.2 The values stated in SI units are to be regarded as
where such specifications are available. Other grades may be
standard. No other units of measurement are included in this
used, provided it is first ascertained that the reagent is of
standard.
sufficiently high purity to permit its use without lessening the
1.3 This standard does not purport to address all of the
accuracy of the determination.
safety concerns, if any, associated with its use. It is the
5.2 Purity of Water—Unless otherwise indicated, references
responsibility of the user of this standard to establish appro-
towatershallbeunderstoodtomeanhalide-freedistilledwater.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
5.3 Isopropyl Alcohol.
tionary statements are given in Section 6.
5.4 Phenolphthalein Indicator Solution(0.05gin100mLof
isopropyl alcohol).
2. Summary of Test Method
5.5 Potassium Acid Phthalate, U.S. National Bureau of
2.1 The total acidity of the solvent is determined by titration
Standards primary standard. Dry this chemical in a 120°C oven
with standard alcoholic potassium hydroxide solution using
for several hours prior to use. Store the dry chemical in a
phenolphthalein solution as the indicator.
desiccator.
5.6 Potassium Hydroxide Pellets.
3. Significance and Use
5.7 Potassium Hydroxide Solution in Isopropyl Alcohol
3.1 This test method determines the total acidity of trichlo-
(0.01 N)—Add approximately1gof solid KOH to approxi-
rotrifluoroethane by titration with alcoholic potassium hydrox-
mately 1 Lof anhydrous isopropyl alcohol in a 2-LErlenmeyer
ide using phenolphthalein for an indicator.
flask. Boil the mixture gently for 5 to 10 min, stirring to
3.2 This test method can be used to develop production and
prevent the solids from forming a cake on the bottom. Add at
purchasing specifications.
least 2 g of barium hydroxide [Ba(OH) ] and boil again gently
for 5 to 10 min. Cool to room temperature. Allow to stand for
4. Apparatus
several hours and filter the supernatant liquid through a fine
4.1 Buret,2-mLin 0.01-mLsubdivisions, self-leveling, with
sintered glass or porcelain filtering funnel. Avoid unnecessary
1000-mL reservoir.
exposure to CO during filtration. Store the solution out of
4.2 Vinyl Tubing. contact with cork or rubber. Protect the solution from CO by
a guard tube containing carbon dioxide adsorbent. Standardize
4.3 Two Indicating Carbon Dioxide Absorbent Tubes, 30–50
against pure potassium acid phthalate in about 25 mL of
mesh.
CO -free water using phenolphthalein to detect the end point.
This test method is under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct Reagent Chemicals, American Chemical Society Specifications, American
responsibility of Subcommittee D26.04 on Test Methods. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
CurrenteditionapprovedJune1,2010.PublishedJuly2010.Originallyapproved listed by the American Chemical Society, see Analar Standards for Laboratory
in 1975. Last previous edition approved in 2005 as D3444 – 00(2005). DOI: Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
10.1520/D3444-00R10E1. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Tygon has been found satisfactory. An equivalent may be used. MD.
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D3444−00 (2010)
6. Hazards 8. Calculation
6.1 Trichlorotrifluoroethane removes natural oils from skin.
8.1 Calculate the acid number of the solvent as follows:
Avoid skin contact. The solvent is not flammable and has a
Total acid number in 1 mg of KOH/g sample
threshold limit value of 1000 ppm by volume in air. See the
5 ~A 3 N 356.1!/W (1)
manufacturer’s MSDS.
wher
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