ASTM D3444-00(2015)

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
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Designation: D3444 − 00 (Reapproved 2010) D3444 − 00 (Reapproved 2015)
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
1.1 This test method covers the determination of total acidity 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. Specific precautionary statements are given in Section 6.
2. Summary of Test Method
2.1 The total acidity of the solvent is determined by titration with standard alcoholic potassium hydroxide solution using
phenolphthalein solution as the indicator.
3. Significance and Use
3.1 This test method determines the total acidity of trichlorotrifluoroethane by titration with alcoholic potassium hydroxide
using phenolphthalein for an indicator.
3.2 This test method can be used to develop production and purchasing specifications.
4. Apparatus
4.1 Buret, 2-mL in 0.01-mL subdivisions, self-leveling, with 1000-mL reservoir.
4.2 Vinyl Tubing.
4.3 Two Indicating Carbon Dioxide Absorbent Tubes, 30–50 mesh.
5. Reagents
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
5.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean halide-free distilled water.
5.3 Isopropyl Alcohol.
5.4 Phenolphthalein Indicator Solution (0.05 g in 100 mL of isopropyl alcohol).
5.5 Potassium Acid Phthalate, U.S. National Bureau of Standards primary standard. Dry this chemical in a 120°C oven for
several hours prior to use. Store the dry chemical in a desiccator.
This test method is under the jurisdiction of ASTM Committee D26 on Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct responsibility of
Subcommittee D26.04 on Test Methods.
Current edition approved June 1, 2010June 1, 2015. Published July 2010June 2015. Originally approved in 1975. Last previous edition approved in 20052010 as
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D3444 – 00(2005).(2010) . DOI: 10.1520/D3444-00R10E1.10.1520/D3444-00R15.
Tygon has been found satisfactory. An equivalent may be used.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3444 − 00 (2015)
5.6 Potassium Hydroxide Pellets.
5.7 Potassium Hydroxide Solution in Isopropyl Alcohol (0.01N)—Add approximately 1 g of solid KOH to approximately 1 L
of anhydrous isopropyl alcohol in a 2-L Erlenmeyer flask. Boil the mixture gently for 5 to 10 min, stirring to prevent the solids
from forming a cake on the bottom. Add at 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 several hours and filter the supernatant liquid through a fine sintered glass or porcelain
filtering funnel. Avoid unnecessary exposure to CO during filtration. Store the solution out of contact with cork or rubber. Protect
the solution from CO by a guard tube containing carbon dioxide adsorbent. Standardize against pure potassium acid phthalate in
about 25 mL of CO -free water using phenolphthalein to detect the end point.
6. Hazards
6.1 Trichlorotrifluoroethane removes natural oils from skin. Avoid skin contact. The solvent is not flammable and has a
threshold limit value of 1000 ppm by volume in air. See the manufacturer’s MSDS.
6.2 Isopropyl alcohol is flammable, and has a threshold
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