ASTM D3444-00(2020)

Standard Test Method for Total Acid Number of Trichlorotrifluoroethane

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.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Dec-2019
• ICS: 71.080.20 - Halogenated hydrocarbons
• Technical Committee: D26 - Halogenated Organic Solvents and Fire Extinguishing Agents
• Drafting Committee: D26.04 - Test Methods

Relations

• Replaces: ASTM D3444-00(2015) - Standard Test Method for Total Acid Number of Trichlorotrifluoroethane
• Effective Date: 01-Jan-2020
• Referred By: ASTM D4995-10(2020) - Standard Specification for Electronic and Degreasing Grades of 1,1,2–Trichloro 1,2,2,–Trifluoroethane Solvent
• Effective Date: 01-Jan-2020
• Referred By: ASTM D5248-04(2020) - Standard Specification for Reclaimed 1,1,2-Trichloro 1,2,2-Trifluoroethane
• Effective Date: 01-Jan-2020

Overview

ASTM D3444-00(2020): Standard Test Method for Total Acid Number of Trichlorotrifluoroethane provides an established procedure for determining the total acidity in trichlorotrifluoroethane (CFC-113) and other halocarbons that remain liquid at room temperature. This standard, developed by ASTM International, supports quality assurance and regulatory compliance in the production and purchasing of halogenated organic solvents. The test method is crucial for industries that require consistent solvent quality in manufacturing, laboratory, and environmental applications.

The procedure utilizes titration with alcoholic potassium hydroxide and phenolphthalein as an indicator, adhering strictly to SI units for accuracy and universality in reporting results.

Key Topics

• Total Acid Number Determination
  The standard describes a precise titration technique to measure the acidity present in trichlorotrifluoroethane and similar halocarbons by calculating the amount of potassium hydroxide required to neutralize acidic components.

• Reagent and Apparatus Requirements
  Only reagent-grade chemicals and halide-free distilled water are specified, ensuring high accuracy. Essential apparatus include a 2 mL buret, 250 mL Erlenmeyer flasks, and carbon dioxide absorbent tubes.

• Safety and Environmental Considerations
  While the standard provides guidance on best laboratory practices, it emphasizes the user's responsibility to address all relevant safety, health, and environmental concerns. Key hazards include the removal of skin oils by trichlorotrifluoroethane, flammability of isopropyl alcohol, and the corrosivity of potassium hydroxide.

• Quality Assurance in Production
  This test method is directly applicable for establishing production and purchasing specifications, promoting consistent solvent purity and performance for end-users.

Applications

• Quality Control in Solvent Manufacturing
  Producers of trichlorotrifluoroethane and similar halocarbons use this method to monitor and certify total acidity, ensuring their products meet industry and customer requirements.

• Purchasing and Supplier Qualification
  Companies purchasing CFC-113 or related halocarbons can specify adherence to ASTM D3444-00(2020) during procurement, guaranteeing product consistency between batches and suppliers.

• Environmental and Laboratory Analysis
  Laboratories performing assessments or compliance testing on halocarbons utilize this standard method to generate reliable, repeatable data in support of regulatory filing and internal checks.

• Standardization and Regulatory Compliance
  By following an internationally recognized test method, organizations demonstrate compliance with global standards and industry best practices, reducing risks of non-conformance in regulated sectors.

Related Standards

• ASTM D1193: Standard Specification for Reagent Water - Specifies requirements for water purity, applicable for titrations in this method.
• ASTM D2989: Standard Test Methods for Acidity-Base Number-Color of Halogenated Organic Solvents and Their Admixtures - Covers similar determinations in other halogenated solvent systems.
• ISO 9001: Quality Management Systems - Requirements - Referenced for laboratory quality assurance and process control in analytical testing.
• Globally Harmonized System of Classification and Labelling of Chemicals (GHS) - Provides chemical safety and hazard labeling guidance, referenced for reagent handling.

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By using ASTM D3444-00(2020), stakeholders in chemical manufacturing, environmental testing, and quality assurance benefit from a reliable, standardized assessment of total acid number in trichlorotrifluoroethane and related halocarbons, facilitating consistent product quality and regulatory alignment.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3444 −00 (Reapproved 2020)
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 4.2 Vinyl Tubing.
1.1 This test method covers the determination of total 4.3 Two Indicating Carbon Dioxide Absorbent Tubes, 30–50
acidity in trichlorotrifluoroethane and other halocarbons that mesh.
are liquid at room temperature.
5. Reagents
1.2 The values stated in SI units are to be regarded as
5.1 Purity of Reagents—Reagent grade chemicals shall be
standard. No other units of measurement are included in this
used in all tests. Unless otherwise indicated, it is intended that
standard.
all reagents shall conform to the specifications of the Commit-
1.3 This standard does not purport to address all of the
tee onAnalytical Reagents of theAmerican Chemical Society,
safety concerns, if any, associated with its use. It is the
where such specifications are available. Other grades may be
responsibility of the user of this standard to establish appro-
used, provided it is first ascertained that the reagent is of
priate safety, health, and environmental practices and deter-
sufficiently high purity to permit its use without lessening the
mine the applicability of regulatory limitations prior to use.
accuracy of the determination.
Specific precautionary statements are given in Section 6.
1.4 This international standard was developed in accor- 5.2 Purity of Water—Unless otherwise indicated, references
towatershallbeunderstoodtomeanhalide-freedistilledwater.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5.3 Isopropyl Alcohol.
Development of International Standards, Guides and Recom-
5.4 Phenolphthalein Indicator Solution(0.05gin100mLof
mendations issued by the World Trade Organization Technical
isopropyl alcohol).
Barriers to Trade (TBT) Committee.
5.5 Potassium Acid Phthalate, U.S. National Bureau of
2. Summary of Test Method
Standards primary standard. Dry this chemical in a 120 °C
oven for several hours prior to use. Store the dry chemical in a
2.1 The total acidity of the solvent is determined by titration
desiccator.
with standard alcoholic potassium hydroxide solution using
phenolphthalein solution as the indicator. 5.6 Potassium Hydroxide Pellets.
5.7 Potassium Hydroxide Solution in Isopropyl Alcohol
3. Significance and Use
(0.01 N)—Add approximately1gof solid KOH to approxi-
3.1 This test method determines the total acidity of trichlo-
mately 1 Lof anhydrous isopropyl alcohol ina2LErlenmeyer
rotrifluoroethane by titration with alcoholic potassium hydrox-
flask. Boil the mixture gently for 5 to 10 min, stirring to
ide using phenolphthalein for an indicator.
prevent the solids from forming a cake on the bottom. Add at
least 2 g of barium hydroxide [Ba(OH) ] and boil again gently
3.2 This test method can be used to develop production and
for 5 to 10 min. Cool to room temperature. Allow to stand for
purchasing specifications.
several hours and filter the supernatant liquid through a fine
sintered glass or porcelain filtering funnel. Avoid unnecessary
4. Apparatus
exposure to CO during filtration. Store the solution out of
4.1 Buret, 2 mLin 0.01 mLsubdivisions, self-leveling, with
contact with cork or rubber. Protect the solution from CO by
1000 mL reservoir.
Tygon has been found satisfactory. An equivalent may be used.
1 3
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 Methods. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Jan. 1, 2020. Published January 2020. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1975. Last previous edition approved in 2015 as D3444–00(2015). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D3444–00R20. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3444 − 00 (2020)
a guard tube containing carbon dioxide adsorbent. Standardize 7.4.7 Titrate the standard with the approximate 0.01 N
against pure potassium acid phthalate in about 25 mL of potassium hydroxide solution to the phenolphthalein indicator
CO -free water using phenolphthalein to detect the end point. end point. Record the titer.
8. Calculation
6. Hazards
8.1 Calculate the acid number of the s
...