ASTM D4755-95(2020)

Standard Test Method for Free Halogens in Halogenated Organic Solvents and Their Admixtures

SIGNIFICANCE AND USE
4.1 Free halogens will react with any residual moisture in a solvent to form acid. These acids can cause corrosion to process and storage equipment used for halogenated solvents.  
4.2 The presence of free halogens in halogenated solvents is often an indication that the stabilizers in the solvent system are breaking down.  
4.3 This test method provides a means of detecting the presence of free halogens in halogenated solvents and their admixtures.
SCOPE
1.1 This test method covers the evaluation of free halogens in halogenated organic solvents and their admixtures.  
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.  
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-Mar-2020
• 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 D4755-95(2015)e1 - Standard Test Method for Free Halogens in Halogenated Organic Solvents and Their Admixtures
• Effective Date: 01-Apr-2020
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Referred By: ASTM D7509-09(2021) - Standard Specification for Fluorocarbon Feedstock Grade Chloroform
• Effective Date: 01-Apr-2020
• Referred By: ASTM D6368-06(2023) - Standard Specification for Vapor-Degreasing Solvents Based on <emph type="bdit">normal</emph >-Propyl Bromide and Technical Grade <emph type="bdit">normal</emph >-Propyl Bromide
• Effective Date: 01-Apr-2020
• Referred By: ASTM D4701-00(2020) - Standard Specification for Technical Grade Methylene Chloride
• Effective Date: 01-Apr-2020

Overview

ASTM D4755-95(2020), titled Standard Test Method for Free Halogens in Halogenated Organic Solvents and Their Admixtures, is a widely recognized standard developed by ASTM International. This test method provides a reliable procedure for evaluating the presence of free halogens in halogenated organic solvents and their mixtures. The determination of free halogens is important for ensuring the quality and stability of solvents used in industrial, laboratory, and manufacturing processes.

Assessing free halogens helps detect potential breakdowns in solvent stabilizers and prevents acid formation, which can cause corrosion in storage and processing equipment. The method, developed in line with the World Trade Organization’s international standardization principles, is a pass/fail qualitative test designed to enhance solvent safety and reliability.

Key Topics

• Purpose: Detect free halogens in halogenated solvents and their admixtures.
• Significance:
  • Free halogens can react with moisture to form acids, imparting corrosive properties to solvents.
  • Presence of free halogens may indicate the breakdown of stabilizing additives.
• Test Method: Employs a qualitative approach where halogens are extracted with water and tested using potassium iodide and starch indicator; a blue color indicates free halogens.
• Limitations:
  • Designed as a presence/absence test and does not quantify the concentration of free halogens.
  • Detection may be influenced by interfering substances such as ferric ion, phosgene, iodine, oxidizing agents, and strong acids.
• Reporting: Results are recorded as positive or negative for the presence of free halogens.

Applications

ASTM D4755-95(2020) is valuable for a wide range of industries that rely on halogenated organic solvents. Its main applications include:

• Quality Control in Manufacturing: Ensures solvents used in the production of chemicals, pharmaceuticals, coatings, and electronics do not contain corrosive contaminants that could affect final product quality or process equipment.
• Laboratory Testing: Used by quality assurance labs to verify solvent stability and detect degradation, particularly for solvents stored over extended periods.
• Maintenance of Storage and Process Equipment: Protects storage tanks, pipes, and process lines from acid corrosion by ensuring solvent purity.
• Environmental and Regulatory Compliance: Helps organizations comply with regulatory standards and best practices for safe chemical handling and use.
• Solvent Lifecycle Management: Assists in determining whether halogenated solvents can continue to be used safely or require replacement due to stabilizer breakdown.

Related Standards

Several other standards provide related guidance for solvent analysis and laboratory practices. Key references include:

• ASTM D1193 - Specification for Reagent Water: Details purity requirements for water used in analytical procedures, including this test method.
• General ASTM Solvent and Reagent Standards: Standards developed by ASTM Committee D26 on Halogenated Organic Solvents and Fire Extinguishing Agents.
• International Guidance: The standard aligns with the World Trade Organization’s Technical Barriers to Trade (TBT) Committee's principles for developing globally recognized methods.

For organizations seeking comprehensive solvent testing and quality assurance, referencing ASTM D4755-95(2020) and its related standards is essential for maintaining process safety, product quality, and regulatory compliance in chemical and manufacturing environments.

Keywords: free halogens, halogenated organic solvent, ASTM D4755, solvent quality, solvent corrosion, laboratory testing, stabilizer breakdown, international standards, halogen test method

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: D4755 − 95 (Reapproved 2020)
Standard Test Method for
Free Halogens in Halogenated Organic Solvents and Their
Admixtures
This standard is issued under the fixed designation D4755; 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 The presence of free halogens in halogenated solvents is
often an indication that the stabilizers in the solvent system are
1.1 This test method covers the evaluation of free halogens
breaking down.
in halogenated organic solvents and their admixtures.
4.3 This test method provides a means of detecting the
1.2 The values stated in SI units are to be regarded as
presence of free halogens in halogenated solvents and their
standard. No other units of measurement are included in this
admixtures.
standard.
1.3 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
5.1 The following materials interfere with this test giving a
responsibility of the user of this standard to establish appro-
false positive: ferric ion; phosgene; iodine; oxidizing agents;
priate safety, health, and environmental practices and deter-
and strong acid (catalyze atmospheric oxidation of the KI).
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
6. Apparatus
dance with internationally recognized principles on standard-
6.1 Glass-Stoppered Graduate, 25 mL.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
7. Reagents
mendations issued by the World Trade Organization Technical
7.1 Purity of Reagents—Reagent grade chemicals shall be
Barriers to Trade (TBT) Committee.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
2. Referenced Documents
2 tee onAnalytical Reagents of theAmerican Chemical Society,
2.1 ASTM Standards:
where such specifications are available. Other grades may be
D1193 Specification for Reagent Water
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
3. Summary of Test Method
accuracy of the determination.
3.1 Anyfreehalogenspresentinthehalogenatedsolventare
7.2 Purity of Water—Unless otherwise indicated, references
extracted with water and reacted with potassium iodide test
to water shall be understood to mean reagent water conforming
solution containing starch indicator.Ablue color indicates that
to Type III of Specification D1193.
presence of free halogens.
7.3 Potassium Iodide (KI) Test Solution—Dissolve 16.5 g of
4. Significance and Use
potassium iodide in water to make 100 mL. Store in light-
4.1 Free halogens will react with any residual moisture in a resistant containers.
solvent to form acid. These acids can cause corrosion to
7.4 Starch Test Solution—Mix1gof soluble starch with 10
process and storage equipment used for halogenated solvents.
mg of red mercuric iodide and sufficient cold water to make a
thin paste. Add 200 mL of boiling water, and boil for 1 min
1 with continuous stirring. Cool, and use only the clear solution.
This test method is under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct
respon
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