ASTM D4755-95(2004)

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

SIGNIFICANCE AND USE
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.
The presence of free halogens in halogenated solvents is often an indication that the stabilizers in the solvent system are breaking down.
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 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.

General Information

• Status: Historical
• Publication Date: 14-Mar-1995
• 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(2000) - Standard Test Method for Free Halogens in Halogenated Organic Solvents and Their Admixtures
• Effective Date: 15-Mar-1995
• Replaced By: ASTM D4755-95(2010) - Standard Test Method for Free Halogens in Halogenated Organic Solvents and Their Admixtures
• Effective Date: 01-Feb-2010
• Referred By: ASTM D7509-09(2021) - Standard Specification for Fluorocarbon Feedstock Grade Chloroform
• Effective Date: 15-Mar-1995
• Referred By: ASTM D4701-00(2020) - Standard Specification for Technical Grade Methylene Chloride
• Effective Date: 15-Mar-1995
• 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: 15-Mar-1995

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information.
Designation:D4755–95 (Reapproved 2004)
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 6. Apparatus
6.1 Glass-Stoppered Graduate, 25-mL.
1.1 This test method covers the evaluation of free halogens
in halogenated organic solvents and their admixtures.
7. Reagents
1.2 This standard does not purport to address all of the
7.1 Purity of Reagents—Reagent grade chemicals shall be
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
2. Referenced Documents
used, provided it is first ascertained that the reagent is of
2.1 ASTM Standards: sufficiently high purity to permit its use without lessening the
D1193 Specification for Reagent Water accuracy of the determination.
7.2 Purity of Water— Unless otherwise indicated, refer-
3. Summary of Test Method
ences to water shall be understood to mean reagent water
3.1 Anyfreehalogenspresentinthehalogenatedsolventare conforming to Type III of Specification D1193.
extracted with water and reacted with potassium iodide test
7.3 Potassium Iodide (KI) Test Solution—Dissolve16.5gof
solution containing starch indicator.Ablue color indicates that potassium iodide in water to make 100 mL. Store in light-
presence of free halogens.
resistant containers.
7.4 Starch Test Solution—Mix1gofsolublestarch with10
4. Significance and Use
mg of red mercuric iodide and sufficient cold water to make a
4.1 Free halogens will react with any residual moisture in a
thin paste. Add 200 mL of boiling water, and boil for 1 min
solvent to form acid. These acids can cause corrosion to
with continuous stirring. Cool, and use only the clear solution.
process and storage equipment used for halogenated solvents.
8. Procedure
4.2 The presence of free halogens in halogenated solvents is
often an indication that the stabilizers in the solvent system are 8.1 Transfer 10 mL of sample to a glass-stoppered graduate
breaking down.
and add 10 mL of potassium iodide test solution and 1 mL of
4.3 This test method provides a means of detecting the starch indicator solution. Shake vigorously for 2 min and
presence of free halogens in halogenated solvents and their
observe color of the aqueous layer. The presence of free
admixtures. halogens is indicated by a blue coloration.
NOTE 1—The potassium iodide solution can generate free iodine via air
5. Interferences
oxidation. For this reason, the test procedure should first be performed on
5.1 The following materials interfere with this test giving a
a reagent blank (10 mLof potassiu
...