ASTM D4755-95(2020)

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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