ASTM D4755-95(2015)e1
(Test Method)Standard Test Method for Free Halogens in Halogenated Organic Solvents and Their Admixtures
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D4755 − 95 (Reapproved 2015)
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.
ε NOTE—Units statement was inserted in Section 1.2 editorially in June 2015.
1. Scope 4.3 This test method provides a means of detecting the
presence of free halogens in halogenated solvents and their
1.1 This test method covers the evaluation of free halogens
admixtures.
in halogenated organic solvents and their admixtures.
1.2 The values stated in SI units are to be regarded as
5. Interferences
standard. No other units of measurement are included in this
5.1 The following materials interfere with this test giving a
standard.
false positive: ferric ion; phosgene; iodine; oxidizing agents;
1.3 This standard does not purport to address all of the
and strong acid (catalyze atmospheric oxidation of the KI).
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
6. Apparatus
priate safety and health practices and determine the applica-
6.1 Glass-Stoppered Graduate, 25-mL.
bility of regulatory limitations prior to use.
7. Reagents
2. Referenced Documents
7.1 Purity of Reagents—Reagent grade chemicals shall be
2.1 ASTM Standards:
used in all tests. Unless otherwise indicated, it is intended that
D1193 Specification for Reagent Water
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
3. Summary of Test Method
where such specifications are available. Other grades may be
3.1 Anyfreehalogenspresentinthehalogenatedsolventare
used, provided it is first ascertained that the reagent is of
extracted with water and reacted with potassium iodide test
sufficiently high purity to permit its use without lessening the
solution containing starch indicator.Ablue color indicates that
accuracy of the determination.
presence of free halogens.
7.2 Purity of Water—Unless otherwise indicated, references
4. Significance and Use to water shall be understood to mean reagent water conforming
to Type III of Specification D1193.
4.1 Free halogens will react with any residual moisture in a
solvent to form acid. These acids can cause corrosion to 7.3 Potassium Iodide (KI) Test Solution—Dissolve 16.5 g of
process and storage equipment used for halogenated solvents.
potassium iodide in water to make 100 mL. Store in light-
resistant containers.
4.2 The presence of free halogens in halogenated solvents is
often an indication that the stabilizers in the solvent system are
7.4 Starch Test Solution—Mix1gof soluble starch with 10
breaking down.
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
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
responsibility of Subcommittee D26.04 on Test Methods.
Current edition approved June 1, 2015. Published June 2015. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1987. La
...
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.
´1
Designation: D4755 − 95 (Reapproved 2010) D4755 − 95 (Reapproved 2015)
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.
ε NOTE—Units statement was inserted in Section 1.2 editorially in June 2015.
1. 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
3. Summary of Test Method
3.1 Any free halogens present in the halogenated solvent are extracted with water and reacted with potassium iodide test
solution containing starch indicator. A blue color indicates that presence of free halogens.
4. 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.
5. Interferences
5.1 The following materials interfere with this test giving a false positive: ferric ion; phosgene; iodine; oxidizing agents; and
strong acid (catalyze atmospheric oxidation of the KI).
6. Apparatus
6.1 Glass-Stoppered Graduate, 25-mL.
7. Reagents
7.1 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
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 Feb. 1, 2010June 1, 2015. Published March 2010June 2015. Originally approved in 1987. Last previous edition approved in 20042010 as
D4755 – 95(04).(2010). DOI: 10.1520/D4755-95R10.10.1520/D4755-95R15E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4755 − 95 (2015)
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purit
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