ASTM D2988-96

Standard Test Methods for Water-Soluble Halide Ion In Halogenated Organic Solvents and Their Admixtures

SCOPE
1.1 Test Methods 1, 2, and 3--These test methods cover the determination of water-extractable halide ion in halogenated organic solvents and their admixtures. Fluoride ion is not measured due to the solubility of silver fluoride.
1.2 Test Method 4--This test method covers the determination of chloride ion in halogenated organic solvents and their admixtures.
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. Specific precautionary statements are given in Section 6.

General Information

• Status: Historical
• Publication Date: 31-Dec-1999
• Technical Committee: D26 - Halogenated Organic Solvents and Fire Extinguishing Agents
• Drafting Committee: D26.04 - Test Methods

Relations

• Replaced By: ASTM D2988-96(2000) - Standard Test Methods for Water-Soluble Halide Ion In Halogenated Organic Solvents and Their Admixtures
• Effective Date: 01-Jan-2000

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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: D 2988 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Methods for
Water-Soluble Halide Ion in Halogenated Organic Solvents
1
and Their Admixtures
This standard is issued under the fixed designation D 2988; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4.4 Colorimeter or Turbidimeter, Method 2.
1.1 Test Methods 1, 2, and 3—These test methods cover the
5. Reagents
determination of water-extractable halide ion in halogenated
5.1 Purity of Reagents—Reagent grade chemicals shall be
organic solvents and their admixtures. Fluoride ion is not
used in all test. Unless otherwise indicated it is intended that all
measured due to the solubility of silver fluoride.
reagents shall conform to the specifications of the Committee
1.2 Test Method 4—This test method covers the determina-
on Analytical Reagents of the American Chemical Society,
tion of chloride ion in halogenated organic solvents and their
2
where such specification are available. Other grades may be
admixtures.
used, provided it is first ascertained that the reagent is of
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the sufficiently high purity to permit its use without lessening the
accuracy of the determination.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean halide-free distilled water.
bility of regulatory limitations prior to use. Specific precau-
−
tionary statements are given in Section 6. 5.3 Chloride Standard (1 mL > 0.0001 g Cl ), Test Methods
1, 2, and 3—Prepare by adding 0.165 g of sodium chloride
2. Summary of Test Methods
(NaCl) to 1 L of halide-free distilled water.
−
5.4 Chloride Standard (1 mL 5 0.000001 g Cl ), Test
2.1 Summary of Test Methods 1, 2, 3—Halide ion present in
Method 4—Dissolve 0.0660 g of sodium chloride in water and
halogenated organic solvents is extracted with water and
dilute to 1000 mL. Pipet 25 mL of this solution into a 1000-mL
precipitated as the silver halide salt with silver nitrate. Quantity
volumetric flask, dilute to volume, and mix.
of the halide present is determined by comparing the turbidity
5.5 Nitric Acid (sg gr 1.42), concentrated nitric acid
of the sample to known standards. The distilled water, as well
(HNO ).
as all glassware used, must be halide-free.
3
5.6 Silver Nitrate Solution 0.1 N—Prepare a 0.1 N solution
2.2 Summary of Test Method 4—This test method is based
of silver nitrate (AgNO ).
on the determination of ionizable chloride by titration with
3
5.6.1 Prepare the silver nitrate solution by adding 16.99 g of
mercuric acetate solution using s-diphenylcarbazone as the
silver nitrate to a 1-L volumetric flask and fill to the line with
indicator.
halide-free distilled water. After shaking to dissolve the
3. Significance and Use
AgNO , store in an amber bottle.
3
5.7 Mercuric Acetate Solution, Test Method 4.
3.1 These test methods are used to establish manufacturing
5.7.1 Stock Mercuric Acetate Solution—Dissolve 1.6 g of
and purchasing specifications. These test methods will provide
mercuric acetate in 500 mL of water containing 3.5 mL of nitric
a means of determining the condition of the solvent in use. A
acid. Dilute to 1000 mL and mix.
high water soluble chloride level may indicate the start of
5.7.2 Standard Mercuric Acetate Solution—Dilute 40 mL of
solvent decomposition.
stock mercuric acetate solution to 1000 mL and adjust the pH
4. Apparatus
to 1.6 with nitric acid. Standardize in accordance with 7.5.5.
5.7.3 s-Diphenylcarbazone Solution (Test Method 4)—
4.1 Separatory Funnel, 500-mL,
Dissolve 0.5 g of s-diphenylcarbazone in 100 mL of methanol.
4.2 Nessler Tubes, 50-mL,
4.3 Erlenmeyer Flask, 125-mL, and
2
Reagent Chemicals, American Chemical Society Specifications, American
1
These test methods are under the jurisdiction of ASTM Committee D-26 on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct listed by the American Chemical Society, see Analar Standards for Laboratory
responsibility of Subcommittee D26.04 on Test Methods. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved Dec. 10, 1996. Published June 1997. Originally and National Formulary, U.S. P
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