ASTM D2988-96(2020)

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

SIGNIFICANCE AND USE
3.1 These test methods are used to establish manufacturing and purchasing specifications. These test methods will provide a means of determining the condition of the solvent in use. A high water soluble chloride level may indicate the start of solvent decomposition.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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. Specific precautionary statements are given in Section 6.  
1.5 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 D2988-96(2015) - Standard Test Methods for Water-Soluble Halide Ion in Halogenated Organic Solvents and Their Admixtures
• Effective Date: 01-Apr-2020
• Referred By: ASTM D5396-04(2020) - Standard Specification for Reclaimed Perchloroethylene
• Effective Date: 01-Apr-2020
• Referred By: ASTM D4376-15(2020) - Standard Specification for Vapor-Degreasing Grade Perchloroethylene
• Effective Date: 01-Apr-2020
• Referred By: ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants
• Effective Date: 01-Apr-2020
• Referred By: ASTM D5395-03(2023) - Standard Specification for Reclaimed Methylene Chloride
• Effective Date: 01-Apr-2020
• Referred By: ASTM D4080-15(2020) - Standard Specification for Trichloroethylene, Technical and Vapor-Degreasing Grade
• Effective Date: 01-Apr-2020

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: D2988 − 96 (Reapproved 2020)
Standard Test Methods for
Water-Soluble Halide Ion in Halogenated Organic Solvents
and Their Admixtures
This standard is issued under the fixed designation D2988; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 2.2 Summary of Test Method 4—This test method is based
on the determination of ionizable chloride by titration with
1.1 Test Methods 1, 2, and 3—These test methods cover the
mercuric acetate solution using s-diphenylcarbazone as the
determination of water-extractable halide ion in halogenated
indicator.
organic solvents and their admixtures. Fluoride ion is not
measured due to the solubility of silver fluoride.
3. Significance and Use
1.2 Test Method 4—This test method covers the determina-
3.1 These test methods are used to establish manufacturing
tion of chloride ion in halogenated organic solvents and their
and purchasing specifications.These test methods will provide
admixtures.
a means of determining the condition of the solvent in use. A
high water soluble chloride level may indicate the start of
1.3 The values stated in SI units are to be regarded as
solvent decomposition.
standard. No other units of measurement are included in this
standard.
4. Apparatus
1.4 This standard does not purport to address all of the
4.1 Separatory Funnel, 500 mL,
safety concerns, if any, associated with its use. It is the
4.2 Nessler Tubes, 50 mL,
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 4.3 Erlenmeyer Flask, 125 mL, and
mine the applicability of regulatory limitations prior to use.
4.4 Colorimeter or Turbidimeter, Method 2.
Specific precautionary statements are given in Section 6.
1.5 This international standard was developed in accor-
5. Reagents
dance with internationally recognized principles on standard-
5.1 Purity of Reagents—Reagent grade chemicals shall be
ization established in the Decision on Principles for the
usedinalltest.Unlessotherwiseindicateditisintendedthatall
Development of International Standards, Guides and Recom-
reagents shall conform to the specifications of the Committee
mendations issued by the World Trade Organization Technical
on Analytical Reagents of the American Chemical Society,
Barriers to Trade (TBT) Committee.
where such specification are available. Other grades may be
used, provided it is first ascertained that the reagent is of
2. Summary of Test Method
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
2.1 Summary of Test Methods 1, 2, 3—Halide ion present in
halogenated organic solvents is extracted with water and 5.2 Purity of Water—Unless otherwise indicated, references
precipitatedasthesilverhalidesaltwithsilvernitrate.Quantity towatershallbeunderstoodtomeanhalide-freedistilledwater.
−
of the halide present is determined by comparing the turbidity
5.3 Chloride Standard (1 mL> 0.0001 g Cl ), Test Methods
of the sample to known standards. The distilled water, as well
1, 2, and 3—Prepare by adding 0.165 g of sodium chloride
as all glassware used, must be halide-free.
(NaCl) to 1 L of halide-free distilled water.
1 2
These test methods are under the jurisdiction of ASTM Committee D26 on Reagent Chemicals, American Chemical Society Specifications, American
Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct Chemical Society, Washington, DC. For suggestions on the testing of reagents not
responsibility of Subcommittee D26.04 on Test Methods. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved April 1, 2020. Published April 2020. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1971. Last previous edition approved in 2015 as D2988–96(2015). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D2988–96R20. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2988 − 96 (2020)
−
mately2mintoreactcompletely.Excessivetime,however,canpermitthe
5.4 Chloride Standard (1 mL = 0.000001 g Cl ), Test
halogenated solvent itself to hydrolyze.
Method 4—Dissolve 0.0660 g of sodium chloride in water and
NOTE 2—For example, if trichloroethylene were being tested, 1.46/2 or
diluteto1000mL.Pipet25mLofthissolutionintoa1000mL
0.73 mL of standard chloride solution would be needed for each part per
volumetric flask, dilute to volume, and mix.
million (ppm) of chloride ion desired. For 2 ppm, 0.73×2=1.5 mL
would be added. Since the water-soluble halides are usually less than 1
5.5 Nitric Acid (sg gr 1.42), concentrated nitric acid
ppm, it will seldom be necessary to prepare more than one or two
(HNO ).
standards.
NOTE 3—The standards and samples should be prepared simultane-
5.6 Silver Nitrate Solution 0.1 N—Prepare a 0.1 N solution
ously.Tominimizeeffectsofentrainedairandchangingcharacterofsilver
of silver nitrate (AgNO ).
chloride turbidity, let the samples set for 15 min in the dark. This waiting
5.6.1 Preparethesilvernitratesolutionbyadding16.99gof
period is especially important when low chlorides (less than 1 ppm) are
silver nitrate toa1L volumetric flask and fill to the line with
being determined. Dark storage prevents change in the silver nitrate
halide-free distilled water. After shaking to dissolve the concentration.
AgNO , store in an amber bottle.
3 7.2 Test Method 1A—The accuracy ofTest Method 1 can be
improved for samples with chloride levels less than 2 ppm by
5.7 Mercuric Acetate Solution, Test Method 4.
increasing the solvent-water ratio from 1:1 to 4:1.
5.7.1 Stock Mercuric Acetate Solution—Dissolve 1.6 g of
mercuricacetatein500mLofwatercontaining3.5mLofnitric
7.3 Test Method 2—Readtheturbidityofstandardsprepared
acid. Dilute to 1000 mL and mix.
as described in Test Methods 1 and 1A using a colorimeter or
5.7.2 Standard Mercuric Acetate Solution—Dilute40mLof
a turbidimeter. Set up a graph to determine chloride levels in
stock mercuric acetate solution to 1000 mL and adjust the pH
samples.
to 1.6 with nitric acid. Standardize in accordance with 7.5.5.
7.4 Test Metho
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