ASTM D2988-96(2015)
(Test Method)Standard Test Methods for Water-Soluble Halide Ion in Halogenated Organic Solvents and Their Admixtures
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.
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Designation: D2988 − 96 (Reapproved 2015)
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 a means of determining the condition of the solvent in use. A
high water soluble chloride level may indicate the start of
1.1 Test Methods 1, 2, and 3—These test methods cover the
solvent decomposition.
determination of water-extractable halide ion in halogenated
organic solvents and their admixtures. Fluoride ion is not
4. Apparatus
measured due to the solubility of silver fluoride.
4.1 Separatory Funnel, 500-mL,
1.2 Test Method 4—This test method covers the determina-
4.2 Nessler Tubes, 50-mL,
tion of chloride ion in halogenated organic solvents and their
admixtures.
4.3 Erlenmeyer Flask, 125-mL, and
1.3 The values stated in SI units are to be regarded as
4.4 Colorimeter or Turbidimeter, Method 2.
standard. No other units of measurement are included in this
5. Reagents
standard.
1.4 This standard does not purport to address all of the 5.1 Purity of Reagents—Reagent grade chemicals shall be
safety concerns, if any, associated with its use. It is the usedinalltest.Unlessotherwiseindicateditisintendedthatall
responsibility of the user of this standard to establish appro- reagents shall conform to the specifications of the Committee
priate safety and health practices and determine the applica- on Analytical Reagents of the American Chemical Society,
bility of regulatory limitations prior to use. Specific precau- where such specification are available. Other grades may be
tionary statements are given in Section 6. used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
2. Summary of Test Method
accuracy of the determination.
2.1 Summary of Test Methods 1, 2, 3—Halide ion present in
5.2 Purity of Water—Unless otherwise indicated, references
halogenated organic solvents is extracted with water and
towatershallbeunderstoodtomeanhalide-freedistilledwater.
precipitatedasthesilverhalidesaltwithsilvernitrate.Quantity
−
5.3 Chloride Standard (1 mL> 0.0001 g Cl ), Test Methods
of the halide present is determined by comparing the turbidity
1, 2, and 3—Prepare by adding 0.165 g of sodium chloride
of the sample to known standards. The distilled water, as well
(NaCl) to 1 L of halide-free distilled water.
as all glassware used, must be halide-free.
−
5.4 Chloride Standard (1 mL = 0.000001 g Cl ), Test
2.2 Summary of Test Method 4—This test method is based
Method 4—Dissolve 0.0660 g of sodium chloride in water and
on the determination of ionizable chloride by titration with
diluteto1000mL.Pipet25mLofthissolutionintoa1000-mL
mercuric acetate solution using s-diphenylcarbazone as the
volumetric flask, dilute to volume, and mix.
indicator.
5.5 Nitric Acid (sg gr 1.42), concentrated nitric acid
3. Significance and Use
(HNO ).
3.1 These test methods are used to establish manufacturing
5.6 Silver Nitrate Solution 0.1 N—Prepare a 0.1 N solution
and purchasing specifications.These test methods will provide
of silver nitrate (AgNO ).
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 June 1, 2015. Published June 2015. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1971. Last previous edition approved in 2010 as D2988–96(2010). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D2988-96R15. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2988 − 96 (2015)
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 to a 1-L 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.
7.2 Test Method 1A—The accuracy ofTest Method 1 can be
5.7 Mercuric Acetate Solution, Test Method 4.
improved for samples with chloride levels less than 2 ppm by
5.7.1 Stock Mercuric Acetate Solution—Dissolve 1.6 g of
increasing the solvent-water ratio from 1:1 to 4:1.
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.
5.7.3 s-Diphenylcarbazone Solution (Test Method 4)— 7.4 Test Method 3—Extract the sample as described in Test
Dissolve 0.5 g of s-diphenylcarbazone in 100 mLof methanol. Method 1. Analyze the water extract with an ion chromato-
graphthathasbeencalibratedwithstandardsintheappropriate
6. Hazards
ranges. This test method gives superior data over turbidity
methods.
6.1 Solvent Hazards—Contact with the skin should be
avoided to prevent removal of natural oils. There are varying
7.5 Test Method 4:
degrees of danger to inhalation, ingestion, and contact. The 7.5.1 Wash all glassware with chloride-free water until 10
usershouldrefertothemostrecenthealthregulationsconcern-
mL of the washings show no trace of turbidity when 1 mL of
ing the individual solvent. silver nitrate solution is added.
7.5.2 Transfer 100 mL of the sample into a 250-mL sepa-
6.
...
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.
Designation: D2988 − 96 (Reapproved 2010) D2988 − 96 (Reapproved 2015)
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. A number 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
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Section 6.
2. Summary of Test Methods Method
2.1 Summary of Test Methods 1, 2, 3—Halide ion present in halogenated organic solvents is extracted with water and
precipitated as the silver halide salt with silver nitrate. Quantity of the halide present is determined by comparing the turbidity of
the sample to known standards. The distilled water, as well as all glassware used, must be halide-free.
2.2 Summary of Test Method 4—This test method is based on the determination of ionizable chloride by titration with mercuric
acetate solution using s-diphenylcarbazone as the indicator.
3. 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.
4. Apparatus
4.1 Separatory Funnel, 500-mL,
4.2 Nessler Tubes, 50-mL,
4.3 Erlenmeyer Flask, 125-mL, and
4.4 Colorimeter or Turbidimeter, Method 2.
5. Reagents
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all test. 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
such specification are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
These test methods are under the jurisdiction of ASTM Committee D26 on Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct responsibility
of Subcommittee D26.04 on Test Methods.
Current edition approved June 1, 2010June 1, 2015. Published July 2010June 2015. Originally approved in 1971. Last previous edition approved in 20052010 as
D2988 – 96(2005).(2010). DOI: 10.1520/D2988-96R10.10.1520/D2988-96R15.
Reagent Chemicals, American Chemical Society Specifications, , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2988 − 96 (2015)
5.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean halide-free distilled water.
−
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 (NaCl)
to 1 L of halide-free distilled water.
−
5.4 Chloride Standard (1 mL = 0.000001 g Cl ), Test Method 4—Dissolve 0.0660 g of sodium chloride in water and dilute to
1000 mL. Pipet 25 mL of this solution into a 1000-mL volumetric flask, dilute to volume, and mix.
5.5 Nitric Acid (sg gr 1.42), concentrated nitric acid (HNO ).
5.6 Silver Nitrate Solution 0.1 N—Prepare a 0.1 N solution of silver nitrate (AgNO ).
5.6.1 Prepare the silver nitrate solution by adding 16.99 g of silver nitrate to a 1-L volumetric flask and fill to the line with
halide-free distilled water. After shaking to dissolve the AgNO , store in an amber bottle.
5.7 Mercuric Acetate Solution, Test Method 4.
5.7.1 Stock Mercuric Acetate Solution—Dissolve 1.6 g of mercuric acetate in 500 mL of water containing 3.5 mL of nitric acid.
Dilute to 1000 mL and mix.
5.7.2 Standard Mercuric Acetate Solution—Dilute 40 mL of stock mercuric acetate solution to 1000 mL and adjust the pH to
1.6 with nitric acid. Standardize in accordance with 7.5.5.
5.7.3 s-Diphenylcarbazone Solution (Test Method 4)—Dissolve 0.5 g of s-diphenylcarbazone in 100 mL of methanol.
6. Hazards
6.1 Solvent Hazards—Contact with the skin should be avoided to prevent removal of natural oils. There are varying degrees of
danger to inhalation, ingestion, and contact. The user should refer to the most recent health regulations concerning the individual
solvent.
6.2 Concentrated nitric acid is very hazardous in contact with the skin or eyes. The vapors are very toxic and corrosive.
6.3 Warning(Warning—Wear safety glasses and rubber gloves when handling the silver nitrate or its solution.—Wear safety
glasses and rubber gloves when handling the silver nitrate or its solution.)
6.4 Mercuric acetate is toxic.
6.5 The hazards of s-diphenylcarbazone are not known.
7. Procedure
7.1 Test Method 1:
7.1.1 Transfer 100 mL of sample to a separatory funnel and add an equal volume of halide-free distilled water. Shake vigorously
for 2 min to extract the water-soluble halides (see Note 1).
7.1.2 Allow the liquids to separate and discard the solvent layer. Transfer 50 mL of the water extract into a 50-mL Nessler tube
and add ten drops of concentrated nitric acid. Prepare standard chloride ion solutions in 50-mL Nessler tubes by adding a volume
of standard chloride solution, in millilitres, equal to the density of the solvent being tested divided by two for each part per million
(ppm) of equivalent chloride ion desired (see Note 2). Dilute each standard with halide-free distilled water to 50 mL and add ten
drops of concentrated nitric acid. Finally, add 1 mL of 0.1 N silver nitrate solution to each sample
...
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