ASTM D2988-96(2005)
(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
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 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 2005)
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 Department of Defense.
1. Scope 4. Apparatus
1.1 Test Methods 1, 2, and 3—These test methods cover the 4.1 Separatory Funnel, 500-mL,
determination of water-extractable halide ion in halogenated 4.2 Nessler Tubes, 50-mL,
organic solvents and their admixtures. Fluoride ion is not 4.3 Erlenmeyer Flask, 125-mL, and
measured due to the solubility of silver fluoride. 4.4 Colorimeter or Turbidimeter, Method 2.
1.2 Test Method 4—This test method covers the determina-
5. Reagents
tion of chloride ion in halogenated organic solvents and their
admixtures. 5.1 Purity of Reagents—Reagent grade chemicals shall be
usedinalltest.Unlessotherwiseindicateditisintendedthatall
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the reagents shall conform to the specifications of the Committee
on Analytical Reagents of the American Chemical Society,
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- where such specification are available. Other grades may be
used, provided it is first ascertained that the reagent is of
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Section 6. sufficiently high purity to permit its use without lessening the
accuracy of the determination.
2. Summary of Test Methods
5.2 Purity of Water—Unlessotherwiseindicated,references
2.1 Summary of Test Methods 1, 2, 3—Halideionpresentin towatershallbeunderstoodtomeanhalide-freedistilledwater.
−
halogenated organic solvents is extracted with water and 5.3 Chloride Standard (1 mL> 0.0001 g Cl ), Test Methods
precipitatedasthesilverhalidesaltwithsilvernitrate.Quantity 1, 2, and 3—Prepare by adding 0.165 g of sodium chloride
of the halide present is determined by comparing the turbidity (NaCl) to 1 L of halide-free distilled water.
−
of the sample to known standards. The distilled water, as well 5.4 Chloride Standard (1 mL = 0.000001 g Cl ), Test
as all glassware used, must be halide-free. Method 4—Dissolve 0.0660 g of sodium chloride in water and
2.2 Summary of Test Method 4—This test method is based diluteto1000mL.Pipet25mLofthissolutionintoa1000-mL
on the determination of ionizable chloride by titration with volumetric flask, dilute to volume, and mix.
mercuric acetate solution using s-diphenylcarbazone as the 5.5 Nitric Acid (sg gr 1.42), concentrated nitric acid
indicator. (HNO ).
5.6 Silver Nitrate Solution 0.1 N—Prepare a 0.1 N solution
3. Significance and Use
of silver nitrate (AgNO ).
3.1 These test methods are used to establish manufacturing
5.6.1 Preparethesilvernitratesolutionbyadding16.99gof
and purchasing specifications.These test methods will provide silver nitrate to a 1-L volumetric flask and fill to the line with
a means of determining the condition of the solvent in use. A
halide-free distilled water. After shaking to dissolve the
high water soluble chloride level may indicate the start of AgNO , store in an amber bottle.
solvent decomposition.
5.7 Mercuric Acetate Solution, Test Method 4.
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, 2005. Published June 2005. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1971. Last previous edition approved in 2000 as D2988–96(00). DOI: and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
10.1520/D2988-96R05. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2988–96 (2005)
5.7.1 Stock Mercuric Acetate Solution—Dissolve 1.6 g of 7.3 TestMethod2—Readtheturbidityofstandardsprepared
mercuricacetatein500mLofwatercontaining3.5mLofnitric as described in Test Methods 1 and 1A using a colorimeter or
acid. Dilute to 1000 mL and mix. a turbidimeter. Set up a graph to determine chloride levels in
5.7.2 Standard MercuricAcetate Solution—Dilute40mLof samples.
stock mercuric acetate solution to 1000 mL and adjust the pH
7.4 Test Method 3—Extract the sample as described in Test
to 1.6 with nitric acid. Standardize in accordance with 7.5.5. Method 1. Analyze the water extract with an ion chromato-
5.7.3 s-Diphenylcarbazone Solution (Test Method 4)—
graphthathasbeencalibratedwithstandardsintheappropriate
Dissolve 0.5 g of s-diphenylcarbazone in 100 mLof methanol. ranges. This test method gives superior data over turbidity
methods.
6. Hazards
7.5 Test Method 4:
6.1 Solvent Hazards—Contact with the skin should be
7.5.1 Wash all glassware with chloride-free water until 10
avoided to prevent removal of natural oils. There are varying
mL of the washings show no trace of turbidity when 1 mL of
degrees of danger to inhalation, ingestion, and contact. The
silver nitrate solution is added.
usershouldrefertothemostrecenthealthregulationsconcern-
7.5.2 Transfer 100 mL of the sample into a 250-mL sepa-
ing the individual solvent.
ratory funnel, add 25 mL of chloride-free water to the sample
6.2 Concentrated nitric acid is very hazardous in contact
and shake for 1 min. Transfer the sample to a second 250-mL
with the skin or eyes. The vapors are very toxic and corrosive.
separatory funnel and drain the water into a 125-mL Erlenm-
6.3 Precaution—Wear safety glasses and rubber gloves
eyer flask. Rep
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