ASTM D2988-96(2000)
(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
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 2000)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4.3 Erlenmeyer Flask, 125-mL, and
4.4 Colorimeter or Turbidimeter, Method 2.
1.1 Test Methods 1, 2, and 3—These test methods cover the
determination of water-extractable halide ion in halogenated
5. Reagents
organic solvents and their admixtures. Fluoride ion is not
5.1 Purity of Reagents—Reagent grade chemicals shall be
measured due to the solubility of silver fluoride.
usedinalltest.Unlessotherwiseindicateditisintendedthatall
1.2 Test Method 4—This test method covers the determina-
reagents shall conform to the specifications of the Committee
tion of chloride ion in halogenated organic solvents and their
on Analytical Reagents of the American Chemical Society,
admixtures.
where such specification are available. Other grades may be
1.3 This standard does not purport to address all of the
used, provided it is first ascertained that the reagent is of
safety concerns, if any, associated with its use. It is the
sufficiently high purity to permit its use without lessening the
responsibility of the user of this standard to establish appro-
accuracy of the determination.
priate safety and health practices and determine the applica-
5.2 Purity of Water—Unlessotherwiseindicated,references
bility of regulatory limitations prior to use. Specific precau-
towatershallbeunderstoodtomeanhalide-freedistilledwater.
tionary statements are given in Section 6.
−
5.3 Chloride Standard (1 mL> 0.0001 g Cl ), Test Methods
2. Summary of Test Methods 1, 2, and 3—Prepare by adding 0.165 g of sodium chloride
(NaCl) to 1 L of halide-free distilled water.
2.1 Summary of Test Methods 1, 2, 3—Halideionpresentin
−
5.4 Chloride Standard (1 mL = 0.000001 g Cl ), Test
halogenated organic solvents is extracted with water and
Method 4—Dissolve 0.0660 g of sodium chloride in water and
precipitatedasthesilverhalidesaltwithsilvernitrate.Quantity
diluteto1000mL.Pipet25mLofthissolutionintoa1000-mL
of the halide present is determined by comparing the turbidity
volumetric flask, dilute to volume, and mix.
of the sample to known standards. The distilled water, as well
5.5 Nitric Acid (sg gr 1.42), concentrated nitric acid
as all glassware used, must be halide-free.
(HNO ).
2.2 Summary of Test Method 4—This test method is based
5.6 Silver Nitrate Solution 0.1 N—Prepare a 0.1 N solution
on the determination of ionizable chloride by titration with
of silver nitrate (AgNO ).
mercuric acetate solution using s-diphenylcarbazone as the
5.6.1 Preparethesilvernitratesolutionbyadding16.99gof
indicator.
silver nitrate to a 1-L volumetric flask and fill to the line with
3. Significance and Use halide-free distilled water. After shaking to dissolve the
AgNO , store in an amber bottle.
3.1 These test methods are used to establish manufacturing 3
5.7 Mercuric Acetate Solution, Test Method 4.
and purchasing specifications.These test methods will provide
5.7.1 Stock Mercuric Acetate Solution—Dissolve 1.6 g of
a means of determining the condition of the solvent in use. A
mercuricacetatein500mLofwatercontaining3.5mLofnitric
high water soluble chloride level may indicate the start of
acid. Dilute to 1000 mL and mix.
solvent decomposition.
5.7.2 Standard MercuricAcetate Solution—Dilute40mLof
4. Apparatus
stock mercuric acetate solution to 1000 mL and adjust the pH
to 1.6 with nitric acid. Standardize in accordance with 7.5.5.
4.1 Separatory Funnel, 500-mL,
4.2 Nessler Tubes, 50-mL,
Reagent Chemicals, American Chemical Society Specifications, American
These test methods are under the jurisdiction of ASTM Committee D26 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. Pharmacopeial Convention, Inc. (USPC), Rockville,
published as D2988–71T. Last previous edition D2988–92. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2988
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:
7.5.1 Wash all glassware with chloride-free water until 10
6.1 Solvent Hazards—Contact with the skin should be
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. Repeat the extraction once with another 25 mL of
when handling the silver nitrate or its solution. water. Combine the water extracts in the Erlenmeyer flask.
6.4 Mercuric acetate is toxic. 7.5.3 Warm the water extract to 60°C to drive off any
6.5 The hazards of s-diphenylcarbazone are not known. remaining sample. Cool to room temperature.
7.5.4 Add five drops of s
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