Standard Test Method for Acidity-Alkalinity of Halogenated Organic Solvents and Their Admixtures

SCOPE
1.1 This test method covers the determination of acidity in halogenated organic solvents and admixtures thereof. The alkalinity may be determined utilizing Test Method D2106, by substituting the end point measured at pH7 by bromothymol blue or pH meter.  
1.2 This standard does not purport to address all of the safety problems, 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 7.

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ASTM D2989-97 - Standard Test Method for Acidity-Alkalinity of Halogenated Organic Solvents and Their Admixtures
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 2989 – 97
Standard Test Method for
Acidity-Alkalinity of Halogenated Organic Solvents and
Their Admixtures
This standard is issued under the fixed designation D 2989; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 5. Apparatus
1.1 This test method covers the determination of acidity in 5.1 Separatory Funnel, 250-mL.
halogenated organic solvents and admixtures thereof. The 5.2 Graduated Cylinder, 100 mL.
alkalinity may be determined utilizing Test Method D 2106, by 5.3 Volumetric Pipets, 1 mL, 10 mL, 25 mL, 50 mL.
substituting the end point measured at pH7 by bromothymol 5.4 Beaker, 100 mL.
blue or pH meter. 5.5 Borosilicate or Stainless Steel Beaker,2L.
1.2 This standard does not purport to address all of the 5.6 Erlenmeyer Flask, 100 mL.
safety concerns, if any, associated with its use. It is the 5.7 pH Meter with pH Electrodes.
responsibility of the user of this standard to establish appro- 5.8 Buret,10mL.
priate safety and health practices and determine the applica- 5.9 Volumetric Flask, 100 mL, 1 L.
bility of regulatory limitations prior to use. Specific precau-
6. Reagents
tionary statements are given in Section 7.
6.1 Purity of Reagents—Reagent grade chemicals shall be
2. Referenced Documents
used in all tests. Unless otherwise indicated, it is intended that
2.1 ASTM Standards: all reagents shall conform to the specifications of the Commit-
D 2106 Test Method for the Determination of Amine Acid tee on Analytical Reagents of the American Chemical Society,
2 3
Acceptance (Alkalinity) of Halogenated Organic Solvents where such specifications are available. Other grades may be
D 2110 Test Method for pH of Water Extractions of Halo- used, provided it is first ascertained that the reagent is of
genated Organic Solvents and Their Admixtures sufficiently high purity to permit its use without lessening the
accuracy of the determination.
3. Summary of Test Method
6.2 Water—Prepare neutral distilled water as follows: Boil 1
3.1 A sample of halogenated solvent or admixture is mea-
L of distilled water for 5 min in a borosilicate glass or stainless
sured for pH using Test Method D 2110. If the pH of the steel container, then cover and cool to room temperature.
sample is above 7.0, the alkalinity is determined using Test
Titrate a 50-mL aliquot to a pH of 7.0 to 7.3 with either 0.01
Method D 2106 (to an end point of pH 7). If the pH is below N sodium hydroxide (NaOH) solution or 0.01 N hydrochloric
7.0, the free acid content of the halogenated organic solvent or
acid (HCl), depending upon whether the initial pH is above or
admixture is determined after water extraction using Procedure
below 7. From this titer, calculate the volume of 0.01 N NaOH
A or B, or can be determined directly using Procedure C. solution or 0.01 N HCl required to adjust the pH of the
3.1.1 Procedure A, using glass electrode pH meter, or
remaining 950 mL of boiled distilled water to a pH of 7.0 to
3.1.2 Procedure B, using indicator. 7.3. Add the calculated volume of 0.01 N NaOH solution or
3.2 Procedure C, anhydrous methanolic sodium hydroxide
0.01 N HCl together with the titrated 50-mL aliquot of
titration. neutralized water to the 950-mL stock and mix thoroughly.
Determine the pH of a second aliquot. If further adjustment is
4. Significance and Use
necessary to obtain a pH of 7.0 to 7.3, repeat this procedure.
4.1 This test method can be used to establish manufacturing
6.3 Bromothymol Blue Indicator Solution (0.1 %)—
and purchasing specifications. It can also be used to determine
Indicator solution may be purchased from a laboratory supply
the condition of solvents in use.
Reagent Chemicals, American Chemical Society Specifications, American
This test method is under the jurisdiction of ASTM Committee D-26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and is 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 Dec. 10, 1997. Published May 1998. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 2989 – 71 T. Last previous edition D 2989 – 93. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.05. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 2989
house or prepared as follows: Dissolve 0.1 g of dibromothymol for 2 min, then let stand and allow the layers to separate. Pipet
sulfonephthalein in 1.6 mL of 0.1 N NaOH solution and dilute a 25-mL aliquot of the water layer into a 100-mL beaker. Add
to 100 mL with methanol. 1 mL of bromothymol blue indicator solution to the sample.
6.4 Sodium Hydroxide Solution (0.01 N), Procedures A and Titrate, with
...

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