Standard Test Methods for Determination of Amine Acid Acceptance (Alkalinity) of Halogenated Organic Solvents

SIGNIFICANCE AND USE
4.1 This test method is useful for the determination of the amount of acid acceptance contributed by amines or bases as compared to other acid-accepting compounds.
SCOPE
1.1 These test methods, where applicable, cover the determination of the acid acceptance of halogenated organic solvents due to the presence therein of an organic amine titratable by standard acid. These test methods are suitable for samples of 0.001 to 0.02 weight percent (10 ppm to 200 ppm) alkalinity as NaOH. Two test methods are covered as follows:  
1.1.1 Test Method A—pH Method, and  
1.1.2 Test Method B—Indicator Method.  
1.1.3 Test Method C—GC Method.  
1.2 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.  
1.3 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.

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ASTM D2106-07(2022) - Standard Test Methods for Determination of Amine Acid Acceptance (Alkalinity) of Halogenated Organic Solvents
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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: D2106 − 07 (Reapproved 2022)
Standard Test Methods for
Determination of Amine Acid Acceptance (Alkalinity) of
Halogenated Organic Solvents
This standard is issued under the fixed designation D2106; 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 3. Terminology
3.1 Definitions:
1.1 These test methods, where applicable, cover the deter-
mination of the acid acceptance of halogenated organic sol- 3.1.1 amine acid acceptance—the degree to which an or-
ganic amine present in the halogenated organic solvent is
vents due to the presence therein of an organic amine titratable
bystandardacid.Thesetestmethodsaresuitableforsamplesof capable of absorbing or neutralizing acid generated by the
solvent or introduced into it from an external source.
0.001 to 0.02 weight percent (10 ppm to 200 ppm) alkalinity as
NaOH. Two test methods are covered as follows:
4. Significance and Use
1.1.1 Test Method A—pH Method, and
1.1.2 Test Method B—Indicator Method.
4.1 This test method is useful for the determination of the
1.1.3 Test Method C—GC Method.
amount of acid acceptance contributed by amines or bases as
1.2 This standard does not purport to address all of the compared to other acid-accepting compounds.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5. Purity of Reagents
priate safety, health, and environmental practices and deter-
5.1 Reagent grade chemicals shall be used in all tests.
mine the applicability of regulatory limitations prior to use.
Unless otherwise indicated, it is intended that all reagents shall
1.3 This international standard was developed in accor-
conform to the specifications of the Committee on Analytical
dance with internationally recognized principles on standard-
Reagents of the American Chemical Society, where such
ization established in the Decision on Principles for the
specifications are available. Other grades may be used, pro-
Development of International Standards, Guides and Recom-
vided it is first ascertained that the reagent is of sufficiently
mendations issued by the World Trade Organization Technical
high purity to permit its use without lessening the accuracy of
Barriers to Trade (TBT) Committee.
the determination.
5.2 Purity of Water—Unless otherwise indicated, references
2. Referenced Documents
to water shall be understood to mean distilled water or water of
2.1 ASTM Standards:
equal purity. Additional requirements are specified in 8.1 and
D6806 Practice for Analysis of Halogenated Organic Sol-
12.1.
vents and Their Admixtures by Gas Chromatography
TEST METHOD A—pH METHOD
E70 Test Method for pH of Aqueous Solutions With the
Glass Electrode
6. Summary of Test Method
E200 Practice for Preparation, Standardization, and Storage
of Standard and Reagent Solutions for ChemicalAnalysis
6.1 The amine acid acceptance of the halogenated organic
solvent is determined, after extraction into a volume of water
preadjusted to a pH of 3.9, by titrating with standard acid to a
pH of 3.9. The extraction is performed either by stirring the
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 May 1, 2022. Published May 2022. Originally
approved in 1962. Last previous edition approved in 2017 as D2106 – 07 (2017). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D2106-07R22. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2106 − 07 (2022)
immiscible liquids mechanically or by shaking the immiscible the stirrer. Stir vigorously for 10 s again. Remove the stirrer,
layers of liquids manually. inserttheelectrodes,andagaintitratetoapHof3.9.Repeatthe
steps until additional stirring does not result in a change of pH
7. Apparatus
(Note 2). Record the final titration and calculate the amine acid
7.1 pH Meter, equipped with a pH indicating electrode and acceptance. When a magnetic stirring bar is used, it is not
pH reference electrode or combination electrode. necessary to remove it between agitation periods.
7.2 Stirrer, electric stirring bar, air-driven or magnetic.
NOTE 2—If the readings of the pH meter are erratic because the
electrodes have been wet with halogenated solvent, it may be treated by
8. Reagents
rinsing the electrode with acetone or alcohol, followed by thorough
rinsing with water and soaking in water for a short time.
8.1 Water—Adjust the pH of 1 L (or any convenient
quantity) of water to 3.9. Boil 1 L of distilled water for 5 min
9.3 Using Hand Agitation—If no stirrer is available, the
in a borosilicate glass or stainless steel container, then cover
extraction and titration may be carried out as follows: Transfer
and cool to room temperature. Titrate a 50 mL aliquot to a pH
50 mL of the halogenated organic solvent to a 250 mL
of 3.8 to 4.0 with 0.01 N hydrochloric acid (HCl) (or 0.01
glass-stoppered Erlenmeyer flask, add 50 mL of water pread-
N NaOH if the pH is below 3.8). From this titer, calculate the
justed to a pH of 3.9, and stopper the flask. Shake vigorously
volume of 0.01 N HCl (or NaOH) required to adjust the pH of
for 5 s. Pour the contents into a 150 mL beaker and allow the
the remaining 950 mL of boiled distilled water to a pH of 3.8
immiscible liquids to separate into layers. Insert the pH meter
to 4.0. The calculation is as follows:
electrodes and titrate the water layer with 0.01 N HCl to a pH
of 3.9. When the end point has been reached, remove the
3titer (1)
electrodes, return the liquids to the flask, and extract again for
5s.Repeatthetitration.Repeattheextractionandtitrationuntil
Add the calculated amount of 0.01 N HCl (or NaOH)
no change in pH results from additional shaking (Note 2).
together with the titrated 50 mLaliquot of water to the 950 mL
Record the final titration and calculate the amine acid accep-
stock and mix thoroughly. Determine the pH of a second
tance.
aliquot. If further adjustment is necessary to obtain a pH of 3.8
to 4.0, repeat the preceding procedure.
10. Calculation
8.2 Hydrochloric Acid, Standard (0.01 N)—Dilute 1.8 mL
10.1 Calculate the Amine Acid Acceptance (alkalinity) as
of concentrated hydrochloric acid (HCl, sp gr 1.19) to 1 Lwith
NaOH, in weight percent as follows:
water and standardize in accordance with Practice E200,
Sections 20 through 23. Certified reagent of 0.01 N HCl may
Amine Acid Acceptance alkalinity , as NaOH, Weight Percent5(2)
~ !
be purchased from supply houses.
V 2 B/2 3NX 0.040 /W 3100
$@~ ~ !! # %
8.3 pH 4.0 Buffer Solution, available from most supply
houses.
or as parts per million as follows:
8.4 pH 7.0 Buffer Solution, available from most supply
Amine Acid Acceptance ~alk
...

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