ASTM D2106-07(2017)

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 – 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.

General Information

• Status: Historical
• Publication Date: 31-Oct-2017
• ICS: 71.080.20 - Halogenated hydrocarbons
• Technical Committee: D26 - Halogenated Organic Solvents and Fire Extinguishing Agents
• Drafting Committee: D26.04 - Test Methods

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D2106 − 07 (Reapproved 2017)
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 – 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 Nov. 1, 2017. Published December 2017. Originally
approved in 1962. Last previous edition approved in 2012 as D2106 – 07 (2012). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D2106-07R17. 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 [e-mail]. 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 (2017)
immiscible liquids mechanically or by shaking the immiscible and reinsert the stirrer. Stir vigorously for 10 s again. Remove
layers of liquids manually. the stirrer, insert the electrodes, and again titrate to a pH of 3.9.
Repeat the steps until additional stirring does not result in a
7. Apparatus
change of pH (Note 2). Record the final titration and calculate
7.1 pH Meter, equipped with a pH indicating electrode and the amine acid acceptance. When a magnetic stirring bar is
pH reference electrode or combination electrode. used,itisnotnecessarytoremoveitbetweenagitationperiods.
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 N
glass-stoppered Erlenmeyer flask, add 50 mL of water pread-
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,
Sections20through23.Certifiedreagentof0.01 NHClmaybe
Amine Acid Acceptance alkalinity , as NaOH, Weight Percent5(2)
~ !
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 ~alkalinity!, as NaOH, ppm5 (3)
houses.
NOTE 1—Hydrochloric acid of about
...

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: D2106 − 07 (Reapproved 2012) D2106 − 07 (Reapproved 2017)
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
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 – 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 safety, health, and healthenvironmental 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.
2. Referenced Documents
2.1 ASTM Standards:
D6806 Practice for Analysis of Halogenated Organic Solvents and Their Admixtures by Gas Chromatography
E70 Test Method for pH of Aqueous Solutions With the Glass Electrode
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
3. Terminology
3.1 Definitions:
3.1.1 amine acid acceptance—the degree to which an organic amine present in the halogenated organic solvent is capable of
absorbing or neutralizing acid generated by the solvent or introduced into it from an external source.
4. 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.
5. Purity of Reagents
5.1 Reagent grade chemicals shall be used in all tests. 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 specifications 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 Sept. 1, 2012Nov. 1, 2017. Published November 2012December 2017. Originally approved in 1962. Last previous edition approved in 20072012
as D2106 – 07.D2106 – 07 (2012). DOI: 10.1520/D2106-07R12.10.1520/D2106-07R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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
D2106 − 07 (2017)
5.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean distilled water or water of
equal purity. Additional requirements are specified in 8.1 and 12.1.
TEST METHOD A—pH METHOD
6. Summary of Test Method
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
immiscible liquids mechanically or by shaking the immiscible layers of liquids manually.
7. Apparatus
7.1 pH Meter, equipped with a pH indicating electrode and pH reference electrode or combination electrode.
7.2 Stirrer, electric stirring bar, air-driven or magnetic.
8. Reagents
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 in a
borosilicate glass or stainless steel container, then cover and cool to room temperature. Titrate a 50-mL aliquot to a pH of 3.8 to
4.0 with 0.01 N hydrochloric acid (HCl) (or 0.01 N NaOH if the pH is below 3.8). From this titer, calculate the volume of 0.01
N HCl (or NaOH) required to adjust the pH of the remaining 950 mL of boiled distilled water to a pH of 3.8 to 4.0. The calculation
is as follows:
3titer (1)
Add the calculated amount of 0.01 N HCl (or NaOH) together with the titrated 50 mL aliquot of water to the 950 mL stock and
mix thoroughly. Determine the pH of a second aliquot. If further adjustment is necessary to obtain a pH of 3.8 to 4.0, repeat the
preceding procedure.
8.2 Hydrochloric Acid, Standard (0.01 N)—Dilute 1.8 mL of concentrated hydrochloric acid (HCl, sp gr 1.19) to 1 L with water
and standardize in accordance with Practice E200, Sections 20 through 23. Certified reagent of 0.01 N HCl may be purchased from
supply houses.
8.3 pH 4.0 Buffer Solution, available from most supply houses.
8.4 pH 7.0 Buffer Solution, available from most supply houses.
NOTE 1—Hydrochloric acid of about 0.01 to about 0.02 N can be used. It can be difficult to see the end point when using hydrochloric acid much below
about 0.01 N and concentrations much above 0.02 N increase the likelihood of over-titrating the end point when titrating samples of low alkalinity. For
alkalinity below about 0.00075 % (75 ppm), 0.01 N HCl is appropriate. For alkalinity above about 75 ppm, 0.02 N HCl is appropriate.
9. Procedure
9.1 Calibrate the pH meter in accordance with Test Method E70.
9.1.1 Prepare a blank using 100 mL of water previously adjusted to pH 3.9, and subject it to the same type and degree of
agitation as the test samples. Titrate the blank to pH 3.9 and record the volume of titrant as B.
9.2 Using Mechanical Agitation—Transfer 50 mL of the halogenated organic solvent to a 150-mL beaker and add 50 mL 50 mL
of water previously adjusted to a pH of 3.9. Insert a stirrer, and stir as vigorously as possible for 10 s. Stop the stirrer and lift it
out of the beaker. Allow the liquids to separate. Insert the pH meter electrodes into the separated aqueous upper layer, avoiding
contact of the electrodes with the solvent layer, 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 electrodes and reinsert the stirrer. Stir vigorously for 10 s again. Remove the stirrer, insert the
electrodes, and again titrate to a pH of 3.9. Repeat the steps until additional stirring does not result in a change of pH (Note 2).
Record the final titration and calculate the amine acid acceptance. When a magnetic stirring bar is used, it is not necessa
...