ASTM D2106-07(2012)
(Test Method)Standard Test Methods for Determination of Amine Acid Acceptance (Alkalinity) of Halogenated Organic Solvents
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D2106 − 07 (Reapproved 2012)
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 Department of Defense.
1. Scope 4. Significance and Use
1.1 These test methods, where applicable, cover the deter- 4.1 This test method is useful for the determination of the
mination of the acid acceptance of halogenated organic sol- amount of acid acceptance contributed by amines or bases as
vents due to the presence therein of an organic amine titratable compared to other acid-accepting compounds.
bystandardacid.Thesetestmethodsaresuitableforsamplesof
0.001 to 0.02 weight percent (10 – 200 ppm) alkalinity as 5. Purity of Reagents
NaOH. Two test methods are covered as follows:
5.1 Reagent grade chemicals shall be used in all tests.
1.1.1 Test Method A— pH Method, and
Unless otherwise indicated, it is intended that all reagents shall
1.1.2 Test Method B— Indicator Method.
conform to the specifications of the Committee on Analytical
1.1.3 Test Method C—GC Method.
Reagents of the American Chemical Society, where such
1.2 This standard does not purport to address all of the specifications are available. Other grades may be used, pro-
safety concerns, if any, associated with its use. It is the vided it is first ascertained that the reagent is of sufficiently
responsibility of the user of this standard to establish appro- high purity to permit its use without lessening the accuracy of
priate safety and health practices and determine the applica- the determination.
bility of regulatory limitations prior to use.
5.2 Purity of Water—Unlessotherwiseindicated,references
to water shall be understood to mean distilled water or water of
2. Referenced Documents
equal purity. Additional requirements are specified in 8.1 and
2.1 ASTM Standards:
12.1.
D6806 Practice for Analysis of Halogenated Organic Sol-
TEST METHOD A—pH METHOD
vents and Their Admixtures by Gas Chromatography
E70 Test Method for pH of Aqueous Solutions With the
6. Summary of Test Method
Glass Electrode
E200 Practice for Preparation, Standardization, and Storage
6.1 The amine acid acceptance of the halogenated organic
of Standard and Reagent Solutions for ChemicalAnalysis
solvent is determined, after extraction into a volume of water
preadjusted to a pH of 3.9, by titrating with standard acid to a
3. Terminology
pH of 3.9. The extraction is performed either by stirring the
3.1 Definitions: immiscible liquids mechanically or by shaking the immiscible
3.1.1 amine acid acceptance—the degree to which an or-
layers of liquids manually.
ganic amine present in the halogenated organic solvent is
capable of absorbing or neutralizing acid generated by the 7. Apparatus
solvent or introduced into it from an external source.
7.1 pH Meter, equipped with a pH indicating electrode and
pH reference electrode or combination electrode.
These test methods are under the jurisdiction of ASTM Committee D26 on
7.2 Stirrer, electric stirring bar, air-driven or magnetic.
Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct
responsibility of Subcommittee D26.04 on Test Methods.
Current edition approved Sept. 1, 2012. Published November 2012. Originally
approved in 1962. Last previous edition approved in 2007 as D2106 – 07. DOI: Reagent Chemicals, American Chemical Society Specifications , American
10.1520/D2106-07R12. 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 (2012)
rinsing the electrode with acetone or alcohol, followed by thorough
8. Reagents
rinsing with water and soaking in water for a short time.
8.1 Water—Adjust the pH of 1 L (or any convenient
9.3 Using Hand Agitation—If no stirrer is available, the
quantity) of water to 3.9. Boil 1 L of distilled water for 5 min
extraction and titration may be carried out as follows: Transfer
in a borosilicate glass or stainless steel container, then cover
50 mL of the halogenated organic solvent to a 250-mL
and cool to room temperature. Titrate a 50-mL aliquot to a pH
glass-stoppered Erlenmeyer flask, add 50 mL of water pread-
of 3.8 to 4.0 with 0.01 N hydrochloric acid (HCl) (or 0.01 N
justed to a pH of 3.9, and stopper the flask. Shake vigorously
NaOH if the pH is below 3.8). From this titer, calculate the
for 5 s. Pour the contents into a 150-mL beaker and allow the
volume of 0.01 N HCl (or NaOH) required to adjust the pH of
immiscible liquids to separate into layers. Insert the pH meter
the remaining 950 mL of boiled distilled water to a pH of 3.8
electrodes and titrate the water layer with 0.01 N HCl to a pH
to 4.0. The calculation is as follows:
of 3.9. When the end point has been reached, remove the
electrodes, return the liquids to the flask, and extract again for
3titer (1)
5s.Repeatthetitration.Repeattheextractionandtitrationuntil
no change in pH results from additional shaking (Note 2).
Add the calculated amount of 0.01 N HCl (or NaOH)
Record the final titration and calculate the amine acid accep-
together with the titrated 50 mLaliquot of water to the 950 mL
tance.
stock and mix thoroughly. Determine the pH of a second
aliquot. If further adjustment is necessary to obtain a pH of 3.8
10. Calculation
to 4.0, repeat the preceding procedure.
10.1 Calculate the Amine Acid Acceptance (alkalinity) as
8.2 Hydrochloric Acid, Standard (0.01 N)—Dilute 1.8 mL
NaOH, in weight percent as follows:
of concentrated hydrochloric acid (HCl, sp gr 1.19) to 1 Lwith
water and standardize in accordance with Practice E200,
Amine Acid Acceptance ~alkalinity!, as NaOH, Weight Percent5(2)
Sections20through23.Certifiedreagentof0.01 NHClmaybe
V 2 B/2 3NX 0.040 /W 3100
$@~ ~ !! # %
purchased from supply houses.
8.3 pH 4.0 Buffer Solution, available from most supply or as parts per million as follows:
houses.
Amine Acid Acceptance alkalinity , as NaOH, ppm5 (3)
~ !
8.4 pH 7.0 Buffer Solution, available from most supply
V 2 B/2 3NX 0.040 /W 31000000
$@~ ~ !! # %
houses.
NOTE 1—Hydrochloric acid of about 0.01 to about 0.02 N can be used.
where:
It can be difficult to see the end point when using hydrochloric acid much
V = millilitres HCl required for titration of the sample, mL,
below about 0.01 N and concentrations much above 0.02 N increase the
N = normality of the HCl,
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 B = millilitres HCl required for titration of the blank, mL,
appropriate.Foralkalinityaboveabout75ppm,0.02 NHClisappropriate.
and
W = weight sample used (or volume in millilitres times its
9. Procedur
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