ASTM D2106-00
(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
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 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.
1.2 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:D2106–00
Standard Test Methods for
Determination of Amine Acid Acceptance (Alkalinity) of
Halogenated Organic Solvents
This standard is issued under the fixed designation D 2106; 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. Purity of Reagents
1.1 These test methods, where applicable, cover the deter- 5.1 Reagent grade chemicals shall be used in all tests.
mination of the acid acceptance of halogenated organic sol- Unless otherwise indicated, it is intended that all reagents shall
vents due to the presence therein of an organic amine titratable conform to the specifications of the Committee on Analytical
bystandardacid.Thesetestmethodsaresuitableforsamplesof Reagents of the American Chemical Society, where such
0.001 to 0.02 weight percent alkalinity as NaOH. Two test specifications are available. Other grades may be used, pro-
methods are covered as follows: vided it is first ascertained that the reagent is of sufficiently
1.1.1 Test Method A— pH Method, and high purity to permit its use without lessening the accuracy of
1.1.2 Test Method B— Indicator Method. the determination.
1.2 This standard does not purport to address all of the 5.2 Purity of Water— Unless otherwise indicated, refer-
safety concerns, if any, associated with its use. It is the ences to water shall be understood to mean distilled water or
responsibility of the user of this standard to establish appro- water of equal purity. Additional requirements are specified in
priate safety and health practices and determine the applica- 8.1 and 12.1.
bility of regulatory limitations prior to use.
TEST METHOD A—pH METHOD
2. Referenced Documents
6. Summary of Test Method
2.1 ASTM Standards:
6.1 The amine acid acceptance of the halogenated organic
E 70 Test Method for pH of Aqueous Solutions With the
2 solvent is determined, after extraction into a volume of water
Glass Electrode
preadjusted to a pH of 3.9, by titrating with standard acid to a
E 200 Practice for Preparation, Standardization, and Stor-
pH of 3.9. The extraction is performed either by stirring the
age of Standard and Reagent Solutions for Chemical
2 immiscible liquids mechanically or by shaking the immiscible
Analysis
layers of liquids manually.
3. Terminology
7. Apparatus
3.1 Definition:
7.1 pH Meter, equipped with a pH indicating electrode and
3.1.1 amine acid acceptance—the degree to which an or-
pH reference electrode or combination electrode.
ganic amine present in the halogenated organic solvent is
7.2 Stirrer, electric stirring bar, air-driven or magnetic.
capable of absorbing or neutralizing acid generated by the
solvent or introduced into it from an external source.
8. Reagents
8.1 Water—Adjust the pH of 1 L (or any convenient
4. Significance and Use
quantity) of water to 3.9. Boil 1 L of distilled water for 5 min
4.1 This test method is useful for the determination of the
in a borosilicate glass or stainless steel container, then cover
amount of acid acceptance contributed by amines or bases as
and cool to room temperature. Titrate a 50-mL aliquot to a pH
compared to other acid-accepting compounds.
1 3
These test methods are under the jurisdiction of ASTM Committee D26 on Reagent Chemicals, American Chemical Society Specifications, American
Halogenated Organic Solvents and Fire Extinguishing Agents and are 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 June 10, 2000. Published September 2000. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
issued as D 2106 – 62 T. Last previous edition D 2106 – 95. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.05. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2106
of 3.8 to 4.0 with 0.01 N hydrochloric acid (HCl) (or 0.01 N 5s.Repeatthetitration.Repeattheextractionandtitrationuntil
NaOH if the pH is below 3.8). From this titer, calculate the no change in pH results from additional shaking (Note 1).
volume of 0.01 N HCl (or NaOH) required to adjust the pH of Record the final titration and calculate the amine acid accep-
the remaining 950 mL of boiled distilled water to a pH of 3.8 tance.
to 4.0. The calculation is as follows:
10. Calculation
3 titer (1)
10.1 Calculate the amine acid acceptance as equivalent
sodium hydroxide in weight percent as follows:
Add the calculated amount of 0.01 N HCl (or NaOH)
Equivalent NaOH, weight percent 5
together with the titrated 50 mLaliquot of water to the 950 mL
$@~V– B/2 3 N 3 0.040 /W 3 100 (2)
~ !! # %
stock and mix thoroughly. Determine the pH of a second
aliquot. If further adjustment is necessary to obtain a pH of 3.8
where:
to 4.0, repeat the preceding procedure.
V = HCl required for titration of the sample, mL,
8.2 Hydrochloric Acid, Standard (0.02 N)—Dilute 1.8 mL
N = normality of the HCl,
of concentrated hydrochloric acid (HCl, sp gr 1.19) to 1 Lwith
B = HCl required for titration of the blank, mL, and
water and standardize in accordance with Practice E 200, W = sample used (volume in millilitres times its specific
Sections20through23.Certifiedreagentof0.02NHClmaybe
gravity), g.
purchased from supply houses.
NOTE 2—Example:Where the solvent is trichloroethylene, the equation
8.3 pH 4.0 Buffer Solution, available from most supply
becomes:
houses.
Equivalent NaOH, weight percent 5 @~ VN 3 0.04!/~50 3 1.463!#
8.4 pH 7.0 Buffer Solution, available from most supply
3 100
houses.
5 VN 3 0.055 (3)
9. Procedure
11. Precision and Bias
9.1 Calibrate the pH meter in accordance with Test Method
11.1 The precision limits of this test have been determined
E 70.
as 0.0005 % (equivalent
...
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