ASTM D2073-92(1998)e1

Standard Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines, Amidoamines, and Diamines by Referee Potentiometric Method (Withdrawn 2007)

SCOPE
1.1 These referee test methods cover the potentiometric determination of the total, primary, secondary, and tertiary amine values of fatty amines and diamines, and the total amine value of fatty amidoamines. Test methods for primary, secondary, and tertiary amine values are not applicable to fatty amidoamines.  
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 hazard statements are given in Notes 1 and 2 and 6.1.
WITHDRAWN RATIONALE
These referee test methods cover the potentiometric determination of the total, primary, secondary, and tertiary amine values of fatty amines and diamines, and the total amine value of fatty amidoamines. Test methods for primary, secondary, and tertiary amine values are not applicable to fatty amidoamines.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1991
• Withdrawal Date: 19-Mar-2007
• ICS: 71.080.30 - Organic nitrogen compounds
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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Designation:D2073–92(Reapproved1998)
Standard Test Methods for
Total, Primary, Secondary, and Tertiary Amine Values of
Fatty Amines, Amidoamines, and Diamines by Referee
Potentiometric Method
This standard is issued under the fixed designation D 2073; 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.
These methods were prepared jointly by ASTM and the American Oil Chemists’ Society.
e NOTE—Former Footnote 6 was deleted editorially in May 1998.
1. Scope 3.1.3 secondary amine value—the number of milligrams of
potassiumhydroxide(KOH)equivalenttothesecondaryamine
1.1 These referee test methods cover the potentiometric
basicity in1gof specimen.
determination of the total, primary, secondary, and tertiary
3.1.4 tertiary amine value—the number of milligrams of
amine values of fatty amines and diamines, and the total amine
potassium hydroxide (KOH) equivalent to the tertiary amine
value of fatty amidoamines. Test methods for primary, second-
basicity in1gof specimen.
ary, and tertiary amine values are not applicable to fatty
amidoamines.
4. Apparatus
1.2 This standard does not purport to address all of the
4.1 Air Condenser, minimum length 650 mm.
safety concerns, if any, associated with its use. It is the
4.2 Erlenmeyer Flask, wide-mouth, alkali-resistant,
responsibility of the user of this standard to establish appro-
borosilicate-glass, 250-mL capacity.
priate safety and health practices and determine the applica-
4.3 Glass Electrode pH Meter, conforming to the require-
bility of regulatory limitations prior to use. Specific hazard
ments of Test Method E 70 or similar potentiometric titrator.
statements are given in Note 1 and Note 2 and Note 6.1.
4.4 Hot Plate, with variable heat control.
2. Referenced Documents 4.5 Magnetic Stirrer, with inert plastic-coated stirring bar.
4.6 Microburet, graduated to 0.02 mLand having a capacity
2.1 ASTM Standards:
of 10 mL.
D 1193 Specification for Reagent Water
D 2080 Test Method forAverage MolecularWeight of Fatty
5. Reagents
Quaternary Ammonium Chlorides
5.1 Purity of Reagents—Reagent grade chemicals shall be
E 70 Test Method for pH of Aqueous Solutions with the
4 used in all tests. Unless otherwise indicated, it is intended that
Glass Electrode
all reagents shall conform to the specifications of the Commit-
3. Terminology tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
3.1 Definitions:
used, provided it is first ascertained that the reagent is of
3.1.1 total amine value—the number of milligrams of po-
sufficiently high purity to permit its use without lessening the
tassium hydroxide (KOH) equivalent to the basicity in1gof
accuracy of the determination.
specimen.
5.2 Purity of Water—Unless otherwise indicated, references
3.1.2 primary amine value—the number of milligrams of
towatershallbeunderstoodtomeanreagentwaterconforming
potassium hydroxide (KOH) equivalent to the primary amine
to Type II of Specification D 1193.
basicity in1gof specimen.
5.3 Acetic Acid, Glacial (CH COOH). (Warning—See
Note 1).
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD-1onPaint
and Related Coatings, Materials, andApplications, and are the direct responsibility
of Subcommittee D01.32 on Drying Oils. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved March 15, 1992. Published May 1992. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
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published as D 2073 – 62. Last previous edition D 2073 – 66 (1987) . listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 06.03. 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.
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D2073–92 (1998)
TABLE 1 Specimen Weights
5.4 Acetic Anhydride.
5.5 Chloroform (CHCl ). (Warning—See Note 2). Specimen Weight
Secondary plus
5.6 Hydrochloric Acid, Standard Solution (0.5 N)—Add 85
Type of Fatty Amine Tertiary Amine
Tertiary Amine
Value, g
mLofconcentratedhydrochloricacid(HCl,spgr1.19)to1000
Value, g
mL of isopropyl alcohol in a 2-L volumetric flask. Dilute to Primary fatty amine 5 5
Secondary fatty amine 1 5
volumeandmix.StandardizewithsodiumcarbonatetoapHof
Tertiary fatty amine 1 1
3.5.
5.7 Isopropanol (1 + 19)—Add 5 mL of water to 95 mL of
isopropyl alcohol (99 %).
temperature. Add 5 to 6 mL of salicylaldehyde and allow to
5.8 Perchloric Acid, Standard Solution (0.1 N)—Prepare
stand for 30 min. After 30 min add 10 mL of isopropanol
and standardize in accordance with Test Method D 2080.
solution. Insert the stirring bar into the beaker and adjust the
5.9 Salicylaldehyde.
beaker so that the lower half of each electrode of the pH meter
6. Hazards is immersed in the sample. Start the stirrer and adjust the speed
sothatthereisvigorousstirringwithoutspattering.Titratewith
6.1 Fatty amines and diamines can sensitize and irritate.
0.5 N HCl using the millivolt scale. Record the millivolt
Wash from clothing and body surfaces immediately on contact.
readings every 1 mL, but in the vicinity of the end point record
NOTE 1—Warning: Glacial acetic acid, concentrated hydrochloric
the millivolt readings every 0.1 mL. Plot a graph showing the
acid, 70 to 72 % perchloric acid, and acetic anhydride can cause burns of
millivolts against the millilitres require
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