ASTM D2072-92(1998)e1

Standard Test Method for Water in Fatty Nitrogen Compounds (Withdrawn 2007)

SCOPE
1.1 This test method covers the determination of water in fatty nitrogen compounds by titration with a water-methanol solution after addition of an excess of Karl Fischer reagent.  
1.2 The procedures appear in the following order:  Sections Fatty Primary Amines, Diamines, and Amidoamines 4 to 8 Difatty Secondary Amines 9 to 12 Quaternary Ammonium Chlorides 13 to 16
1.3 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 5.3, 6.1, and 11.2.
WITHDRAWN RATIONALE
This test method covers the determination of water in fatty nitrogen compounds by titration with a water-methanol solution after addition of an excess of Karl Fischer reagent.
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the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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• Status: Withdrawn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: 02-Jun-1998
• Withdrawal Date: 19-Mar-2007
• ICS: 87.060.30 - Solvents
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications

Relations

• Referred By: ASTM E203-23 - Standard Test Method for Water Using Volumetric Karl Fischer Titration
• Effective Date: 03-Jun-1998

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
e1
Designation:D2072–92 (Reapproved 1998)
Standard Test Method for
Water in Fatty Nitrogen Compounds
This standard is issued under the fixed designation D 2072; 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 test method was prepared jointly by ASTM and the American Oil Chemists’ Society.
e NOTE—Former Footnote 4 was deleted editorially in May l998.
1. Scope is back-titrated with water-methanol solution. The end point is
best detected electrometrically, but with practice it may be
1.1 This test method covers the determination of water in
satisfactorily determined visually.
fatty nitrogen compounds by titration with a water-methanol
solution after addition of an excess of Karl Fischer reagent.
FATTY PRIMARYAMINES, DIAMINES,AND
1.2 The procedures appear in the following order:
AMIDOAMINES
Sections
4. Apparatus
Fatty Primary Amines, Diamines, and Amidoamines 4-8
Difatty Secondary Amines 9-12
4.1 Buret and Bottle Assemblies (or other convenient ar-
Quaternary Ammonium Chlorides 13-16
rangement), protected with silica gel so as to maintain Karl
1.3 This standard does not purport to address all of the Fischer reagent and water-methanol solutions free from con-
tamination with moisture either through the atmosphere or
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- otherwise (Note 1). The titration should be performed in a
closed system to avoid the absorption of water. The electrode
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard and buret shall be mounted through a close-fitting stopper, and
provision made for mechanical stirring by means of a magnetic
statements are given in 5.3, 6.1, and 11.2.
stirrer.
2. Referenced Documents
NOTE 1—It is essential that the Karl Fischer reagent, water-methanol
2.1 ASTM Standards:
solution,andanhydrousmethanolbeprotectedfromatmosphericmoisture
D 1193 Specification for Reagent Water
at all times. In humid seasons or climates, the drying tubes used to protect
D 1364 Test Method for Water in Volatile Solvents (Fischer
thereagentsagainstmoistureintheairmustbewatchedclosely.Thesilica
gel must be changed as soon as there is evidence of color change in it.
Reagent Titration Method)
Care also must be taken to minimize the exposure of the sample and
3. Summary of Test Method solutions to atmospheric moisture during the determinations.
3.1 An excess of Karl Fischer reagent is added to the 4.2 Magnetic Stirrer, that can be used with the closed
specimen dissolved in the prescribed solvent. After reaction titration beaker with inert plastic-coated stirring bar.
with the water in the specimen, the excess Karl Fischer reagent 4.3 Pipet, automatic, 25-mL.
4.4 Pipet, weighing, or equivalent for weighing water, for
standardization of reagent.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
4.5 Electrometric Titrator of the “dead stop” type,
and Related Coatings, Materials, andApplications, and is the direct responsibility of
equipped with platinum electrodes. On operation a small
Subcommittee D01.32 on Drying Oils.
electrical potential is imposed across the electrodes.At the end
Current edition approved March 15, 1992. Published May 1992. Originally
e1
published as D 2072 – 65 T. Last previous edition D 2072 – 66 (1987) .
point there is a change in the flow of current due to the change
Annual Book of ASTM Standards, Vol 11.01.
in polarization of the electrodes.
Annual Book of ASTM Standards, Vol 06.04.
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D2072
5. Reagents N~L 2 M!
F 5 1 N (1)
25 1 M 2 L
5.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
where:
all reagents shall conform to the specifications of the Commit-
F 5 water per millilitre of water-methanol solution, mg,
tee onAnalytical Reagents of theAmerican Chemical Society,
L 5 water-methanol solution required for titration of 25
where such specifications are available. Other grades may be
mL of Karl Fischer reagent, mL,
used, provided it is first ascertained that the reagent is of
M 5 water-methanol solution required for titration of 25
sufficiently high purity to permit its use without lessening the
mL of Karl Fischer reagent plus 25 mL of absolute
accuracy of the determination.
methanol, mL, and
5.2 Purity of Water—Unless otherwise indicated, references N 5 water added per millilitre to the water-methanol
to water shall be understood to mean reagent water conforming solution described in 5.6, mg.
to Type II of Specification D 1193.
8. Procedure
5.3 Acetic Acid, Glacial (CH COOH). Warning—(see
6.2). 8.1 Melt the sample, if it is not already liquid, in a water
5.4 Karl Fischer Reagent—Suitable reagent is available bath. Mix thoroughly and weigh into a dry beaker 10 g of
from most chemical s
...