ASTM D2075-92(1998)

Standard Test Method for Iodine Value of Fatty Amines, Amidoamines, and Diamines (Withdrawn 2007)

SCOPE
1.1 This test method (Note 1) covers the determination of the iodine value of fatty amines, diamines, and amidoamines by the Wijs procedure.  Note 1-This test method is essentially equivalent to Test Methods D2078 and D1959. Use of mercuric acetate permits reduced reaction time compared to Test Methods D2078 (30 min) and D1959 (1 h).
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.>
WITHDRAWN RATIONALE
This test method covers the determination of the iodine value of fatty amines, diamines, and amidoamines by the Wijs procedure. This test method is essentially equivalent to Test Methods D 2078 and D 1959. Use of mercuric acetate permits reduced reaction time compared to Test Methods D 2078 (30 min) and D 1959 (1 h).
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the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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• Status: Withdrawn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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:D2075–92(Reapproved1998)
Standard Test Method for
Iodine Value of Fatty Amines, Amidoamines, and Diamines
This standard is issued under the fixed designation D 2075; 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 method was prepared jointly by the American Society for Testing and Materials and the American Oil Chemists’ Society.
1. Scope 4.2 Where no conjugated double bonds are present, the
iodine value obtained is a measure of the total unsaturation,
1.1 This test method (Note 1) covers the determination of
and the values obtained are useful for comparative purposes.
the iodine value of fatty amines, diamines, and amidoamines
4.3 If conjugated unsaturation is known to be present, use
by the Wijs procedure.
Test Method D 1541.
NOTE 1—This test method is essentially equivalent to Test Methods
D 2078 and D 1959. Use of mercuric acetate permits reduced reaction
5. Apparatus
time compared to Test Methods D 2078 (30 min) and D 1959 (1 h).
5.1 Bottles—Glass-stoppered bottles or wide-mouth Erlen-
1.2 This standard does not purport to address all of the
meyer flasks of 500-mL capacity.
safety concerns, if any, associated with its use. It is the
NOTE 2—Wide-mouth bottles or flasks are essential if stirring is done
responsibility of the user of this standard to establish appro-
by mechanical means.
priate safety and health practices and determine the applica-
5.2 Pipets, 20 and 25-mL capacity.
bility of regulatory limitations prior to use.
6. Reagents
2. Referenced Documents
6.1 Purity of Reagents—Reagent grade chemicals shall be
2.1 ASTM Standards:
used in all tests. Unless otherwise indicated, it is intended that
D 1193 Specification for Reagent Water
all reagents shall conform to the specifications of the Commit-
D 1541 Test Method for Total Iodine Value of Drying Oils
tee onAnalytical Reagents of theAmerican Chemical Society,
and Their Derivatives
where such specifications are available. Other grades may be
D 1959 Test Method for Iodine Value of Drying Oils and
used, provided it is first ascertained that the reagent is of
Fatty Acids
sufficiently high purity to permit its use without lessening the
D 2078 Test Method for Iodine Value of Fatty Quaternary
accuracy of the determination.
Ammonium Chlorides
6.2 Purity of Water—Unless otherwise indicated, references
3. Terminology
to water shall be understood to mean reagent water conforming
to Type II of Specification D 1193.
3.1 Definition:
6.3 Acetic Acid (Glacial)—Verify the absence of sub-
3.1.1 iodine value—a measure of the unsaturation of the
stances reducing permanganate as follows: Dilute 2 mL of the
alkyl group or groups, expressed in terms of percent iodine
acid with 10 mL of water and add 0.1 mL of 0.1 N potassium
absorbed.
permanganate (KMnO ) solution.The pink color should not be
4. Significance and Use
entirely discharged at the end of 2 h.
6.4 Chlorine (99.8 % Cl)—Commercial grades of chlorine
4.1 This test method measures the unsaturation of the alkyl
availableincylindersmaybeused,providedthegasisdriedby
groups as iodine value by addition of an iodine/chlorine
reagent.
Reagent Chemicals, American Chemical Society Specifications, American
This method is under the jurisdiction of ASTM Committee D-1 on Paint and Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Related Coatings, Materials, and Applications and is the direct responsibility of listed by the American Chemical Society, see Analar Standards for Laboratory
Subcommittee D01.32 on Drying Oils. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved March 15, 1992. Published May 1992. Originally and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
published as D 2075 – 62. Last previous edition D 2075 – 89. MD.
2 5
Annual Book of ASTM Standards, Vol 11.01. “Analytical reagents, ACS Specifications,” Am. Chemical Soc., Washington,
Annual Book of ASTM Standards, Vol 06.03. DC, 1950.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2075–92 (1998)
passing through concentrated sulfuric acid (H SO , sp gr 1.84) gas into the iodine solution until the original titration is not
2 4
before passing it into the iodine solution (see 6.10). Alterna- quite doubled. A characteristic color change takes place in the
tively, the chlorine may be prepared by allowing concentrated Wijs solution when the desired amount of chlorine has been
hydrochloric acid (HCl, sp gr 1.19) to drop onto potassium added; this may be used to assist in judging the end point. A
permanganate (KMnO ) or onto a mixture of KMnO and
convenient procedure is to add a small excess of chlorine and
4 4
manganese dioxide (MnO ). Dry the gas thus generated by bring back to the desired titration by addition of some of the
passing it through H SO (sp gr 1.84).
original iodine solution that was taken out at the beginning.
2 4
6.5 Chloroform. Determine the strength of the original iodine solution and the
6.6 Mercuric Acetate Solution—Dissolve 2.5 g of mercuric
finished Wijs solution by titration against 0.1 N Na S O
2 2 3
acetate (Hg (C H O ) ) in glacial acetic acid (CH COOH) and
solution, as directed in 7.6 and 7.7.
2 3 2 2 3
make up to 100 mL.
NOTE 3—Iodine monochloride (Wijs solution) can be purchased com-
6.7 Potassium Iodide Solution(150g/L)—Dissolve150gof
merciallyfromvariouslaboratorysupplyhouses.Thehalogenratioshould
potassium iodide (KI) in water and dilute to 1 L.
be checked prior to use. The halogen ratio, that is, the ratio of iodine to
6.8 Sodium Thiosulfate, Standard Solution (0.1 N)— 7
chlorine, can be determined by the Lopez Method, as follows:
Dissolve 24.8 g of sodium thiosulfate (Na S O ·5H O) in
2 2 3 2 (1) Iodine Content—Pour 150 mL of saturated chlorine water into a
water and dilute to 1 L. Standardize against potassium dichro-
500-mL Erlenmeyer flask and add some glass beads. Pipet 5 mL of Wijs
solution into the flask containing the saturated chlorine water. Shake and
mate (K Cr O ) as follows: Weigh to the nearest 0.1 mg, by
2 2 7
heat to boiling. Boil briskly for 10 min, cool, and add 30 mL of 2 %
difference from a weighing bottle, 0.16 to 0.22 g of K Cr O
2 2 7
sulfuric acid (H SO ) and 15 mL of KI solution. Mix well and titrate
2 4
that has been finely ground and then dried to constant weight
immediately with 0.1 N sodium thiosulfate (Na S O ) solution to a starch
2 2 3
at 110°C prior to use. Place the K Cr O i
...