ASTM D1957-86(2001)

Standard Test Method for Hydroxyl Value of Fatty Oils and Acids (Withdrawn 2007)

SCOPE
1.1 This test method covers the determination of the hydroxyl content of castor oil, dehydrated castor oil, and their derivatives. This test method may also be used for other fatty products such as fatty alcohols, mono- and diglycerides, and hydroxystearic acid, but the precision will not necessarily be as indicated.  
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 whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 6.
WITHDRAWN RATIONALE
This test method covers the determination of the hydroxyl content of castor oil, dehydrated castor oil, and their derivatives. This test method may also be used for other fatty products such as fatty alcohols, mono- and diglycerides, and hydroxystearic acid, but the precision will not necessarily be as indicated.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in February 2007. This standard is being withdrawn without replacement due to its limited use by industry.

General Information

• Status: Withdrawn
• Publication Date: 26-Mar-1986
• Withdrawal Date: 01-Mar-2007
• ICS: 87.060.20 - Binders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications

Relations

• Replaces: ASTM D1957-86(1995)e1 - Standard Test Method for Hydroxyl Value of Fatty Oils and Acids
• Effective Date: 27-Mar-1986
• Referred By: ASTM E222-23 - Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation
• Effective Date: 27-Mar-1986

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1957–86(Reapproved2001)
Standard Test Method for
Hydroxyl Value of Fatty Oils and Acids
This standard is issued under the fixed designation D 1957; 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 4.2 Condensers, straight-tube, Liebig type, having standard
ground-glass joints.
1.1 This test method covers the determination of the hy-
droxyl content of castor oil, dehydrated castor oil, and their
5. Reagents
derivatives. This test method may also be used for other fatty
5.1 Purity of Reagents—Reagent grade chemicals shall be
products such as fatty alcohols, mono- and diglycerides, and
used in all tests. Unless otherwise indicated, it is intended that
hydroxystearic acid, but the precision will not necessarily be as
all reagents shall conform to the Specifications of the Com-
indicated.
mittee on Analytical Reagents of the American Chemical
1.2 This standard does not purport to address all of the
Society, where such specifications are available. Other grades
safety concerns, if any, associated with its use. It is the
may be used provided it is first ascertained that the reagent is
responsibility of whoever uses this standard to consult and
of sufficiently high purity to permit its use without lessening
establish appropriate safety and health practices and deter-
the accuracy of the determination.
mine the applicability of regulatory limitations prior to use.
5.2 Purity of Water—Unless otherwise indicated, references
Specific hazard statements are given in Section 6.
to water shall be understood to mean reagent water conforming
2. Referenced Documents to Type I of Specification D 1193.
5.3 Acetic Anhydride,(Warning—See 6.5) fresh.
2.1 ASTM Standards:
2 5.4 n-Butyl Alcohol (Warning—See 6.1), neutralized with
D 1193 Specification for Reagent Water
0.5 N alcoholic potassium hydroxide (KOH) solution to a faint
3. Significance and Use pink phenolphthalein end point.
5.5 Ethyl Alcohol or Denatured Alcohol, conforming to
3.1 Hydroxyl value is important in establishing reactivity
FormulaNo.3Aor30oftheU.S.BureauofAlcohol,Tobacco,
with acids and isocyanates. It is also a measure of the degree of
and Firearms. Formula No. 3A is a mixture of 100 parts by
dehydration of castor oil.
volume of ethanol to 5 parts by volume of methanol. Formula
3.2 This test method determines the total amount of residual
30 is 100 parts by volume of ethanol and 10 parts by volume
hydroxyl groups present in oils and other fatty acid-containing
of methanol.
materials, reported as hydroxyl value.
5.6 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
3.3 This test method involves the acetylation of hydroxyl-
1 g of phenolphthalein in methanol, ethanol, or isopropanol,
containing fatty oils and acids using pyridine as solvent. Other
and dilute to 100 mL.
groups that will react with acetic anhydride such as primary
5.7 Potassium Hydroxide, Alcoholic Solution (0.5 N)
and secondary amines under the conditions of the method will
(Warning—See 6.3)—Prepare and standardize a 0.5 N solu-
be reported as hydroxyl. The hydroxyl value is expressed as
tion of potassium hydroxide (KOH) in ethanol. The strength
milligrams of potassium hydroxide equivalent to the hydroxyl
should be not less than 0.5 N in order that the blank titrations
content of1gofthe oil.Acorrection is applied for acid groups
will take less than 50 mL to avoid refilling the buret.
present.
5.8 Pyridine (Warning—See 6.4), distilled at 114 to
4. Apparatus
115°C.
4.1 Erlenmeyer Flask, 250-mL, standard ground-glass-
stoppered.
1 3
This test method is under the jurisdiction of ASTM Committee D01 on Paint Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, andApplications and is the direct responsibility of Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Subcommittee D01.32 on Drying Oils. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved March 27, 1986. Published May 1986. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 1957 – 61 T. Last previous edition D 1957 – 63 (1984). and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1957–86 (2001)
5.9 Pyridine-AceticAnhydride Solution (3 + 1)—Mix3vol- 7.4 Insert reflux condensers into the Erlenmeyer flasks.
umes of pyridine with 1 volume of acetic anhydride. Prepare Place the flasks on an opening of a steam bath and heat for 1
fresh before using. h. By this method of heating only slight, if any, refluxing will
occur.
6. Hazards
7.5 Add 10 mL of water through the condensers to the
6.1 n-Butyl Alcoh
...