ASTM D5554-95(2011)

Standard Test Method for Determination of the Iodine Value of Fats and Oils

SIGNIFICANCE AND USE
This test method is intended for the determination of the iodine value of fats and oils that do not contain conjugated double bonds. The iodine value is a measure of the unsaturation of fats and oils and is expressed in terms of the number of centigrams of iodine absorbed per gram of sample.
SCOPE
1.1 This test method covers the determination of the iodine value of fats and oils.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.

General Information

• Status: Historical
• Publication Date: 31-Dec-2010
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5554-95(2006) - Standard Test Method for Determination of the Iodine Value of Fats and Oils
• Effective Date: 01-Jan-2011
• Referred By: ASTM D2414-23 - Standard Test Method for Carbon Black—Oil Absorption Number (OAN)
• Effective Date: 01-Jan-2011

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5554 − 95(Reapproved 2011)
Standard Test Method for
Determination of the Iodine Value of Fats and Oils
This standard is issued under the fixed designation D5554; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3.5 Glacial Acetic Acid, A.C.S. grade. The permanganate
test shall be applied to be sure that this specification is met.
1.1 This test method covers the determination of the iodine
3.5.1 Two millilitres of the glacial acetic acid shall be
value of fats and oils.
diluted with 10 mL of distilled water and 0.1 mL of 0.1 N
1.2 The values stated in SI units are to be regarded as
KMnO shall be added. The pink color shall not be entirely
standard. No other units of measurement are included in this
discharged within 2 h.
standard.
3.6 Potassium Iodide, A.C.S. grade.
1.3 This standard does not purport to address all of the
3.7 Chlorine, 99.8 %. Satisfactory commercial grades are
safety concerns, if any, associated with its use. It is the
available in cylinders, but this gas must be dried by passing
responsibility of the user of this standard to establish appro-
through sulfuric acid (sp. gr. 1.84) before introducing into the
priate safety and health practices and determine the applica-
iodine solution.
bility of regulatory limitations prior to use.
3.7.1 Chlorine may be prepared by allowing hydrochloric
2. Significance and Use
acid (sp. gr. 1.19) to drop onto potassium permanganate or on
a mixture of potassium permanganate and manganese dioxide.
2.1 This test method is intended for the determination of the
The gas thus generated shall be led through a glass tube into
iodine value of fats and oils that do not contain conjugated
sulfuric acid (sp. gr. 1.84) and then into the iodine solution.
doublebonds.Theiodinevalueisameasureoftheunsaturation
of fats and oils and is expressed in terms of the number of
3.8 Carbon Tetrachloride, A.C.S. grade.
centigrams of iodine absorbed per gram of sample.
3.9 Hydrochloric Acid, A.C.S. grade, sp. gr. 1.19.
3. Apparatus and Reagents
3.10 Soluble Starch, of suitable sensitivity.
3.10.1 The test for starch sensitivity shall be made by
3.1 Glass-Stoppered Bottles or Wide Mouth Erlenmeyer
adding, while stirring, 200 mLof boiling water to a paste made
Flasks, 500 mL. Wide mouth bottles or flasks are essential if
with1gof starch in a small amount of water. After placing 5
stirring is done by mechanical means.
mL of this solution in 100 mL of water, add 0.05 mL of 0.1 N
3.2 Glass-Stoppered Volumetric Flasks, conforming to
iodine solution. The deep blue color produced must be dis-
NIST tolerances and accurately calibrated to contain 1000
charged by 0.05 mL of 0.1 N sodium thiosulfate.
mL.
3.11 Potassium Dichromate, A.C.S. grade, shall be finely
3.3 Pipette, 20 mL.
ground and dried to constant weight at about 110°C before
3.4 Two Pipettes, 25 mL. One pipette is reserved for use
using. (A standard sample of potassium dichromate with a
with the standard potassium dichromate solution and shall
certificate of analysis may be obtained from NIST. This
conform to NIST tolerances and be calibrated to deliver 25
sample is strongly recommended as the primary standard for
mL.
this test method. The dichromate should be treated as directed
in the certificate of analysis accompanying the sample.)
3.12 Sodium Thiosulfate—(Na S O ·5H O), A.C.S. grade.
1 2 2 3 2
This test method is under the jurisdiction ofASTM Committee D31 on Leather
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
3.13 Iodine, A.C.S. grade.
method was developed in cooperation with the American Leather Chemists Assn.
(Method H 32-1957).
3.14 Potassium Iodide Solution, prepared by dissolving 150
Current edition approved Jan. 1, 2011. Published March 2011. Originally
g in distilled water and making up to 1 L.
approved in 1994. Last previous edition approved in 2006 as D5554 – 95(2006).
DOI: 10.1520/D5554-95R11.
3.15 StarchIndicatorSolution, shall be prepared by making
Available from National Institute of Standards and Technology, (NIST),
a homogeneous paste of 10 g of soluble starch in cold distilled
Gaithersburg, MD 20899.
water and adding to this 1 L of boiling distilled water with
WijsSolution(IodineMonochlorideSolution)maybepurchasedcommercially.
rapid stirring; cool. Salicylic acid (1.25 g/L) shall be added to
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D5554 − 95 (2011)
TABLE 1 Guide for Selecting Sample Size
preserve the indicator. If long storage is required, the solution
shall be kept in a refrigerator at 4 to 10°C (40 to 50°F). Fresh Sample Weight, g
Weighing
Iodine Value
Accuracy, g
indicator shall be prepared when the end-point of the titration 100 % Excess 150 % Excess
from blue to colorless fails to be sharp. <3 10 10 ±0.001
3 10.5760 8.4613 0.005
3.16 Standard Potassium Dichromate Solution, 0.1 N, shall
5 6.3460 5.0770 0.0005
10 3.1730 2.5384 0.0002
be prepared by dissolving 4.9035 g of finely ground and dried
20 1.5865 0.8461 0.0002
potassium dichromate in distilled water in the 1000 mL
40 0.7935 0.6346 0.0002
volumetric flask and making to volume at 25°C.
60 0.5288 0.4231 0.0002
80 0.3966 0.3173 0.0001
3.17 Sodium Thiosulfate Solution, 0.1 N,
...