ASTM D5554-95(2006)

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 the standard. The values given in parentheses are for information only.
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-Mar-2006
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5554-95(2001) - Standard Test Method for Determination of the Iodine Value of Fats and Oils
• Effective Date: 01-Apr-2006
• Replaced By: ASTM D5554-95(2011) - 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-Apr-2006

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2006)
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 the
KMnO shall be added. The pink color shall not be entirely
standard. The values given in parentheses are for information
discharged within 2 h.
only.
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
3.8 Carbon Tetrachloride, A.C.S. grade.
of fats and oils and is expressed in terms of the number of
3.9 Hydrochloric Acid, A.C.S. grade, sp. gr. 1.19.
centigrams of iodine absorbed per gram of sample.
3.10 Soluble Starch, of suitable sensitivity.
3. Apparatus and Reagents
3.10.1 The test for starch sensitivity shall be made by
adding, while stirring, 200 mLof boiling water to a paste made
3.1 Glass-Stoppered Bottles or Wide Mouth Erlenmeyer
with1gof starch in a small amount of water. After placing 5
Flasks, 500 mL. Wide mouth bottles or flasks are essential if
mL of this solution in 100 mL of water, add 0.05 mL of 0.1 N
stirring is done by mechanical means.
iodine solution. The deep blue color produced must be dis-
3.2 Glass-Stoppered Volumetric Flasks, conforming to
charged by 0.05 mL of 0.1 N sodium thiosulfate.
NIST tolerances and accurately calibrated to contain 1000
3.11 Potassium Dichromate, A.C.S. grade, shall be finely
mL.
ground and dried to constant weight at about 110°C before
3.3 Pipette,20mL.
using. (A standard sample of potassium dichromate with a
3.4 Two Pipettes, 25 mL. One pipette is reserved for use
certificate of analysis may be obtained from NIST. This
with the standard potassium dichromate solution and shall
sample is strongly recommended as the primary standard for
conform to NIST tolerances and be calibrated to deliver 25
this test method. The dichromate should be treated as directed
mL.
in the certificate of analysis accompanying the sample.)
3.12 Sodium Thiosulfate—(Na S O ·5H O), A.C.S. grade.
2 2 3 2
This test method is under the jurisdiction ofASTM Committee D31 on Leather
3.13 Iodine, A.C.S. grade.
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
3.14 Potassium Iodide Solution, prepared by dissolving 150
method was developed in cooperation with the American Leather Chemists Assn.
g in distilled water and making up to 1 L.
(Method H 32-1957).
3.15 Starch Indicator Solution, shall be prepared by making
Current edition approved April 1, 2006. Published April 2006. Originally
approved in 1994. Last previous edition approved in 2001 as D5554 – 95(2001).
a homogeneous paste of 10 g of soluble starch in cold distilled
DOI: 10.1520/D5554-95R06.
water and adding to this 1 L of boiling distilled water with
Available from National Institute of Standards and Technology, (NIST),
rapid stirring; cool. Salicylic acid (1.25 g/L) shall be added to
Gaithersburg, MD 20899.
WijsSolution(IodineMonochlorideSolution)maybepurchasedcommercially. preserve the indicator. If long storage is required, the solution
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D5554–95 (2006)
TABLE 1 Guide for Selecting Sample Size
shall be kept in a refrigerator at 4 to 10°C (40 to 50°F). Fresh
indicator shall be prepared when the end-point of the titration Sample Weight, g
Weighing
Iodine Value
from blue to colorless fails to be sharp. Accuracy, g
100 % Excess 150 % Excess
3.16 Standard Potassium Dichromate Solution, 0.1 N, shall
<3 10 10 60.001
3 10.5760 8.4613 0.005
be prepared by dissolving 4.9035 g of finely ground and dried
5 6.3460 5.0770 0.0005
potassium dichromate in distilled water in the 1000 mL
10 3.1730 2.5384 0.0002
volumetric flask and making to volume at 25°C.
20 1.5865 0.8461 0.0002
40 0.7935 0.6346 0.0002
3.17 Sodium Thiosulfate Solutio
...