ASTM D5554-15
(Test Method)Standard Test Method for Determination of the Iodine Value of Fats and Oils
Standard Test Method for Determination of the Iodine Value of Fats and Oils
SIGNIFICANCE AND USE
2.1 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.
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Designation: D5554 − 15
Standard Test Method for
1
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 3.5.1 Two millilitres of the glacial acetic acid shall be
diluted with 10 mL of distilled water and 0.1 mL of 0.1 N
1.1 This test method covers the determination of the iodine
KMnO shall be added. The pink color shall not be entirely
4
value of fats and oils.
discharged within 2 h.
1.2 The values stated in SI units are to be regarded as
3.6 Potassium Iodide, A.C.S. grade.
standard. No other units of measurement are included in this
standard. 3.7 Chlorine, 99.8 %. Satisfactory commercial grades are
available in cylinders, but this gas must be dried by passing
1.3 This standard does not purport to address all of the
through sulfuric acid (sp. gr. 1.84) before introducing into the
safety concerns, if any, associated with its use. It is the
iodine solution.
responsibility of the user of this standard to establish appro-
3.7.1 Chlorine may be prepared by allowing hydrochloric
priate safety and health practices and determine the applica-
acid (sp. gr. 1.19) to drop onto potassium permanganate or on
bility of regulatory limitations prior to use.
a mixture of potassium permanganate and manganese dioxide.
2. Significance and Use The gas thus generated shall be led through a glass tube into
sulfuric acid (sp. gr. 1.84) and then into the iodine solution.
2.1 This test method is intended for the determination of the
iodine value of fats and oils that do not contain conjugated 3.8 Carbon Tetrachloride, A.C.S. grade. (Warning—
doublebonds.Theiodinevalueisameasureoftheunsaturation Carbon Tetrachloride is a known carcinogen. It is toxic by
of fats and oils and is expressed in terms of the number of inhalation, ingestion and skin absorption. Always handle Car-
centigrams of iodine absorbed per gram of sample. bon Tetrachloride inside a fume hood. Use only with adequate
ventilation.
3. Apparatus and Reagents
3
3.9 Cyclohexane , A.C.S. grade.
3.1 Glass-Stoppered Bottles or Wide Mouth Erlenmeyer
3.10 ReagentforDilutingSample—Prepare by mixing fresh
Flasks, 500 mL. Wide mouth bottles or flasks are essential if
cyclohexane and glacial acetic acid, 1:1, v/v. (After mixing,
stirring is done by mechanical means.
verify the absence of oxidizable matter in the reagent by
3.2 Glass-Stoppered Volumetric Flasks, conforming to
shaking 10 mL of the reagent with 1 mL of saturated aqueous
2
NIST tolerances and accurately calibrated to contain 1000
potassium dichromate solution and 2 mL of concentrated
mL.
sulfuric acid: no green coloration should appear. A green
coloration indicates presence of oxidizable matter, so discard
3.3 Pipette, 20 mL.
and remix using fresh cyclohexane.)
3.4 Two Pipettes, 25 mL. One pipette is reserved for use
3.11 Hydrochloric Acid, A.C.S. grade, sp. gr. 1.19.
with the standard potassium dichromate solution and shall
2
conform to NIST tolerances and be calibrated to deliver 25
3.12 Soluble Starch, of suitable sensitivity.
mL.
3.12.1 The test for starch sensitivity shall be made by
adding, while stirring, 200 mLof boiling water to a paste made
3.5 Glacial Acetic Acid, A.C.S. grade. The permanganate
with1gof starch in a small amount of water. After placing 5
test shall be applied to be sure that this specification is met.
mL of this solution in 100 mL of water, add 0.05 mL of 0.1 N
iodine solution. The deep blue color produced must be dis-
1
This test method is under the jurisdiction ofASTM Committee D31 on Leather
charged by 0.05 mL of 0.1 N sodium thiosulfate.
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
method was developed in cooperation with the American Leather Chemists Assn.
3.13 Potassium Dichromate, A.C.S. grade, shall be finely
(Method H 32-1957).
ground and dried to constant weight at about 110°C before
Current edition approved Sept. 1, 2015. Published October 2015. Originally
approved in 1994. Last previous edition approved in 2011 as D5554 – 95(2011).
DOI: 10.1520/D5554-15.
2 3
Available from National Institute of Standards and Technology, (NIST), Comparison study showed excellent agreement between Carbon Tetrachloride
Gaithersburg, MD 20899. and Cyclohexane (ISO/IUPAP Smalley program).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5554 − 15
using. (A standard sample of potassium dichromate with a 4. Procedure
2
certifi
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5554 − 95 (Reapproved 2011) D5554 − 15
Standard Test Method for
1
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
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.
2. Significance and Use
2.1 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.
3. Apparatus and Reagents
3.1 Glass-Stoppered Bottles or Wide Mouth Erlenmeyer Flasks, 500 mL. Wide mouth bottles or flasks are essential if stirring
is done by mechanical means.
2
3.2 Glass-Stoppered Volumetric Flasks, conforming to NIST tolerances and accurately calibrated to contain 1000 mL.
3.3 Pipette, 20 mL.
3.4 Two Pipettes, 25 mL. One pipette is reserved for use with the standard potassium dichromate solution and shall conform
2
to NIST tolerances and be calibrated to deliver 25 mL.
3.5 Glacial Acetic Acid, A.C.S. grade. The permanganate test shall be applied to be sure that this specification is met.
3.5.1 Two millilitres of the glacial acetic acid shall be diluted with 10 mL of distilled water and 0.1 mL of 0.1 N KMnO shall
4
be added. The pink color shall not be entirely discharged within 2 h.
3.6 Potassium Iodide, A.C.S. grade.
3.7 Chlorine, 99.8 %. Satisfactory commercial grades are available in cylinders, but this gas must be dried by passing through
sulfuric acid (sp. gr. 1.84) before introducing into the iodine solution.
3.7.1 Chlorine may be prepared by allowing hydrochloric acid (sp. gr. 1.19) to drop onto potassium permanganate or on a
mixture of potassium permanganate and manganese dioxide. The gas thus generated shall be led through a glass tube into sulfuric
acid (sp. gr. 1.84) and then into the iodine solution.
3.8 Carbon Tetrachloride, A.C.S. grade. (Warning—Carbon Tetrachloride is a known carcinogen. It is toxic by inhalation,
ingestion and skin absorption. Always handle Carbon Tetrachloride inside a fume hood. Use only with adequate ventilation.
3
3.9 Cyclohexane , A.C.S. grade.
3.10 Reagent for Diluting Sample—Prepare by mixing fresh cyclohexane and glacial acetic acid, 1:1, v/v. (After mixing, verify
the absence of oxidizable matter in the reagent by shaking 10 mL of the reagent with 1 mL of saturated aqueous potassium
1
This test method is under the jurisdiction of ASTM Committee D31 on Leather and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test method
was developed in cooperation with the American Leather Chemists Assn. (Method H 32-1957).
Current edition approved Jan. 1, 2011Sept. 1, 2015. Published March 2011October 2015. Originally approved in 1994. Last previous edition approved in 20062011 as
D5554 – 95(2006).(2011). DOI: 10.1520/D5554-95R11.10.1520/D5554-15.
2
Available from National Institute of Standards and Technology, (NIST), Gaithersburg, MD 20899.
3
Comparison study showed excellent agreement between Carbon Tetrachloride and Cyclohexane (ISO/IUPAP Smalley program).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5554 − 15
dichromate solution and 2 mL of concentrated sulfuric acid: no green coloration should appear. A green coloration indicates
presence of oxidizable matter, so discard and remix using fresh cyclohexane.)
3.11 Hydrochloric Acid, A.C.S. grade, sp. gr. 1.19.
3.12 Soluble Starch, of suitable sensitivity.
3.12.1 The test for starch sensitivity shall be made by adding, while stirring, 200 mL of boiling water to a paste made with 1
g of starch in a small amount of water. Afte
...
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