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

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
14-May-1995
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM D5554-95 - Standard Test Method for Determination of the Iodine Value of Fats and Oils
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5554 – 95
Standard Test Method for
Determination of the Iodine Value of Fats and Oils
This standard is issued under the fixed designation D 5554; 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.
1. Scope 3.6 Potassium Iodide, A.C.S. grade.
3.7 Chlorine, 99.8 %. Satisfactory commercial grades are
1.1 This test method covers the determination of the iodine
available in cylinders, but this gas must be dried by passing
value of fats and oils.
through sulfuric acid (sp. gr. 1.84) before introducing into the
1.2 The values stated in SI units are to be regarded as the
iodine solution.
standard. The values given in parentheses are for information
3.7.1 Chlorine may be prepared by allowing hydrochloric
only.
acid (sp. gr. 1.19) to drop onto potassium permanganate or on
1.3 This standard does not purport to address all of the
a mixture of potassium permanganate and manganese dioxide.
safety concerns, if any, associated with its use. It is the
The gas thus generated shall be led through a glass tube into
responsibility of the user of this standard to establish appro-
sulfuric acid (sp. gr. 1.84) and then into the iodine solution.
priate safety and health practices and determine the applica-
3.8 Carbon Tetrachloride, A.C.S. grade.
bility of regulatory limitations prior to use.
3.9 Hydrochloric Acid, A.C.S. grade, sp. gr. 1.19.
2. Significance and Use
3.10 Soluble Starch, of suitable sensitivity.
3.10.1 The test for starch sensitivity shall be made by
2.1 This test method is intended for the determination of the
adding, while stirring, 200 mL of boiling water to a paste made
iodine value of fats and oils that do not contain conjugated
with1gof starch in a small amount of water. After placing 5
double bonds. The iodine value is a measure of the unsaturation
mL of this solution in 100 mL of water, add 0.05 mL of 0.1 N
of fats and oils and is expressed in terms of the number of
iodine solution. The deep blue color produced must be dis-
centigrams of iodine absorbed per gram of sample.
charged by 0.05 mL of 0.1 N sodium thiosulfate.
3. Apparatus and Reagents
3.11 Potassium Dichromate, A.C.S. grade, shall be finely
ground and dried to constant weight at about 110°C before
3.1 Glass-Stoppered Bottles or Wide Mouth Erlenmeyer
using. (A standard sample of potassium dichromate with a
Flasks, 500 mL. Wide mouth bottles or flasks are essential if
certificate of analysis may be obtained from NIST. This
stirring is done by mechanical means.
sample is strongly recommended as the primary standard for
3.2 Glass-Stoppered Volumetric Flasks, conforming to
this test method. The dichromate should be treated as directed
NIST tolerances and accurately calibrated to contain 1000
in the certificate of analysis accompanying the sample.)
mL.
3.12 Sodium Thiosulfate—(Na S O ·5H O), A.C.S. grade.
3.3 Pipette,20mL. 2 2 3 2
3.13 Iodine, A.C.S. grade.
3.4 Two Pipettes, 25 mL. One pipette is reserved for use
3.14 Potassium Iodide Solution, prepared by dissolving 150
with the standard potassium dichromate solution and shall
g in distilled water and making up to 1 L.
conform to NIST tolerances and be calibrated to deliver 25
3.15 Starch Indicator Solution, shall be prepared by making
mL.
a homogeneous paste of 10 g of soluble starch in cold distilled
3.5 Glacial Acetic Acid, A.C.S. grade. The permanganate
water and adding to this 1 L of boiling distilled water with
test shall be applied to be sure that this specification is met.
rapid stirring; cool. Salicylic acid (1.25 g/L) shall be added to
3.5.1 Two millilitres of the glacial acetic acid shall be
preserve the indicator. If long storage is required, the solution
diluted with 10 mL of distilled water and 0.1 mL of 0.1 N
shall be kept in a refrigerator at 4 to 10°C (40 to 50°F). Fresh
KMnO shall be added. The pink color shall not be entirely
indicator shall be prepared when the end-point of the titration
discharged within 2 h.
from blue to colorless fails to be sharp.
3.16 Standard Potassium Dichromate Solution, 0.1 N, shall
This test method is under the jurisdiction of ASTM Committee D-31 on Leather
be prepared by dissolving 4.9035 g of finely ground and dried
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.
potassium dichromate in distilled water in the 1000 mL
(Method H 32-1957).
volumetric flask and making to volume at 25°C.
Current edition approved May 15, 1995. Published July 1995. Originally
3.17 Sodium Thiosulfate Solution, 0.1 N, prepared by dis-
published as D 5554 – 94. Last previous edition D 5554 – 94.
solving 24.8 g of sodium thiosulfate in distilled water and
Available from National Institute of Standards and Technology, (NIST),
Gaithersburg, MD 20899.
diluting to 1 L.
Wijs Solution (Iodine Monochloride Solution) may be purchased commercially.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5554
TABLE 1 Guide for Selecting Sample Size
3.17.1 Standardization of the Thiosulfate—Pipette 25 mL of
the standard dichromate solution into Erlenmeyer flask or Sample Weight, g
Weighing
Iodine Value
bottle. Add 5 mL of hydroch
...

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