7/27/2019 ASTM D 1467 89 (Reapproved 1995) Fatty Acids Used in Protective Coatings

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Designation: D 1467 89 (Reapproved 1995)e1

Standard Guide for TestingFatty Acids Used in Protective Coatings1

This standard is issued under the fixed designation D 1467; 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.

e1 NOTEKeywords were added editorially in May 1995.

1. Scope

1.1 This guide covers the selection and application of

procedures for testing fatty acids such as cottonseed, linseed,

soybean, dehydrated castor, tall oil, etc. used in protective

coatings.

1.2 The test methods included are listed as follows:

Test Method SectionASTM

Test Method

Acid Value 4 D 1980

Appearance 13 D 1544Ash 9 D 1951

Clarity 13 D 2090

Color:

GardnerPlatinum-Cobalt

1414

D 1544D 1209

Color Change After Heating 6 D 1981

Fatty Acid Composition 12 D 1983

Hydroxyl Value 10 D 1957

Rosin Acids 11 D 1240

Sampling 3 D 1466

Saponification Value 7 D 1962

Titer 15 D 1982

Unsaponifiable Matter 8 D 1965

Unsaturation:

Diene Value

Iodine Value

5

5

D 1358

D 1959

1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is the

responsibility of the user of this standard to establish appro-

priate safety and health practices and determine the applica-

bility of regulatory limitations prior to use.

2. Referenced Documents

2.1 ASTM Standards:

D 1209 Test Method for Color of Clear Liquids (Platinum-

Cobalt Scale)2

D 1240 Test Method for Rosin Acids Content of Naval

Stores, Including Rosin, Tall Oil and Related Products3

D 1358 Test Methods for Spectrophotometric Diene Value

of Dehydrated Castor Oil and Its Derivatives3

D 1466 Test Method for Sampling Liquid Oils and Fatty

Acids Commonly Used in Paints, Varnishes, and Related

Materials3

D 1541 Test Method for Total Iodine Value of Drying Oils

and Their Derivatives3

D 1544 Test Method for Color of Transparent Liquids

(Gardner Color Scale)4

D 1951 Test Method for Ash in Drying Oils and Fatty

Acids3

D 1957 Test Method for Hydroxyl Value of Fatty Oils and

Acids3

D 1959 Test Method for Iodine Value of Drying Oils and

Fatty Acids3

D 1962 Test Method for Saponification Value of Drying

Oils, Fatty Acids, and Polymerized Fatty Acids3

D 1965 Test Method for Unsaponifiable Matter in Drying

Oils, Fatty Acids and Polymerized Fatty Acids3

D 1980 Test Method for Acid Value of Fatty Acids and

Polymerized Fatty Acids3

D 1981 Test Method for Measuring Color After Heating of

Fatty Acids3

D 1982 Test Method for Titer of Fatty Acids3

D 1983 Test Method for Fatty Acid Composition by Gas-

Liquid Chromatography of Methyl Esters3

D 2090 Test Method for Clarity and Cleanness of Paint and

Ink Liquids3

D 3457 Test Method for Preparation of Methyl Esters from

Fatty Acids for Determination of Fatty Acid Composition

by Gas-Liquid Chromatography3

2.2 American Oil Chemists Society (AOCS) Methods:5

Tj-1a Polyunsaturated Acids

Cc-13b Color, Wesson Method (Lovibond)

Td-2a Photometric Index

3. Sampling

3.1 Sample the material in accordance with Test Method

D 1466.

3.2 Fatty acids are frequently solid at room temperature and

shall be completely liquified and blended prior to testing.

Temperatures during liquefying of the fatty acids should not

exceed 10 to 15C above the melting point of the sample.1 These methods are under the jurisdiction of ASTM Committee D-1 on Paint

and Related Coatings, Materials, and Applications and are the direct responsibility

of Subcommittee D01.32 on Drying Oils.

Current edition approved March 31, 1989. Published May 1989. Originally

published as D 1467 57 T. Last previous edition D 1467 72 (1981)e1.2 Annual Book of ASTM Standards, Vol 06.04.3 Annual Book of ASTM Standards, Vol 06.03.

4 Annual Book of ASTM Standards, Vol 06.01.5 Available from American Oil Chemists Society, 508 S. 6th St., Champlain, IL

61820.

1

AMERICAN SOCIETY FOR TESTING AND MATERIALS

100 Barr Harbor Dr., West Conshohocken, PA 19428

Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

7/27/2019 ASTM D 1467 89 (Reapproved 1995) Fatty Acids Used in Protective Coatings

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3.3 Samples should be stored preferably in the dark, in full

glass containers. Partially filled containers should be filled with

inert gas or carbon dioxide to prevent oxidation.

4. Acid Value

4.1 Acid value is a measure of the quantity of free fatty

acids and is defined as the number of milligrams of potassium

hydroxide required to neutralize the fatty acids in 1 g of

sample. Acid value determination is useful in establishing theidentity and purity of a fatty acid.

4.2 Determine the acid value in accordance with Test

Method D 1980 which is the referee method. Other solvents

should be checked out carefully before using for control

purposes.

5. Unsaturation

5.1 Iodine value is a convenient test for expressing the

degree of unsaturation of a fatty acid. Iodine value is the

weight percent of iodine absorbed.

5.2 Determine the iodine value in accordance with Test

Method D 1959 which gives fairly good accuracy and preci-

sion (Note 1) when applied to normal fatty acids. When TestMethod D 1959 is applied to fatty acids containing conjugated

double bonds such as dehydrated castor or tung an empirical

figure is obtained giving only a relative measure of the total

unsaturation. Refer to Test Method D 1541 for a more accurate

procedure for the determination of the total unsaturation of

tung oil acids. When Test Method D 1959 is used for dehy-

drated castor acids, a specimen weight of 0.11 to 0.13 g of fatty

acids must be used to get comparative results between labora-

tories.

NOTE 1The analyst is cautioned to follow the test method exactly as

written since small deviations in sample size, reagents, and time of

reaction will definitely affect the accuracy and precision of the test

method.

5.3 When Test Methods D 1358 is applied to dehydrated

castor acids an empirical value is also obtained due to the high

linoleic acid content. In this method the conjugated diene

content is derived from spectrophotometric measurements.

Determine the amount of conjugated diene content of fatty

acids in accordance with Test Methods D 1358, noting the

empirical nature of the result for dehydrated castor acids.

5.4 The iodine value of tall oil fatty acids containing

appreciable amounts of rosin acids is not a reliable measure of

the fatty acid unsaturation because of the unsaturation of the

rosin acids.

6. Color Change After Heating

6.1 The color stability of fatty acids when subjected toelevated temperatures is of importance to many commercial

users of fatty acids. The conditions under which the color

stability is determined such as temperature, time of heating,

time of upheat, exposure to air, etc, all affect the final results.

6.2 Measure the color of fatty acids after heating by Test

Method D 1981, which is applicable to all normal fatty acids.

It has been shown to have good precision within and between

laboratories and should be used as the referee test method.

7. Saponification Value

7.1 Saponification value is a measure of the alkali-reactive

groups in fatty acids and is expressed as the number of

milligrams of potassium hydroxide that will react with 1 g of

sample. The saponification value on a good grade of vegetable

fatty acids is normally only 1 or 2 points above the acid value

as determined in accordance with Test Method D 1980. The

difference between the saponification value and the acid value

is frequently referred to as the ester value. Saponification value

can be used to calculate the average molecular weight of thefatty acid.

7.2 Determine the saponification value in accordance with

Test Method D 1962.

8. Unsaponifiable Matter

8.1 The term unsaponifiable matter includes all of those

substances that are not saponified by alkali and that are soluble

in the ordinary fat solvents. Included are the higher aliphatic

alcohols, sterols, and hydrocarbons.

8.2 Determine unsaponifiable matter in accordance with

Test Method D 1965. Normal fatty acids contain small amounts

of unsaponifiable matter, usually under 2 %. When excessive

amounts of unsaponifiable matter are found, low quality is

indicated.

9. Ash

9.1 The ash in fatty acids is determined by igniting the acids

under specified conditions and determining the amounts of

noncombustible material. Carry out this procedure in accor-

dance with Test Method D 1951. The ash content of normal

fatty acids should be very small.

10. Hydroxyl Value

10.1 Hydroxyl value is defined as the number of milligrams

of potassium hydroxide equivalent to the hydroxyl (OH)

content of 1 g of sample. Hydroxystearic acid is the only

common fatty acid to which this test is applicable.

10.2 Determine the hydroxyl value in accordance with Test

Method D 1957.

11. Rosin Acids

11.1 Fatty acids derived from tall oils will normally contain

varying amounts of rosin acids. When the amount of the rosin

acids does not exceed 15 %, determine their content in accor-

dance with Test Method D 1240.

11.2 In Test Method D 1240 the rosin acids are determined

by titration after esterification of the fatty acids with methanol

in the presence of sulfuric acid as a catalyst, followed by

separation of the acids. The test method requires use of an

experimentally determined correction factor, dependent upon

the amount of rosin acids present.

12. Fatty Acid Composition

12.1 Fatty acid composition can be determined in accor-

dance with Test Method D 1983 after esterification of the fatty

acids in accordance with Test Method D 3457.

NOTE 2The types and amounts of polyunsaturated acids in a sample

of fatty acids may also be determined by use of an ultraviolet spectro-

photometer. By using this test method the percent of conjugated diene,

triene, tetraene, and pentaene acids, and of linoleic, linolenic, arachidonic,

and pentaenoic acids can be calculated. This test method is time-

consuming and the techniques required do not lend themselves to good

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accuracy or precision. The ultraviolet spectrophotometric method is not

included in the ASTM methods, and reference should be made to AOCS

Method Tj-1a.

13. Appearance

13.1 Observations for appearance of fatty acids should be

made on the liquefied sample. Transfer the sample to a

viscosity tube as described in Test Method D 1544 and check

for haze, dirt, skins, or other materials that might indicatecontamination of the material.

13.2 Determine the clarity in accordance with Test Method

D 2090.

14. Color

14.1 The color reference standards described in Test Method

D 1544 provide a rapid and sufficiently accurate means for

determining color on most fatty acids (Note 3). Where the hue

of the fatty acids sample does not exactly match that of the

reference sample, it is suggested that the intensity of color be

matched rather than attempting to match hue.

14.2 Where extremely light colored fatty acids are encoun-

tered, use Test Method D 1209.

NOTE 3No accurate correlation between Test Methods D 1209 and

D 1544 has been possible.

14.3 Lovibond glasses (AOCS Official Method Cc-13b) and

spectrophotometric measurements (AOCS Method Id-2a) are

occasionally used to measure fatty acid colors.

NOTE 4No correlation has been established between these methods

and Test Method D 1544 when used for fatty acids.

15. Titer

15.1 Titer is the solidification point of fatty acids under

specified conditions. Determine titer in accordance with Test

Method D 1982. The titer value can be correlated with the

degree of unsaturation of a fatty acid and is useful in

determining the identity and purity of a fatty acid.

16. Keywords

16.1 fatty acids; protective coatings

The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connectionwith any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any suchpatent rights, and the risk of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards

and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsibletechnical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your

views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

D 1467

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