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Designation: D 1467 89 (Reapproved 1995)e1

AMERICAN SOCIETY FOR TESTING AND MATERIALS 100 Barr Harbor Dr., West Conshohocken, PA 19428 Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Guide for Testing

Fatty Acids Used in Protective Coatings1

This standard is issued under the xed 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 Acid Value Appearance Ash Clarity Color: Gardner Platinum-Cobalt Color Change After Heating Fatty Acid Composition Hydroxyl Value Rosin Acids Sampling Saponication Value Titer Unsaponiable Matter Unsaturation: Diene Value Iodine Value Section 4 13 9 13 14 14 6 12 10 11 3 7 15 8 5 5 ASTM Test Method D 1980 D 1544 D 1951 D 2090 D 1544 D 1209 D 1981 D 1983 D 1957 D 1240 D 1466 D 1962 D 1982 D 1965 D 1358 D 1959

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. Referenced Documents 2.1 ASTM Standards: D 1209 Test Method for Color of Clear Liquids (PlatinumCobalt 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
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.

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 Saponication Value of Drying Oils, Fatty Acids, and Polymerized Fatty Acids3 D 1965 Test Method for Unsaponiable 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 GasLiquid 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 liquied 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.
Annual Book of ASTM Standards, Vol 06.01. Available from American Oil Chemists Society, 508 S. 6th St., Champlain, IL 61820.
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3.3 Samples should be stored preferably in the dark, in full glass containers. Partially lled containers should be lled 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 dened 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 the identity 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 precision (Note 1) when applied to normal fatty acids. When Test Method D 1959 is applied to fatty acids containing conjugated double bonds such as dehydrated castor or tung an empirical gure 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 dehydrated castor acids, a specimen weight of 0.11 to 0.13 g of fatty acids must be used to get comparative results between laboratories.
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 denitely affect the accuracy and precision of the test method.

groups in fatty acids and is expressed as the number of milligrams of potassium hydroxide that will react with 1 g of sample. The saponication 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 saponication value and the acid value is frequently referred to as the ester value. Saponication value can be used to calculate the average molecular weight of the fatty acid. 7.2 Determine the saponication value in accordance with Test Method D 1962. 8. Unsaponiable Matter 8.1 The term unsaponiable matter includes all of those substances that are not saponied by alkali and that are soluble in the ordinary fat solvents. Included are the higher aliphatic alcohols, sterols, and hydrocarbons. 8.2 Determine unsaponiable matter in accordance with Test Method D 1965. Normal fatty acids contain small amounts of unsaponiable matter, usually under 2 %. When excessive amounts of unsaponiable matter are found, low quality is indicated. 9. Ash 9.1 The ash in fatty acids is determined by igniting the acids under specied conditions and determining the amounts of noncombustible material. Carry out this procedure in accordance with Test Method D 1951. The ash content of normal fatty acids should be very small. 10. Hydroxyl Value 10.1 Hydroxyl value is dened 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 accordance with Test Method D 1240. 11.2 In Test Method D 1240 the rosin acids are determined by titration after esterication 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 accordance with Test Method D 1983 after esterication 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 spectrophotometer. 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 timeconsuming and the techniques required do not lend themselves to good

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 to elevated 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 nal 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. Saponication Value 7.1 Saponication value is a measure of the alkali-reactive

D 1467
accuracy or precision. The ultraviolet spectrophotometric method is not included in the ASTM methods, and reference should be made to AOCS Method Tj-1a.

14.2 Where extremely light colored fatty acids are encountered, use Test Method D 1209.
NOTE 3No accurate correlation between Test Methods D 1209 and D 1544 has been possible.

13. Appearance 13.1 Observations for appearance of fatty acids should be made on the liqueed 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 indicate contamination 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.

14.3 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 solidication point of fatty acids under specied 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

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