ASTM D5974-00

Standard Test Methods for Fatty and Rosin Acids in Tall Oil Fractionation Products by Capillary Gas Chromatography

SCOPE
1.1 These test methods cover the determination of the amounts of the individual fatty acids and rosin acids in fractionated tall oil products, using capillary gas chromatographic separation of the volatile methyl esters of these acids.
1.2 Four methods for forming the methyl esters, and two methods for determining the amounts of the individual fatty acids and rosin acids are described.
1.2.1 The classic method for the formation of methyl esters is through the use of diazomethane, but diazomethane is a hazardous and toxic material, and so is no longer the preferred reagent. The use of diazomethane is detailed in the Appendix. Methyl esters may be formed through the use of tetramethylammonium hydroxide (TMAH), trimethylphenylammonium hydroxide (TMPAH), or N,N-dimethylformamide dimethyl acetyl (DMF-DMA).
1.2.2 The two methods for determining the amount of the individual fatty acids and rosin acids are the "internal standard" method, which yields absolute values, and the "area percent" method, which yields relative values.
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: 09-Nov-2000
• ICS: 67.080.10 - Fruits and derived products
• ICS: 67.200.10 - Animal and vegetable fats and oils
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.34 - Pine Chemicals and Hydrocarbon Resins

Relations

• Replaces: ASTM D5974-96 - Standard Test Methods for Fatty and Rosin Acids in Tall Oil Fractionation Products by Capillary Gas Chromatography
• Effective Date: 10-Nov-2000
• Replaced By: ASTM D5974-00(2005) - Standard Test Methods for Fatty and Rosin Acids in Tall Oil Fractionation Products by Capillary Gas Chromatography
• Effective Date: 01-Dec-2005
• Referred By: ASTM D509-20 - Standard Test Methods of Sampling and Grading Rosin
• Effective Date: 10-Nov-2000
• Referred By: ASTM D803-15(2020) - Standard Test Methods for Testing Tall Oil
• Effective Date: 10-Nov-2000

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5974–00
Standard Test Methods for
Fatty and Rosin Acids in Tall Oil Fractionation Products by
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Capillary Gas Chromatography
This standard is issued under the fixed designation D 5974; 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. Significance and Use
1.1 These test methods cover the determination of the 3.1 Tall oil fractionated products derived from tall oil are
amounts of the individual fatty acids and rosin acids in important commercial materials, primarily composed of fatty
fractionated tall oil products, using capillary gas chromato- acidsandrosinacids,butalsocontainingsomeneutralmaterial
graphic separation of the volatile methyl esters of these acids. (see Terminology D 804). For many applications, it is neces-
1.2 Four methods for forming the methyl esters, and two sary to know the level of the individual fatty acids and rosin
methods for determining the amounts of the individual fatty acids present in these products. Gas chromatography has
acids and rosin acids are described. proven to be a useful tool for such determinations (see Test
1.2.1 The classic method for the formation of methyl esters Methods D 509), and capillary chromatography, described in
is through the use of diazomethane, but diazomethane is a these test methods, is considered to be the most effective gas
hazardous and toxic material, and so is no longer the preferred chromatographic technique currently available. In particular
reagent. The use of diazomethane is detailed in the Appendix. situations, other techniques may be more suitable than gas
Methyl esters may be formed through the use of tetramethy- chromatography. For example, the presence of fatty acid esters
lammonium hydroxide (TMAH), trimethylphenylammonium in the sample would result in transesterification during the
hydroxide (TMPAH), or N,N-dimethylformamide dimethyl derivatization step that may affect the results.
acetal (DMF-DMA). 3.2 Due to hydrogen bonding, unmodified tall oil fatty acids
1.2.2 The two methods for determining the amount of the and rosin acids cannot be volatilized at atmospheric pressure
individualfattyacidsandrosinacidsarethe“internalstandard” without undergoing decomposition. So, it is necessary to
method, which yields absolute values, and the “area percent” convert the free acids to the more volatile and more stable
method, which yields relative values. methyl esters, prior to chromatographic separation.
1.3 This standard does not purport to address all of the 3.3 These test methods describe four ways to prepare
safety concerns, if any, associated with its use. It is the methyl esters. The classic method is through the use of
responsibility of the user of this standard to establish appro- diazomethane, but diazomethane is a hazardous and toxic
priate safety and health practices and determine the applica- material, and so is no longer the preferred agent. The use of
bility of regulatory limitations prior to use. diazomethane is detailed in the Appendix.
3.3.1 TMAH causes isomerization of a sample’s di- and
2. Referenced Documents
polyunsaturated fatty acids, when it is used in even a slight
2.1 ASTM Standards:
excess. This leads to inaccurate results for the individual fatty
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D 509 Test Methods of Sampling and Grading Rosin acid components.TMAH should be used for materials contain-
D 804 TerminologyRelatingtoNavalStores,IncludingTall
ing only rosin acids, or when the identification or quantitation
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Oil and Related Products of individual fatty acid components is not important.
E 691 Practice for Conducting an Interlaboratory Study to
3.3.2 TMPAH is the recommended methylating agent when
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Determine the Precision of a Test Method the identification or quantitation of individual di- and polyun-
saturated fatty acids is required. TMPAH produces results that
are very similar to those of diazomethane, but without the
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This test method is under the jurisdiction of ASTM Committee D01 on Paint
hazards that are associated with diazomethane. A considerable
and Related Coatings, Materials, andApplications and is the direct responsibility of
excess of TMPAH may cause isomerization of conjugated
Subcommittee D01.34 on Naval Stores.
Current edition approved Nov. 10, 2000. Published February 2001. Originally compounds similar to that encountered with TMAH.
published as D 5974 – 96. Last previous edition D 5974 – 96.
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Annual Book of ASTM Standards, Vol 06.03.
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Annual Book of ASTM Standards, Vol 14.02.
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