ASTM D94-02
(Test Method)Standard Test Methods for Saponification Number of Petroleum Products
Standard Test Methods for Saponification Number of Petroleum Products
SCOPE
1.1 These test methods cover the determination of the amount of constituents in petroleum products such as lubricants, additives, and transmission fluids that will saponify under the conditions of the test.
1.1.1 Two test methods are described: Method A-Color Indicator Titration (Sections 6-13), and Method B-Potentiometric Titration (Sections 14-23).
1.2 Because compounds of sulfur, phosphorus, the halogens, and certain other elements that are sometimes added to petroleum products also consume alkali and acids, the results obtained indicate the effect of these extraneous materials in addition to the saponifiable material present. Results on products containing such materials, on used internal-combustion-engine crankcase oils, and on used turbine oils must be interpreted with caution.
Note 1—The materials referred to above, which are not normally considered saponifiable matter, include inorganic or certain organic acids, most nonalkali soaps, and so forth. The presence of such materials increases the saponification number above that of fatty saponifiable materials for which the test method is primarily intended. The odor of hydrogen sulfide near the end of the back-titration in the saponification test is an indication that certain types of reactive sulfur compounds are present in the sample. In the case of other reactive sulfur, chlorine, and phosphorus compounds and other interfering materials, no simple indication is given during the test. A gravimetric determination of the actual amount of fatty acids is probably the most reliable method for such compounds. Test Methods D 128 or IP Method 284/86 can be used to determine fatty acids gravimetrically.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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. For specific hazard statements, see Sections 6, 7, 8, 10, 15, 16, 17, and 19.
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An American National Standard
Designation: D 94 – 02
Designation: 136S1/98, 136S2/99
Standard Test Methods for
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Saponification Number of Petroleum Products
ThisstandardisissuedunderthefixeddesignationD94;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope responsibility of the user of this standard to establish appro-
2 priate safety and health practices and determine the applica-
1.1 These test methods cover the determination of the
bility of regulatory limitations prior to use. For specific hazard
amount of constituents in petroleum products such as lubri-
statements, see Sections 6, 7, 8, 10, 15, 16, 17, and 19.
cants, additives, and transmission fluids that will saponify
under the conditions of the test.
2. Referenced Documents
1.1.1 Two test methods are described: Method A—Color
2.1 ASTM Standards:
Indicator Titration (Sections 6-13), and Method
D117 Guide to Test Methods, Specifications, and Guides
B—Potentiometric Titration (Sections 14-23).
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for Electrical Insulating Oils of Petroleum Origin
1.2 Because compounds of sulfur, phosphorus, the halo-
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D128 Test Methods for Analysis of Lubricating Grease
gens, and certain other elements that are sometimes added to
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D1193 Specification for Reagent Water
petroleum products also consume alkali and acids, the results
D4057 Practice for Manual Sampling of Petroleum and
obtained indicate the effect of these extraneous materials in
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Petroleum Products
addition to the saponifiable material present. Results on prod-
D4177 Practice for Automatic Sampling of Petroleum and
ucts containing such materials, on used internal-combustion-
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Petroleum Products
engine crankcase oils, and on used turbine oils must be
D6299 Practice forApplying Statistical QualityAssurance
interpreted with caution.
Techniques to Evaluate Analytical Measurement System
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NOTE 1—The materials referred to above, which are not normally
Performance
considered saponifiable matter, include inorganic or certain organic acids,
2.2 Institute of Petroleum Standards:
most nonalkali soaps, and so forth. The presence of such materials
IP136 Method of Test for Saponification Number of Petro-
increases the saponification number above that of fatty saponifiable
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leum Products
materials for which the test method is primarily intended. The odor of
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IP 284 Method of Test for Fatty Acids
hydrogen sulfide near the end of the back-titration in the saponification
test is an indication that certain types of reactive sulfur compounds are
3. Terminology
present in the sample. In the case of other reactive sulfur, chlorine, and
phosphorus compounds and other interfering materials, no simple indica-
3.1 Definitions:
tion is given during the test. A gravimetric determination of the actual
3.1.1 saponification number, n—the number of milligrams
amount of fatty acids is probably the most reliable method for such
ofpotassiumhydroxideconsumedby1gofasampleunderthe
compounds. Test Methods D128 or IP Method284/86 can be used to
conditions of the test.
determine fatty acids gravimetrically.
3.1.1.1 Discussion—Thevalueofthesaponificationnumber
1.3 The values stated in SI units are to be regarded as the
in these test methods can be affected by the presence of other
standard.
alkali-reactive species, as described in Note 1.
1.4 This standard does not purport to address all of the
3.1.2 saponify, v—to hydrolyze a fat with alkali to form an
safety concerns, if any, associated with its use. It is the
alcohol and the salt of a fatty acid.
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These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
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tee D02.06 on Analysis of Lubricants. Annual Book of ASTM Standards, Vol 10.03.
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Current edition approved June 10, 2002. Published August 2002. Originally Annual Book of ASTM Standards, Vol 05.01.
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published as D94–21T. Last previous edition D94–00. Annual Book of ASTM Standards, Vol 11.01.
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Statements defining this test and its significance when applied to electrical Annual Book of ASTM Standards, Vol 05.02.
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insulating oils of mineral origin will be found in Guide D117. Experience has Annual Book of ASTM Standards, Vol 05.03.
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shown that for transformer oils, Test Method D94, modified by use of 0.1 M KOH Available from Institute of Petroleum, 61 New Cavendish St., London, W.I.,
solution and 0.1 M HCl, is more suitable. England.
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