Standard Test Method for Acid Number of Petroleum Products by Semi-Micro Color Indicator Titration

SIGNIFICANCE AND USE
This test method measures the acid number of oils obtained from laboratory oxidation tests using smaller amounts of sample than Test Methods D 974 or D 664. It has specific application in Test Method D 943 in which small aliquots of oil are periodically removed for testing by Test Method D 3339. This test method, therefore, provides a means of monitoring the relative oxidation of oils, by measuring changes in acid number, at different time intervals and under the various oxidizing test conditions.
FIG. 1 Schematic Drawing of Typical Apparatus
SCOPE
1.1 This test method covers the determination of acidic constituents in new or used petroleum products and lubricants soluble or nearly soluble in mixtures of toluene, and isopropyl alcohol. The test method is especially intended for cases in which the amount of sample available to be analyzed is too small to allow accurate analysis by Test Methods D 974 or D 664. It is applicable for the determination of acids having dissociation constants in water larger than 10−9. Extremely weak acids having dissociation constants smaller than 10−9 do not interfere. Salts titrate if their hydrolysis constants are larger than 10−9.
1.2 This test method can be used to indicate relative changes in acid number that occur in an oil during use under oxidizing conditions. Although the titration is made under definite equilibrium conditions, the method does not measure an absolute acidic property that can be used to predict performance of an oil under service conditions. No general relationship between bearing corrosion and acid number is known.
1.3 Since this test method requires substantially less sample than Test Methods D 974 or D 664, it provides an advantageous means of monitoring an oxidation test by changes in acid number by (1) minimizing test sample depletion for acid number analyses and thus minimizing the disturbance of the test or (2) allowing additional acid number analyses to be made while maintaining the same test sample depletion and thus providing additional data.  
Note 1—Some oils, such as many cutting oils, rust-proofing oils, and similar compounded oils, or excessively dark-colored oils, may be more difficult to analyze by this test method due to obscurity of the color-indicator end point. These oils can be analyzed by Test Method D 664 provided sufficient sample is available. However, this situation is much less likely using Test Method D 3339 than using Test Method D 974 due to the use of a more highly dilute sample during the titration and due to the greater stability of the end point color change. The acid numbers obtained by Test Method D 3339 may or may not be numerically the same as those obtained by Test Method D 664 but they should be of the same order of magnitude.
Note 2—The results obtained using this method have been found to be numerically the same as those obtained using Test Method D 974, within the precision of the two methods, for new or oxidized lubricants of the type primarily intended for hydraulic or steam turbine type service. The oxidized lubricants were obtained using the Test Method D 943 oxidation test. This correlation is shown by the correlation coefficient r = 0.989 with slope s = + 1.017 and intercept  y = + 0.029, calculated using the acid numbers obtained using both titration methods for the samples used for the precision statement (12.2).  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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 warning statements, see Sections 7 and 9, A1.1.4, A2.3.1, and A2.10.1.

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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:D3339–11
Standard Test Method for
Acid Number of Petroleum Products by Semi-Micro Color
1
Indicator Titration
This standard is issued under the fixed designation D3339; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
obtained by Test Method D664 but they should be of the same order of
1. Scope*
magnitude.
1.1 This test method covers the determination of acidic
NOTE 2—Theresultsobtainedusingthismethodhavebeenfoundtobe
constituents in new or used petroleum products and lubricants
numerically the same as those obtained using Test Method D974, within
soluble or nearly soluble in mixtures of toluene, and isopropyl
the precision of the two methods, for new or oxidized lubricants of the
alcohol. The test method is especially intended for cases in type primarily intended for hydraulic or steam turbine type service. The
oxidized lubricants were obtained using the Test Method D943 oxidation
which the amount of sample available to be analyzed is too
test.Thiscorrelationisshownbythecorrelationcoefficient r=0.989with
small to allow accurate analysis by Test Methods D974 or
slope s=+1.017 and intercept y=+0.029, calculated using the acid
D664. It is applicable for the determination of acids having
numbersobtainedusingbothtitrationmethodsforthesamplesusedforthe
−9
dissociation constants in water larger than 10 . Extremely
2
precision statement (12.2).
−9
weak acids having dissociation constants smaller than 10 do
1.4 The values stated in SI units are to be regarded as
notinterfere.Saltstitrateiftheirhydrolysisconstantsarelarger
−9 standard. No other units of measurement are included in this
than 10 .
standard.
1.2 Thistestmethodcanbeusedtoindicaterelativechanges
1.5 This standard does not purport to address all of the
in acid number that occur in an oil during use under oxidizing
safety concerns, if any, associated with its use. It is the
conditions. Although the titration is made under definite
responsibility of the user of this standard to establish appro-
equilibrium conditions, the method does not measure an
priate safety and health practices and determine the applica-
absolute acidic property that can be used to predict perfor-
bility of regulatory limitations prior to use. For specific
mance of an oil under service conditions. No general relation-
warning statements, see Sections 7 and 9,A1.1.4,A2.3.1, and
ship between bearing corrosion and acid number is known.
A2.10.1.
1.3 Sincethistestmethodrequiressubstantiallylesssample
thanTest Methods D974 or D664, it provides an advantageous
2. Referenced Documents
means of monitoring an oxidation test by changes in acid
3
2.1 ASTM Standards:
number by (1) minimizing test sample depletion for acid
D664 Test Method forAcid Number of Petroleum Products
number analyses and thus minimizing the disturbance of the
by Potentiometric Titration
testor(2)allowingadditionalacidnumberanalysestobemade
D943 Test Method for Oxidation Characteristics of Inhib-
while maintaining the same test sample depletion and thus
ited Mineral Oils
providing additional data.
D974 Test Method for Acid and Base Number by Color-
NOTE 1—Some oils, such as many cutting oils, rust-proofing oils, and
Indicator Titration
similar compounded oils, or excessively dark-colored oils, may be more
D1193 Specification for Reagent Water
difficult to analyze by this test method due to obscurity of the color-
indicator end point. These oils can be analyzed by Test Method D664
3. Terminology
provided sufficient sample is available. However, this situation is much
3.1 Definitions:
lesslikelyusingTestMethodD3339thanusingTestMethodD974dueto
3.1.1 acid number, n—the quantity of a specified base,
the use of a more highly dilute sample during the titration and due to the
greaterstabilityoftheendpointcolorchange.Theacidnumbersobtained expressed in milligrams of potassium hydroxide per gram of
by Test Method D3339 may or may not be numerically the same as those
2
UseofthecorrelationcoefficientisgiveninMack,C., Essentials of Statistics
1
This test method is under the jurisdiction of ASTM Committee D02 on for Scientists and Technologists, Plenum Press, New York, NY, 1967, or other
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee publications on statistics.
3
D02.06 on Analysis of Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 15, 2011. Published July 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1974. Last previous edition approved in 2008 as D3339–08. DOI: Standards volume in
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately,ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D3339–08 Designation:D3339–11
Standard Test Method for
Acid Number of Petroleum Products by Semi-Micro Color
1
Indicator Titration
This standard is issued under the fixed designation D3339; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method covers the determination of acidic constituents in new or used petroleum products and lubricants soluble
or nearly soluble in mixtures of toluene, and isopropyl alcohol. The test method is especially intended for cases in which the
amount of sample available to be analyzed is too small to allow accurate analysis byTest Methods D974 or D664. It is applicable
−9
for the determination of acids having dissociation constants in water larger than 10 . Extremely weak acids having dissociation
−9 −9
constants smaller than 10 do not interfere. Salts titrate if their hydrolysis constants are larger than 10 .
1.2 This test method can be used to indicate relative changes in acid number that occur in an oil during use under oxidizing
conditions.Although the titration is made under definite equilibrium conditions, the method does not measure an absolute acidic
property that can be used to predict performance of an oil under service conditions. No general relationship between bearing
corrosion and acid number is known.
1.3 Since this test method requires substantially less sample than Test Methods D974 or D664, it provides an advantageous
meansofmonitoringanoxidationtestbychangesinacidnumberby(1)minimizingtestsampledepletionforacidnumberanalyses
and thus minimizing the disturbance of the test or (2) allowing additional acid number analyses to be made while maintaining the
same test sample depletion and thus providing additional data.
NOTE 1—Someoils,suchasmanycuttingoils,rust-proofingoils,andsimilarcompoundedoils,orexcessivelydark-coloredoils,maybemoredifficult
to analyze by this test method due to obscurity of the color-indicator end point. These oils can be analyzed by Test Method D664 provided sufficient
sample is available. However, this situation is much less likely using Test Method D3339 than using Test Method D974 due to the use of a more highly
dilute sample during the titration and due to the greater stability of the end point color change. The acid numbers obtained by Test Method D3339 may
or may not be numerically the same as those obtained by Test Method D664 but they should be of the same order of magnitude.
NOTE 2—The results obtained using this method have been found to be numerically the same as those obtained using Test Method D974, within the
precision of the two methods, for new or oxidized lubricants of the type primarily intended for hydraulic or steam turbine type service. The oxidized
lubricants were obtained using the Test Method D943 oxidation test. This correlation is shown by the correlation coefficient r=0.989 with slope
s=+1.017 and intercept y=+0.029, calculated using the acid numbers obtained using both titration methods for the samples used for the precision
2
statement (12.2).
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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 warning statements, see Sections 7 and 9, A1.1.4, A2.3.1, and A2.10.1.
2. Referenced Documents
3
2.1 ASTM Standards:
D664 Test Method for Acid Number of Petroleum Products by Potentiometric Titration
D943 Test Method for Oxidation Characteristics of Inhibited Mineral Oils
D974 Test Method for Acid and Base Number by Color-Indicator Titration
D1193 Specification for Reagent Water
1
This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.06 on
Analysis of Lubricants.
Current edition approved July 1, 2008. Published August 2008. Originally approved in 1974. Last previous edition approved in 2007 as D3339–07. DOI:
10.1520/D3339-08.
CurrenteditionapprovedMay15,2011.PublishedJuly2011.Originallyapprovedin1974.Lastpreviouseditionapprovedin2008asD3339–08.DOI:10.1
...

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