ASTM D4684-08
(Test Method)Standard Test Method for Determination of Yield Stress and Apparent Viscosity of Engine Oils at Low Temperature
Standard Test Method for Determination of Yield Stress and Apparent Viscosity of Engine Oils at Low Temperature
SIGNIFICANCE AND USE
When an engine oil is cooled, the rate and duration of cooling can affect its yield stress and viscosity. In this laboratory test, a fresh engine oil is slowly cooled through a temperature range where wax crystallization is known to occur, followed by relatively rapid cooling to the final test temperature. These laboratory test results have predicted as failures the known engine oils that have failed in the field because of lack of oil pumpability. These documented field failing oils have all consisted of oils normally tested at –25°C. These field failures are believed to be the result of the oil forming a gel structure that results in either excessive yield stress or viscosity of the engine oil, or both.
Cooling Profiles:
For oils to be tested at −20°C or colder, Table X1.1 applies. The cooling profile described in Table X1.1 is based on the viscosity properties of the ASTM Pumpability Reference Oils (PRO). This series of oils includes oils with normal low-temperature flow properties and oils that have been associated with low-temperature pumpability problems (1-5). Significance for the −35 and −40°C temperature profiles is based on the data collected from the “Cold Starting and Pumpability Studies in Modern Engines” conducted by ASTM (6,7).
For oils to be tested at −15 or −10°C, Table X1.2 applies. No significance has been determined for this temperature profile because of the absence of appropriate reference oils. Similarly, precision of the test method using this profile for the −10°C test temperature is unknown. The temperature profile of Table X1.2 is derived from the one in Table X1.1 and has been moved up in temperature, relative to Table X1.1, in consideration of the expected higher cloud points of the viscous oils tested at −15 and −10°C.
SCOPE
1.1 This test method covers the measurement of the yield stress and viscosity of engine oils after cooling at controlled rates over a period exceeding 45 h to a final test temperature between –10 and –40°C. The viscosity measurements are made at a shear stress of 525 Pa over a shear rate of 0.4 to 15 s–1. The viscosity as measured at this shear stress was found to produce the best correlation between the temperature at which the viscosity reached a critical value and borderline pumping failure temperature in engines.
1.2 This test method contain two procedures: Procedure A incorporates several equipment and procedural modifications from Test Method D 4684–02 that have shown to improve the precision of the test, while Procedure B is unchanged from Test Method D 4684–02. Additionally, Procedure A applies to those instruments that utilize thermoelectric cooling technology or direct refrigeration technology of recent manufacture for instrument temperature control. Procedure B can use the same instruments used in Procedure A or those cooled by circulating methanol.
1.3 Procedure A of this test method has precision stated for a yield range from less than 35 Pa to 210 Pa and apparent viscosity range from 4300 to 270 000 mPa·s. The test procedure can determine higher yield stress and viscosity levels.
1.4 This test method is applicable for unused oils, sometimes referred to as fresh oils, designed for both light duty and heavy duty engine applications. It also has been shown to be suitable for used diesel and gasoline engine oils. The applicability to petroleum products other than engine oils has not been determined.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5.1 Exception—This test method uses the milliPascal second (mPa·s) as the unit of viscosity. For information, the equivalent unit, centiPoise (cP), is shown in parentheses.
1.6 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 det...
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Designation: D4684 − 08
StandardTest Method for
Determination of Yield Stress and Apparent Viscosity of
1
Engine Oils at Low Temperature
This standard is issued under the fixed designation D4684; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* 1.5.1 Exception—This test method uses the milliPascal
second (mPa·s) as the unit of viscosity. For information, the
1.1 This test method covers the measurement of the yield
equivalent unit, centiPoise (cP), is shown in parentheses.
stress and viscosity of engine oils after cooling at controlled
1.6 This standard does not purport to address all of the
rates over a period exceeding 45 h to a final test temperature
safety concerns, if any, associated with its use. It is the
between–10and–40°C.Theviscositymeasurementsaremade
–1
responsibility of the user of this standard to establish appro-
atashearstressof525Paoverashearrateof0.4to15s .The
priate safety and health practices and determine the applica-
viscosity as measured at this shear stress was found to produce
bility of regulatory limitations prior to use.
the best correlation between the temperature at which the
viscosity reached a critical value and borderline pumping
2. Referenced Documents
failure temperature in engines.
2
2.1 ASTM Standards:
1.2 This test method contain two procedures: Procedure A
D3829Test Method for Predicting the Borderline Pumping
incorporates several equipment and procedural modifications
Temperature of Engine Oil
from Test Method D4684–02 that have shown to improve the
3
precisionofthetest,whileProcedureBisunchangedfromTest 2.2 ISO Standard:
Method D4684–02.Additionally, ProcedureAapplies to those ISO 17025General Requirements for the Competence of
instruments that utilize thermoelectric cooling technology or Testing and Calibration Laboratories
direct refrigeration technology of recent manufacture for in- ISO Guide 34General Requirements for the Competence of
strument temperature control. Procedure B can use the same Reference Material Producers
instruments used in ProcedureAor those cooled by circulating ISO Guide 35Certification of Reference Materials
methanol.
3. Terminology
1.3 ProcedureAof this test method has precision stated for
3.1 Definitions:
a yield range from less than 35 Pa to 210 Pa and apparent
3.1.1 apparent viscosity—the determined viscosity obtained
viscosity range from 4300 to 270 000 mPa·s. The test proce-
by use of this test method.
dure can determine higher yield stress and viscosity levels.
3.1.2 Newtonian oil or fluid—an oil or fluid that at a given
1.4 This test method is applicable for unused oils, some-
temperature exhibits a constant viscosity at all shear rates or
times referred to as fresh oils, designed for both light duty and
shear stresses.
heavy duty engine applications. It also has been shown to be
suitable for used diesel and gasoline engine oils. The applica-
3.1.3 non-Newtonian oil or fluid—an oil or fluid that at a
bilitytopetroleumproductsotherthanengineoilshasnotbeen
given temperature exhibits a viscosity that varies with chang-
determined.
ing shear stress or shear rate.
1.5 The values stated in SI units are to be regarded as 3.1.4 shear rate—the velocity gradient in fluid flow. For a
standard. No other units of measurement are included in this Newtonian fluid in a concentric cylinder rotary viscometer in
standard. whichtheshearstressismeasuredattheinnercylindersurface
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
D02.07 on Flow Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2008. Published January 2009. Originally the ASTM website.
´1 3
approved in 1987. Last previous edition approved in 2007 as D4684–07 . DOI: Available from International Organization for Standardization (ISO), 1 rue de
10.1520/D4684-08. Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland, http://www.iso.ch.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D4684 − 08
(suchasthisapparatus,describedin6.1),andignoringanyend 3.2.5 used oil—an oil which has been used in an oper
...
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.
An American National Standard
´1
Designation:D4684–07 Designation: D 4684 – 08
Standard Test Method for
Determination of Yield Stress and Apparent Viscosity of
1
Engine Oils at Low Temperature
This standard is issued under the fixed designation D4684; 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.
This standard has been approved for use by agencies of the Department of Defense.
1
´ NOTE—Added research report to existing footnote for Section 13 editorially in December 2008.
1. Scope*
1.1 Thistestmethodcoversthemeasurementoftheyieldstressandviscosityofengineoilsaftercoolingatcontrolledratesover
a period exceeding 45 h to a final test temperature between –10 and –40°C.The viscosity measurements are made at a shear stress
–1
of525Paoverashearrateof0.4to15s .Theviscosityasmeasuredatthisshearstresswasfoundtoproducethebestcorrelation
between the temperature at which the viscosity reached a critical value and borderline pumping failure temperature in engines.
1.2ProcedureAof this test method has precision stated for a yield range from less than 35 Pa to 210 Pa and apparent viscosity
range from 4300 to 270 000 mPa·s. The test procedure can determine higher yield stress and viscosity levels.
1.3Thistestmethodisapplicableforunusedoils,sometimesreferredtoasfreshoils,designedforbothlightdutyandheavyduty
engine applications. It also has been shown to be suitable for used diesel and gasoline engine oils. The applicability to petroleum
products other than engine oils has not been determined.
1.4This test method uses the milliPascal second (mPa·s) as the unit of viscosity. For information, the equivalent unit, centiPoise
(cP), is shown in parentheses.
1.5Thistestmethodcontaintwoprocedures:ProcedureAincorporatesseveralequipmentandproceduralmodificationsfromTest
Method D4684–02 that have shown to improve the precision of the test, while Procedure B is unchanged from Test Method
D4684–02.Additionally,ProcedureAappliestothoseinstrumentsthatutilizethermoelectriccoolingtechnologyandthosethatuse
indirect refrigeration technology of recent manufacture for instrument temperature control. Procedure B can use the same
instruments used in Procedure A or those cooled by circulating methanol.
1.2 This test method contain two procedures: Procedure A incorporates several equipment and procedural modifications from
Test Method D4684–02 that have shown to improve the precision of the test, while Procedure B is unchanged from Test Method
D4684–02. Additionally, Procedure A applies to those instruments that utilize thermoelectric cooling technology or direct
refrigerationtechnologyofrecentmanufactureforinstrumenttemperaturecontrol.ProcedureBcanusethesameinstrumentsused
in Procedure A or those cooled by circulating methanol.
1.3 ProcedureAof this test method has precision stated for a yield range from less than 35 Pa to 210 Pa and apparent viscosity
range from 4300 to 270 000 mPa·s. The test procedure can determine higher yield stress and viscosity levels.
1.4 This test method is applicable for unused oils, sometimes referred to as fresh oils, designed for both light duty and heavy
duty engine applications. It also has been shown to be suitable for used diesel and gasoline engine oils. The applicability to
petroleum products other than engine oils has not been determined.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5.1 Exception—This test method uses the milliPascal second (mPa·s) as the unit of viscosity. For information, the equivalent
unit, centiPoise (cP), is shown in parentheses.
1.6 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.
1
This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.07 on
Flow Properties.
Current edition approved Jan. 15, 2007. Published March 2007. Originally approved in 1987. Last previous edition approved in 2002 as D4684–02a.
´1
Current edition approved Dec. 1, 2008. Published January 2009. Originally approved in 1987. Last previ
...
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.
An American National Standard
´1
Designation:D4684–07 Designation: D 4684 – 08
Standard Test Method for
Determination of Yield Stress and Apparent Viscosity of
1
Engine Oils at Low Temperature
This standard is issued under the fixed designation D4684; 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.
This standard has been approved for use by agencies of the Department of Defense.
1
´ NOTE—Added research report to existing footnote for Section 13 editorially in December 2008.
1. Scope*
1.1 Thistestmethodcoversthemeasurementoftheyieldstressandviscosityofengineoilsaftercoolingatcontrolledratesover
a period exceeding 45 h to a final test temperature between –10 and –40°C.The viscosity measurements are made at a shear stress
–1
of525Paoverashearrateof0.4to15s .Theviscosityasmeasuredatthisshearstresswasfoundtoproducethebestcorrelation
between the temperature at which the viscosity reached a critical value and borderline pumping failure temperature in engines.
1.2ProcedureAof this test method has precision stated for a yield range from less than 35 Pa to 210 Pa and apparent viscosity
range from 4300 to 270 000 mPa·s. The test procedure can determine higher yield stress and viscosity levels.
1.3Thistestmethodisapplicableforunusedoils,sometimesreferredtoasfreshoils,designedforbothlightdutyandheavyduty
engine applications. It also has been shown to be suitable for used diesel and gasoline engine oils. The applicability to petroleum
products other than engine oils has not been determined.
1.4This test method uses the milliPascal second (mPa·s) as the unit of viscosity. For information, the equivalent unit, centiPoise
(cP), is shown in parentheses.
1.5Thistestmethodcontaintwoprocedures:ProcedureAincorporatesseveralequipmentandproceduralmodificationsfromTest
Method D4684–02 that have shown to improve the precision of the test, while Procedure B is unchanged from Test Method
D4684–02.Additionally,ProcedureAappliestothoseinstrumentsthatutilizethermoelectriccoolingtechnologyandthosethatuse
indirect refrigeration technology of recent manufacture for instrument temperature control. Procedure B can use the same
instruments used in Procedure A or those cooled by circulating methanol.
1.2 This test method contain two procedures: Procedure A incorporates several equipment and procedural modifications from
Test Method D4684–02 that have shown to improve the precision of the test, while Procedure B is unchanged from Test Method
D4684–02. Additionally, Procedure A applies to those instruments that utilize thermoelectric cooling technology or direct
refrigerationtechnologyofrecentmanufactureforinstrumenttemperaturecontrol.ProcedureBcanusethesameinstrumentsused
in Procedure A or those cooled by circulating methanol.
1.3 ProcedureAof this test method has precision stated for a yield range from less than 35 Pa to 210 Pa and apparent viscosity
range from 4300 to 270 000 mPa·s. The test procedure can determine higher yield stress and viscosity levels.
1.4 This test method is applicable for unused oils, sometimes referred to as fresh oils, designed for both light duty and heavy
duty engine applications. It also has been shown to be suitable for used diesel and gasoline engine oils. The applicability to
petroleum products other than engine oils has not been determined.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5.1 Exception—This test method uses the milliPascal second (mPa·s) as the unit of viscosity. For information, the equivalent
unit, centiPoise (cP), is shown in parentheses.
1.6 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.
1
This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.07 on
Flow Properties.
Current edition approved Jan. 15, 2007. Published March 2007. Originally approved in 1987. Last previous edition approved in 2002 as D4684–02a.
´1
Current edition approved Dec. 1, 2008. Published January 2009. Originally approved in 1987. Last previ
...
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