ASTM D4684-12

Standard Test Method for Determination of Yield Stress and Apparent Viscosity of Engine Oils at Low Temperature

SIGNIFICANCE AND USE
5.1 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.4 These documented field failing oils 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.  
5.2 Cooling Profiles:  
5.2.1 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).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).  
5.2.2 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 precision is stated for test temperatures from –40 to –15°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 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 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 SI based unit of milliPascal second (mPa·s) for viscosity which is equivalent to, centiPoise (cP).  
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 es...

General Information

• Status: Historical
• Publication Date: 30-Nov-2012
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.07 - Flow Properties

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: D4684 − 12
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 U.S. Department of Defense.
1. Scope* 1.5.1 Exception—This test method uses the SI based unit of
milliPascalsecond(mPa·s)forviscositywhichisequivalentto,
1.1 This test method covers the measurement of the yield
centiPoise (cP).
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 –10 and –40°C. The precision is stated for test
responsibility of the user of this standard to establish appro-
temperatures from –40 to –15°C. The viscosity measurements
priate safety and health practices and determine the applica-
are made at a shear stress of 525 Pa over a shear rate of 0.4 to
–1
bility of regulatory limitations prior to use.
15s .Theviscosityasmeasuredatthisshearstresswasfound
to produce the best correlation between the temperature at
2. Referenced Documents
which the viscosity reached a critical value and borderline
2
pumping failure temperature in engines.
2.1 ASTM Standards:
D3829Test Method for Predicting the Borderline Pumping
1.2 This test method contain two procedures: Procedure A
Temperature of Engine Oil
incorporates several equipment and procedural modifications
E1137SpecificationforIndustrialPlatinumResistanceTher-
from Test Method D4684–02 that have shown to improve the
mometers
precisionofthetest,whileProcedureBisunchangedfromTest
3
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.
1.3 ProcedureAof this test method has precision stated for
3. Terminology
a yield range from less than 35 Pa to 210 Pa and apparent
3.1 Definitions:
viscosity range from 4300 to 270 000 mPa·s. The test proce-
3.1.1 apparent viscosity, n—the determined viscosity ob-
dure can determine higher yield stress and viscosity levels.
tained by use of this test method.
1.4 This test method is applicable for unused oils, some-
3.1.2 Digital Contact Thermometer (DCT), n—anelectronic
times referred to as fresh oils, designed for both light duty and
device consisting of a digital display and associated tempera-
heavy duty engine applications. It also has been shown to be
ture sensing probe.
suitable for used diesel and gasoline engine oils. The applica-
3.1.2.1 Discussion—This device consists of a temperature
bilitytopetroleumproductsotherthanengineoilshasnotbeen
sensor connected to a measuring instrument; this instrument
determined.
measures the temperature-dependent quantity of the sensor,
1.5 The values stated in SI units are to be regarded as
computes the temperature from the measured quantity, and
standard. No other units of measurement are included in this
providesadigitaloutputordisplay,orboth,ofthetemperature.
standard.
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, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Subcommittee D02.07 on Flow Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2012. Published April 2013. Originally the ASTM website.
3
approved in 1987. Last previous edition approved in 2008 as D4684–08. DOI: Available from International Organization for Standardization (ISO), 1 rue de
10.1520/D4684-12. 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

---------------------- Page: 1 ----------------------
D4684 − 12
The temperature sensing p
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D4684 − 08 D4684 − 12
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. A number 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*
1.1 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 precision is stated for test temperatures from –40
–1
to –15°C. The viscosity measurements are made at a shear stress of 525 Pa over a shear rate of 0.4 to 15 s . 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 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
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 SI based unit of milliPascal second (mPa·s) as the unit of viscosity. For information,
the equivalent unit, centiPoise (cP), is shown in parentheses.for viscosity which is equivalent to, centiPoise (cP).
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D3829 Test Method for Predicting the Borderline Pumping Temperature of Engine Oil
E1137 Specification for Industrial Platinum Resistance Thermometers
3
2.2 ISO Standard:
ISO 17025 General Requirements for the Competence of Testing and Calibration Laboratories
ISO Guide 34 General Requirements for the Competence of Reference Material Producers
ISO Guide 35 Certification of Reference Materials
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.07 on
Flow Properties.
Current edition approved Dec. 1, 2008Dec. 1, 2012. Published January 2009April 2013. Originally approved in 1987. Last previous edition approved in 20072008 as
ε1
D4684–07–08. . DOI: 10.1520/D4684-08.10.1520/D4684-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from International Organization for Standardization (ISO), 1 rue de 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

---------------------- Page: 1 ----------------------
D4684 − 12
3. Terminology
3.1 Definitions:
3.1.1 apparent viscosity—viscosity, n—the determined viscosity obtained
...