ASTM D5133-05(2011)
(Test Method)Standard Test Method for Low Temperature, Low Shear Rate, Viscosity/Temperature Dependence of Lubricating Oils Using a Temperature-Scanning Technique
Standard Test Method for Low Temperature, Low Shear Rate, Viscosity/Temperature Dependence of Lubricating Oils Using a Temperature-Scanning Technique
SIGNIFICANCE AND USE
Significance of Low-Temperature, Low Shear Rate, Engine Oil Rheology—The low-temperature, low-shear viscometric behavior of an engine oil determines whether the oil will flow to the sump inlet screen, then to the oil pump, then to the sites in the engine requiring lubrication in sufficient quantity to prevent engine damage immediately or ultimately after cold temperature starting.
Two forms of flow problems have been identified, flow-limited and air-binding behavior. The first form of flow restriction, flow-limited behavior, is associated with the oil's viscosity; the second, air-binding behavior, is associated with gelation.
Significance of the Test Method—The temperature-scanning technique employed by this test method was designed to determine the susceptibility of the engine oil to flow-limited and air-binding response to slow cooling conditions by providing continuous information on the rheological condition of the oil over the temperature range of use. , , In this way, both viscometric and gelation response are obtained in one test.
Note 1—This test method is one of three related to pumpability related problems. Measurement of low-temperature viscosity by the two other pumpability Test Methods D3829 and D4684, hold the sample in a quiescent state and generate the apparent viscosity of the sample at shear rates ranging up to 15 sec-1 and shear stresses up to 525 Pa at a previously selected temperature. Such difference in test parameters (shear rate, shear stress, sample motion, temperature scanning, and so forth) can lead to differences in the measured apparent viscosity among these test methods with some test oils, particularly when other rheological factors associated with gelation are present. In addition, the three methods differ considerably in cooling rates.
Gelation Index and Gelation Index Temperature—This test method has been further developed to yield parameters called the Gelation Index and Gelation Index temperature. The first parameter is a...
SCOPE
1.1 This test method covers the measurement of the apparent viscosity of engine oil at low temperatures.
1.2 A shear rate of approximately 0.2 s-1 is produced at shear stresses below 100 Pa. Apparent viscosity is measured continuously as the sample is cooled at a rate of 1°C/h over the range −5 to −40°C, or to the temperature at which the viscosity exceeds 40 000 mPa·s (cP).
1.3 The measurements resulting from this test method are viscosity, the maximum rate of viscosity increase (Gelation Index), and the temperature at which the Gelation Index occurs.
1.4 Applicability to petroleum products other than engine oils has not been determined in preparing this test method.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.
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Designation: D5133 − 05(Reapproved 2011)
Standard Test Method for
Low Temperature, Low Shear Rate, Viscosity/Temperature
Dependence of Lubricating Oils Using a Temperature-
Scanning Technique
This standard is issued under the fixed designation D5133; 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 D4684Test Method for Determination of Yield Stress and
Apparent Viscosity of Engine Oils at Low Temperature
1.1 This test method covers the measurement of the appar-
ent viscosity of engine oil at low temperatures.
3. Terminology
-1
1.2 A shear rate of approximately 0.2 s is produced at
3.1 Definitions:
shear stresses below 100 Pa. Apparent viscosity is measured
3.1.1 apparent viscosity, n—theviscosityobtainedbyuseof
continuouslyasthesampleiscooledatarateof1°C/hoverthe
this test method.
range−5to−40°C,ortothetemperatureatwhichtheviscosity
3.1.1.1 Discussion—See3.1.6fordefinitionofviscosityand
exceeds 40 000 mPa·s (cP).
units.
1.3 The measurements resulting from this test method are
3.1.2 Newtonian oil, n—an oil that, at a given temperature,
viscosity, the maximum rate of viscosity increase (Gelation
exhibits a constant viscosity at all shear rates or shear stresses.
Index), and the temperature at which the Gelation Index
3.1.3 non-Newtonian oil, n—an oil that, at a given
occurs.
temperature,exhibitsaviscositythatvarieswithshearstressor
1.4 Applicability to petroleum products other than engine
shear rate.
oils has not been determined in preparing this test method.
3.1.4 shear rate, n—velocity gradient perpendicular to the
1.5 The values stated in SI units are to be regarded as the
direction of flow.
standard. The values given in parentheses are for information
3.1.4.1 Discussion—The SI unit for shear rate is the recip-
-1
only.
rocal second (1/s; also s ).
1.6 This standard does not purport to address all of the
3.1.5 shear stress, n—force per unit area in the direction of
safety concerns, if any, associated with its use. It is the
flow.
responsibility of the user of this standard to establish appro-
3.1.5.1 Discussion—TheSIunitforshearstressisthePascal
priate safety and health practices and determine the applica-
(Pa).
bility of regulatory limitations prior to use.
3.1.6 viscosity,n—thatpropertyofafluidwhichresistsflow.
3.1.6.1 Discussion—Viscosity is defined as the ratio of the
2. Referenced Documents
applied shear stress (force causing flow) and the shear rate
2.1 ASTM Standards:
(resultant velocity of flow per unit distance from a stationary
D341Practice for Viscosity-Temperature Charts for Liquid
surface wet by the fluid). Mathematically expressed:
Petroleum Products
viscosity 5shearstress/shearrateor, symbolically, η 5 τ/G (1)
D3829Test Method for Predicting the Borderline Pumping
Temperature of Engine Oil in which the symbols in the second portion of Eq 1 are
defined by the terms in the first portion of the equation.
The SI unit for viscosity used herein is milliPascal sec-
1 onds (mPa·s).
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 3
3.2 Definitions of Terms Specific to This Standard:
D02.07 on Flow Properties.
Current edition approved Jan. 1, 2011. Published February 2011. Originally
approved in 1990. Last previous edition approved in 2005 as D5133–05. DOI:
10.1520/D5133-05R11. The sole source of supply of the equipment and materials known to the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or committee at this time is Tannas Co., 4800 James Savage Rd., Midland, MI 48642.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM If you are aware of alternative suppliers, please provide this information toASTM
Standards volume information, refer to the standard’s Document Summary page on International Headquarters. Your comments will receive careful consideration at a
the ASTM website. meeting of the responsible technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5133 − 05 (2011)
3.2.1 air-binding oils—those engine oils whose borderline 3.2.10 Gelation Index reference oils, n—non-Newtonian
pumping temperatures are determined by a combination of oils chosen to give certain levels of Gelation Index as a check
gelation and viscous flow. on instrument performance .
3.2.2 borderline pumping temperature, n—that temperature 3.2.11 Gelation Index temperature, n—the temperature (t
at which an engine oil may have such poor flow characteristics inEq2)indegreesCelsiusatwhichtheGelationIndexoccurs.
that the engine oil pump may not be capable of supplying
3.2.12 pre-treatment sample heating bath, n—a water or air
sufficient lubricant to the engine.
bath to heat the samples for 1.5 to 2.0 h at 90 6 2°C before
3.2.3 calibration oil, n—Newtonianoilsdevelopedandused testing.
to calibrate the viscometer drive module over the viscosity
3.2.13 programmable liquid cold bath, n—a liquid bath
range required for this test method.
having a temperature controller capable of being programmed
3.2.3.1 Discussion—these calibration oils are specially
to run the calibration and the analysis portions of the test
blended to give sufficient sensitivity and range for the special
method.
viscometer head used.
3.2.14 temperature controller, n—a programmable device
3.2.4 computer-programmed automated analysis, n—use of
which, when properly programmed, ramps the temperature
modern techniques for acquiring analog data, converting these
upward or downward at a chosen rate or series of steps while
to digital values and using this information to automatically
simultaneously controlling temperature excursions.
record and analyze torque output from the viscometer drive
3.2.14.1 calibration program, n—a program to run the
module and to render this information into tabular data and
required series of temperatures at which the torque values
plotted relationships.
necessary to calibrate the viscometer drive module are col-
3.2.4.1 analog-to-digital (A-D) converter, n—a device for
lected and analyzed.
converting continuously produced electrical signals into dis-
3.2.14.2 test program, n—a program to run the test oil
crete numerical values capable of being analyzed by computer
analysis at 1°C/h temperature decrease.
technology.
3.2.14.3 hold program, n—a program to reach and hold the
3.2.5 critical pumpability temperature, n—the temperature
programmable liquid cold bath at −5°C.
in the viscometer bath at which an oil reaches a chosen critical
3.2.15 test cell, n—the combination of the rotor and stator.
pumpability viscosity (see 3.2.6).
Critical elements of the test cell are sketched in Fig. 1.
3.2.6 critical pumpability viscosity, n—thatapparentviscos-
ity believed to cause pumpability problems in an engine. This
apparent viscosity is chosen to test an oil for its critical
pumpability temperature.
3.2.7 flow-limited oils, n—those oils whose borderline
pumping temperatures are determined by viscous flow.
3.2.8 gelation, n—a rheological condition of an oil charac-
terized by a marked increase in the flow resistance over and
above the normal exponential increase of viscosity with
decreasingtemperature,particularlyatlowershearstressesand
temperatures.
3.2.8.1 Discussion—Gelation has been attributed to a pro-
cess of nucleation and crystallization of components of the
engine oil and the formation of a structure.
3.2.9 Gelation Index, n—the maximum value of the incre-
mental ratio
21@ log logη 2 log logη / log T 2log T # (2)
~ ! ~ ! ~ !
1 2 1 2
(in which η is dynamic viscosity and T is in degrees Kelvin)
over the temperature range scanned when the incremental
decrease in temperature is 1 K.
3.2.9.1 Discussion—The technique of deriving Gelation In-
dex was first developed and practiced collecting information
FIG. 1 Test Cell
from a strip-chart recording and applying the empirical
MacCoull-Walther-Wright equation (Test Method D341). For
further information, see Appendix X1.
3.2.15.1 rotor, n—a titanium rotor sized to give a compro-
mise of sensitivity and range to the determination of viscosity
Symposium on Low Temperature Lubricant Rheology Measurement and Rel-
and gelation using this test method.
evance to Engine Operation, ASTM STP 1143, Rhodes, R. B., ed., ASTM, 1992.
(1) stator, n—a precision-bore borosilicate glass tube, to
Selby, T.W., “The Use of the Scanning Brookfield Technique to Study the
whichameasuredamountofoilisaddedforthetestandwithin
Critical Degree of Gelation of Lubricants at Low Temperatures”, SAE Paper
910746, Society of Automotive Engineers, 1991. which the specially-made rotor turns.
D5133 − 05 (2011)
pumpability Test Methods D3829 and D4684, hold the sample in a
(2) stator collar, n—a clamp for the stator which also
quiescent state and generate the apparent viscosity of the sample at shear
positions it on the test cell alignment device.
-1
ratesrangingupto15sec andshearstressesupto525Paatapreviously
3.2.16 test cell alignment device , n—a special device used
selected temperature. Such difference in test parameters (shear rate, shear
to support the viscometer drive module while maintaining the
stress, sample motion, temperature scanning, and so forth) can lead to
stator and the rotor coaxial and vertical in regard to the
differences in the measured apparent viscosity among these test methods
with some test oils, particularly when other rheological factors associated
viscometer driveshaft. Later designs permit dry gas into the
with gelation are present. In addition, the three methods differ consider-
cell to prevent moisture and frost buildup.
ably in cooling rates.
3.2.17 test oil, n—any oil for which apparent viscosity is to
5.3 Gelation Index and Gelation Index Temperature—This
be determined using the procedure described by this test
test method has been further developed to yield parameters
method.
called the Gelation Index and Gelation Index temperature.The
3.2.18 viscometer drive module, n—the rotor drive and
first parameter is a measure of the maximum rate of torque
torque-sensing component of a rotational viscometer.
increasecausedbytherheologicalresponseoftheoilastheoil
3.2.19 viscometer module support, n—a part of the test cell is cooled slowly. The second parameter is the temperature at
alignment device supporting the viscometer drive module.
which the Gelation Index occurs.
4. Summary of Test Method
6. Apparatus
4.1 After pre-heating approximately 20 mLof the test oil in
6.1 TestCell,showninFig.1,consistingofamatchedrotor
a glass stator at 90°C for 1.5 to 2.0 h., the test cell containing
and a stator of the following critical dimensions:
the test oil is attached to a suitable viscometer drive module
6.1.1 Rotordimensionsfor:criticallengthis65.5mm(60.1
and the test cell immersed in a liquid cold bath and cooled at
mm) and critical diameter is 18.40 mm (60.02 mm).
1°C/h over the temperature range of −5 to −40°C. Data from
6.1.2 Stator dimensions for: critical diameter is 22.05 mm
the viscometer drive module is collected and fed to a comput-
(60.02 mm) at whatever length will satisfy the immersion
erized data assimilation program to determine the Gelation
depth when the upper oil level is a minimum of 15 mm below
Index, Gelation Index temperature, and Critical Pumpability
the cooling liquid level over the entire temperature range.
temperature for a selected viscosity such as 30 000 or 40 000
6.2 Viscometer Drive Modules, rotational viscometer drive
mPa·s (cP).
modules capable of producing an analog signal to an analog-
5. Significance and Use
to-digital converter or other analog signal data processor such
5.1 Significance of Low-Temperature, Low Shear Rate, En- as a strip-chart recorder.
gine Oil Rheology—Thelow-temperature,low-shearviscomet- 6.2.1 With the rotor and stator described in 6.1.1 and 6.1.2,
ric behavior of an engine oil determines whether the oil will the viscometer drive module shall be capable of measuring to
flow to the sump inlet screen, then to the oil pump, then to the at least 45 000 mPa·s (cP).
sitesintheenginerequiringlubricationinsufficientquantityto
6.3 Test Cell Alignment Device, simultaneously maintains a
prevent engine damage immediately or ultimately after cold
vertical axial alignment and reasonably consistent positioning
temperature starting.
of the rotor in the stator to give repeatable torque readout from
5.1.1 Two forms of flow problems have been identified,
test to test when setting up the apparatus for analysis.
flow-limited and air-binding behavior. The first form of flow
6.3.1 Viscometer Support, supports the viscometer drive
restriction, flow-limited behavior, is associated with the oil’s
module and aligns it vertically.
viscosity; the second, air-binding behavior, is associated with
6.3.2 Stator Collar, clamps the stator and supports it when
gelation.
the stator collar is attached to the viscometer support.
5.2 Significance of the Test Method—The temperature-
6.4 Ameansofprovidingadrygasatmosphereoverthetop
scanningtechniqueemployedbythistestmethodwasdesigned
of the test sample is necessary to prevent condensation and
to determine the susceptibility of the engine oil to flow-limited
freezing of water on the oil surface.
andair-bindingresponsetoslowcoolingconditionsbyprovid-
6.5 Programmable Liquid Cooling Bath, liquid bath ca-
ing continuous information on the rheological condition of the
4 ,5,7
pable of running either the calibration or the testing program
oil over the temperature range of use. In this way, both
withtemperaturecontrolof 60.1°Coverthetemperaturerange
viscometric and gelation response are obtained in one test.
desired at 1°C/h.
NOTE1—Thistestmethodisoneofthreerelatedtopumpabilityrelated
6.5.1 Temperature Controller, is set up to operate according
problems. Measurement of low-temperature viscosity by the two other
totwoprograms,theCalibrationprogramandthetestprogram.
At any temperature the controller modulates temperature
The test cell alignment device is covered by patents. Interested parties are
within 0.1°C of the desired value.
invited to submit information regarding the identification of alternatives to this
patented item to ASTM International Headquarters. Your comments will receive
6.6 Computer, Analog-to-Digital Converter, and Analysis
careful consideration at a meeting of the responsible technical committee, which
Program, means of receiving data from the viscometer drive
you may attend.
Shaub,H
...
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