ASTM D5133-99
(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
SCOPE
1.1 This test method was developed to measure 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 mPas (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 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.
1.6 All terms in this test method are in SI units.
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Designation: D 5133 – 99 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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 D 5133; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope exhibits a constant viscosity at all shear rates or shear stresses.
3.1.3 non-Newtonian oil, n—an oil that, at a given tempera-
1.1 This test method was developed to measure the apparent
ture, exhibits a viscosity that varies with shear stress or shear
viscosity of engine oil at low temperatures.
-1
rate.
1.2 A shear rate of approximately 0.2 s is produced at
3.1.4 shear rate, n—velocity gradient perpendicular to the
shear stresses below 100 Pa. Apparent viscosity is measured
direction of flow.
continuously as the sample is cooled at a rate of 1°C/h over the
3.1.4.1 Discussion—The SI unit for shear rate is the recip-
range −5 to −40°C, or to the temperature at which the viscosity
-1
rocal second (1/s; also s ).
exceeds 40 000 mPa·s (cP).
3.1.5 shear stress, n—force per unit area in the direction of
1.3 The measurements resulting from this test method are
flow.
viscosity, the maximum rate of viscosity increase (Gelation
3.1.5.1 Discussion—The SI unit for shear stress is the
Index) and the temperature at which the Gelation Index occurs.
Pascal (Pa).
1.4 Applicability to petroleum products other than engine
3.1.6 viscosity, n—that property of a fluid which resists
oils has not been determined in preparing this test method.
flow.
1.5 This standard does not purport to address all of the
3.1.6.1 Discussion—Viscosity is defined as the ratio of the
safety concerns, if any, associated with its use. It is the
applied shear stress (force causing flow) and the shear rate
responsibility of the user of this standard to establish appro-
(resultant velocity of flow per unit distance from a stationary
priate safety and health practices and determine the applica-
surface wet by the fluid). Mathematically expressed:
bility of regulatory limitations prior to use.
1.6 All terms in this test method are in SI units. viscosity 5 shear stress/shear rate or, symbolically,h5t/G (1)
in which the symbols in the second portion of Eq 1 are
2. Referenced Documents
defined by the terms in the first portion of the equation. The SI
2.1 ASTM Standards:
unit for viscosity used herein is milliPascal seconds (mPa·s).
D 341 Test Method for Viscosity-Temperature Charts for 4
3.2 Definitions of Terms Specific to This Test Method:
Liquid Petroleum Products
3.2.1 air-binding oils—those engine oils whose borderline
D 3829 Test Method for Predicting the Borderline Pumping
pumping temperatures are determined by a combination of
Temperature of Engine Oils
gelation and viscous flow.
D 4684 Test Method for Determination of Yield Stress and
3.2.2 borderline pumping temperature, n—that temperature
Apparent Viscosity of Engine Oils at Low Temperature
at which an engine oil may have such poor flow characteristics
that the engine oil pump may not be capable of supplying
3. Terminology
sufficient lubricant to the engine.
3.1 Definitions:
3.2.3 calibration oil, n—Newtonian oils developed and
3.1.1 apparent viscosity, n—the viscosity obtained by use of
used to calibrate the viscometer drive module over the viscos-
this test method.
ity range required for this test method.
3.1.1.1 Discussion—See 3.1.6 for definition of viscosity and
3.2.3.1 Discussion—these calibration oils are specially
units.
blended to give sufficient sensitivity and range for the special
3.1.2 Newtonian oil, n—an oil that, at a given temperature,
viscometer head used.
3.2.4 computer-programmed automated analysis, n—use of
modern techniques for acquiring analog data, converting these
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
to digital values and using this information to automatically
D02.070C on Low-Temperature Rheology of Non-Newtonian Fluids.
Current edition approved Apr. 10, 1999. Published June 1999. Originally
published as D 5133 – 90. Last previous edition D 5133 – 96.
2 4
Annual Book of ASTM Standards, Vol. 05.01. Equipment and materials for this method are available from Tannas Co., 4800
Annual Book of ASTM Standards, Vol. 05.02. James Savage Rd., Midland, MI 48642.
D 5133
record and analyze torque output from the viscometer drive necessary to calibrate the viscometer drive module are col-
module and to render this information into tabular data and lected and analyzed.
plotted relationships. 3.2.14.2 test program, n—a program to run the test oil
3.2.4.1 analog-to-digital (A-D) converter, n—a device for analysis at 1°C/h temperature decrease.
converting continuously produced electrical signals into dis- 3.2.14.3 hold program, n—a program to reach and hold the
crete numerical values capable of being analyzed by computer programmable liquid cold bath at −5°C.
technology. 3.2.15 test cell, n—the combination of the rotor and stator.
3.2.5 critical pumpability temperature, n—the temperature Critical elements of the test cell are sketched in Fig. 1.
in the viscometer bath at which an oil reaches a chosen critical 3.2.15.1 rotor, n—a titanium rotor sized to give a compro-
pumpability viscosity (see 3.2.6). mise of sensitivity and range to the determination of viscosity
3.2.6 critical pumpability viscosity, n—that apparent viscos- and gelation using this test method.
ity believed to cause pumpability problems in an engine. This (a) stator, n—a precision-bore borosilicate glass tube, to
apparent viscosity is chosen to test an oil for its critical which a measured amount of oil is added for the test and within
pumpability temperature. which the specially-made rotor turns.
3.2.7 flow-limited oils, n—those oils whose borderline (b) stator collar, n—a clamp for the stator which also
pumping temperatures are determined by viscous flow. positions it on the test cell alignment device.
3.2.8 gelation, n—a rheological condition of an oil charac- 3.2.16 test cell alignment device , n—a special device used
terized by a marked increase in the flow resistance over and to support the viscometer drive module while maintaining the
above the normal exponential increase of viscosity with stator and the rotor coaxial and vertical in regard to the
decreasing temperature, particularly at lower shear stresses and viscometer driveshaft. Later designs permit dry gas into the
temperatures. cell to prevent moisture and frost buildup.
3.2.8.1 Discussion—Gelation has been attributed to a pro- 3.2.17 test oil, n—any oil for which apparent viscosity is to
cess of nucleation and crystallization of components of the be determined using the procedure described by this test
engine oil and the formation of a structure. method.
3.2.9 Gelation Index, n—the maximum value of the incre- 3.2.18 viscometer drive module, n—the rotor drive and
mental ratio torque-sensing component of a rotational viscometer.
3.2.19 viscometer module support, n—a part of the test cell
21@~log log h !2~log log h !/~log T 2 log T !# (2)
1 2 1 2
alignment device supporting the viscometer drive module.
(in which h is dynamic viscosity and T is in degrees Kelvin)
over the temperature range scanned when the incremental
4. Summary of Test Method
decrease in temperature is 1 K.
4.1 After pre-heating approximately 20 mL of the test oil in
3.2.9.1 Discussion—The technique of deriving Gelation
Index was first developed and practiced collecting information
The test cell alignment device is covered by patents. Interested parties are
from a strip-chart recording and applying the empirical
invited to submit information regarding the identification of alternatives to this
MacCoull-Walther-Wright equation (Test Method D 341 ). For
patented item to ASTM Headquarters. Your comments will receive careful consid-
further information, see Appendix X1.
eration at a meeting of the responsible technical committee, which you may attend.
3.2.10 Gelation Index reference oils, n—non-Newtonian
oils chosen to give certain levels of Gelation Index as a check
on instrument performance .
3.2.11 Gelation Index temperature, n—the temperature (t
in Eq 2) in degrees Celsius at which the Gelation Index occurs.
3.2.12 pre-treatment sample heating bath, n—a water or air
bath to heat the samples for 1.5 h at 90 6 2°C before testing.
3.2.13 programmable liquid cold bath, n—a liquid bath
having a temperature controller capable of being programmed
to run the calibration and the analysis portions of the test
method.
3.2.14 temperature controller, n—a programmable device
which, when properly programmed, ramps the temperature
upward or downward at a chosen rate or series of steps while
simultaneously controlling temperature excursions.
3.2.14.1 calibration program, n—a program to run the
required series of temperatures at which the torque values
Symposium on Low Temperature Lubricant Rheology Measurement and Rel-
evance to Engine Operation, ASTM STP 1143, Rhodes, R. B., ed., ASTM, 1992.
Selby, T.W., “The Use of the Scanning Brookfield Technique to Study the
Critical Degree of Gelation of Lubricants at Low Temperatures”, SAE Paper
910746, Society of Automotive Engineers, 1991. FIG. 1 Test Cell
D 5133
a glass stator at 90°C for 1.5 h., the test cell containing the test 6.1.2 Stator dimensions for: critical diameter is 22.05 mm
oil is attached to a suitable viscometer drive module and the (6 0.02 mm) at whatever length will satisfy the immersion
test cell immersed in a liquid cold bath and cooled at 1°C/h depth when the upper oil level is a minimum of 15 mm below
over the temperature range of −5 to −40°C. Data from the the cooling liquid level over the entire temperature range.
viscometer drive module is collected and fed to a computerized 6.2 Viscometer Drive Modules, rotational viscometer drive
data assimilation program to determine the Gelation Index, modules capable of producing an analog signal to an analog-
Gelation Index temperature, and Critical Pumpability tempera- to-digital converter or other analog signal data processor such
ture for a selected viscosity such as 30 000 or 40 000 mPa·s as a strip-chart recorder.
(cP). 6.2.1 With the rotor and stator described in 6.1.1 and 6.1.2,
the viscometer drive module shall be capable of measuring to
5. Significance and Use
at least 45 000 mPa·s (cP).
5.1 Significance of Low-Temperature, Low Shear Rate, En- 6.3 Test Cell Alignment Device, simultaneously maintains a
vertical axial alignment and reasonably consistent positioning
gine Oil rheology—The low-temperature, low-shear viscomet-
ric behavior of an engine oil determines whether the oil will of the rotor in the stator to give repeatable torque readout from
test to test when setting up the apparatus for analysis.
flow to the sump inlet screen, then to the oil pump, then to the
sites in the engine requiring lubrication in sufficient quantity to 6.3.1 Viscometer Support, supports the viscometer drive
module and aligns it vertically.
prevent engine damage immediately or ultimately after cold
temperature starting. 6.3.2 Stator Collar, clamps the stator and supports it when
the stator collar is attached to the viscometer support.
5.1.1 Two forms of flow problems have been identified ,
6.4 A means of providing a dry gas atmosphere over the top
flow-limited and air-binding behavior. The first form of flow
restriction, flow-limited behavior, is associated with the oil’s of the test sample is necessary to prevent condensation and
freezing of water on the oil surface.
viscosity; the second, air-binding behavior, is associated with
gelation. 6.5 Programmable Liquid Cooling Bath, liquid bath ca-
pable of running either the calibration or the testing program
5.2 Significance of the Test Method—The temperature-
scanning technique employed by this test method was designed with temperature control of 6 0.1°C over the temperature
range desired at 1°C/h.
to determine the susceptibility of the engine oil to flow-limited
and air-binding response to slow cooling conditions by provid- 6.5.1 Temperature Controller, is set up to operate according
to two programs, the Calibration program and the test program.
ing continuous information on the rheological condition of the
, ,
5 6 8
oil over the temperature range of use . In this way, both At any temperature the controller modulates temperature
within 0.1°C of the desired value.
viscometric and gelation response are obtained in one test.
6.6 Computer, Analog-to-Digital Converter, and Analysis
NOTE 1—This test method is one of three related to pumpability related
Program, means of receiving data from the viscometer drive
problems. Measurement of low-temperature viscosity by the two other
module and converting this data into the desired information.
pumpability Test Methods D 3829 and D 4684, hold the sample in a
6.7 Sample Pre-treatment Water or Air Bath, a program-
quiescent state and generate the apparent viscosity of the sample at shear
-1
rates ranging up to 15 sec and shear stresses up to 525 Pa at a previously
mable water or air bath for both precise control of the test oils
selected temperature. Such difference in test parameters (shear rate, shear
at 90 6 2°C and immersion time after the sample reaches
stress, sample motion, temperature scanning, and so forth) can lead to
pre-treatment temperature.
differences in the measured apparent viscosity among these test methods
6.8 Calibrated Partial-Immersion Mercury Thermometer, an
with some test oils, particularly when other rheological factors associated
ASTM 34C thermometer, calibrated at 90°C and reading to 6
with gelation are present. In addition, the three methods differ consider-
0.2°C.
ably in cooling rates.
7. Materials
5.3 Gelation Index and Gelation Index Temperature—This
test method has been further developed to yield parameters
7.1 Calibration Oil, a Newtonian calibration oil of specified
called the Gelation Index and Gelation Index temperature. The
dynamic viscosity and viscosity index over a temperature range
first parameter is a measure of the maximum rate of torque
of −5 to −35°C.
increase caused by the rheological response of the oil as the oil
7.2 Gelation Index Reference Oils, GIR-Series, Non-
is cooled slowl
...
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