Designation: D6896 − 14

Standard Test Method for

Determination of Yield Stress and Apparent Viscosity of
Used Engine Oils at Low Temperature1
This standard is issued under the fixed designation D6896; 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.

1. Scope* D5133 Test Method for Low Temperature, Low Shear Rate,
1.1 This test method covers the measurement of the yield Viscosity/Temperature Dependence of Lubricating Oils
stress and viscosity of engine oils after cooling at controlled Using a Temperature-Scanning Technique
rates over a period of 43 h or 45 h to a final test temperature of E563 Practice for Preparation and Use of an Ice-Point Bath
–20 °C or –25 °C. The precision is stated for test temperatures as a Reference Temperature
–20 °C and –25 °C. The viscosity measurements are made at a E644 Test Methods for Testing Industrial Resistance Ther-
shear stress of 525 Pa over a shear rate of 0.4 s-1 to 15 s-1. This mometers
test method is suitable for measurement of viscosities ranging E1137 Specification for Industrial Platinum Resistance Ther-
from 4000 mPa·s to >400 000 mPa·s, and is suitable for yield mometers
stress measurements of 7 Pa to >350 Pa. E2877 Guide for Digital Contact Thermometers
2.2 ISO Standards:3
1.2 This test method is applicable for used diesel oils. The ISO 17025 General Requirements for the Competence of
applicability and precision to other used or unused engine oils Testing and Calibration Laboratories
or to petroleum products other than engine oils has not been ISO Guide 34 General Requirements for the Competence of
determined. Reference Material Producers
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3. Terminology
standard. 3.1 Definitions:
1.3.1 Exception—This test method uses the SI based unit of 3.1.1 apparent viscosity, n—the determined viscosity ob-
milliPascal second (mPa·s) for viscosity which is equivalent to tained by use of this test method.
centiPoise (cP). 3.1.2 Digital Contact Thermometer (DCT), n—an electronic
1.4 This standard does not purport to address all of the device consisting of a digital display and associated tempera-
safety concerns, if any, associated with its use. It is the ture sensing probe.
responsibility of the user of this standard to establish appro- 3.1.2.1 Discussion—This device consists of a temperature
priate safety and health practices and determine the applica- sensor connected to a measuring instrument; this instrument
bility of regulatory limitations prior to use. measures the temperature-dependent quantity of the sensor,
computes the temperature from the measured quantity, and
2. Referenced Documents provides a digital output or display of the temperature, or both.
2.1 ASTM Standards:2 The temperature sensing probe is in contact with the material
D3829 Test Method for Predicting the Borderline Pumping whose temperature is being measured. This device is some-
Temperature of Engine Oil times referred to as a digital thermometer.
D4684 Test Method for Determination of Yield Stress and NOTE 1—Portable electronic thermometers (PET) is an acronym some-
Apparent Viscosity of Engine Oils at Low Temperature times used to refer to a subset of the devices covered by this definition.
3.1.3 Newtonian oil or fluid, n—an oil or fluid that at a given
1
This test method is under the jurisdiction of ASTM Committee D02 on temperature exhibits a constant viscosity at all shear rates or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of shear stresses.
Subcommittee D02.07 on Flow Properties.
Current edition approved July 1, 2014. Published August 2014. Originally 3.1.4 non-Newtonian oil or fluid, n—an oil or fluid that at a
approved in 2003. Last previous edition approved in 2012 as D6896 – 12. DOI: given temperature exhibits a viscosity that varies with chang-
10.1520/D6896-14.
2
ing shear stress or shear rate.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.

*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

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 D6896 − 14
3.1.5 shear rate, n—the velocity gradient in fluid flow. For rate, soak time, and temperature. Yield stress measurement by
a Newtonian fluid in a concentric cylinder rotary viscometer in this test method determines only whether the test oil has a yield
which the shear stress is measured at the inner cylinder surface stress of at least 35 Pa; a yield stress below 35 Pa is considered
(such as the apparatus described in 6.1), and ignoring any end to be insignificant for engine oils.
effects, the shear rate is given as follows:
2 ~ Ω ! R 2s
4. Summary of Test Method
γ̇ 5 (1) 4.1 A used engine oil sample is heated at 80 °C and then
R 2s 2 R 2r
4~π!R 2 vigorously agitated. The sample is then cooled at a pro-
s
5
t ~ R 2s 2 R 2r !
(2) grammed cooling rate to a final test temperature. A low torque
is applied to the rotor shaft to measure the yield stress. A higher
where: torque is then applied to determine the apparent viscosity of the
γ̇ = shear rate at the surface of the rotor in reciprocal sample.
seconds, s-1,
Ω = angular velocity, rad/s, 5. Significance and Use
Rs = stator radius, mm, 5.1 When an engine oil is cooled, the rate and duration of
Rr = rotor radius, mm, and cooling can affect its yield stress and viscosity. In this
t = time for one revolution of the rotor, s.
laboratory test, used engine oil is slowly cooled through a
For the specific apparatus described in 6.1, temperature range where wax crystallization is known to occur,
γ̇ 5 63/t (3) followed by relatively rapid cooling to the final test tempera-
ture. As in other low temperature rheological tests such as Test
3.1.6 shear stress, n—the motivating force per unit area for
Methods D3829, D4684, and D5133, a preheating condition is
fluid flow. For the rotary viscometer being described, the rotor
required to ensure that all residual waxes are solubilized in the
surface is the area under shear or the shear area.
oil prior to the cooldown (that is, remove thermal memory).
T r 5 9.81 M ~ R o 1R t ! 3 1026 (4) However, it is also known that highly sooted used diesel engine
Tr oils can experience a soot agglomerization phenomenon when
τ5 3 109 (5) heated under quiescent conditions. The current method uses a
2 ~ π ! R 2r h
separate preheat and agitation step to break up any soot
where:
agglomerization that may have occurred prior to cooldown.
Tr = torque applied to rotor, N·m, The viscosity of highly sooted diesel engine oils as measured
M = applied mass, g, in this test method have been correlated to pressurization times
Ro = radius of the shaft, mm, in a motored engine test (1).4
Rt = radius of the string, mm,
τ = shear stress at the rotor surface, Pa, and 5.2 Cooling Profiles:
h = height of the rotor, mm. 5.2.1 For oils to be tested at –20 °C and –25 °C, Table X1.1
For the dimensions given in 6.1.1, applies. The cooling profile described in Table X1.1 is based on
the viscosity properties of the ASTM Pumpability Reference
T r 5 31.7 M 3 1026 (6) Oils (PRO). This series of oils includes oils with normal
τ 5 3.5 M (7) low-temperature flow properties and oils that have been
3.1.7 viscosity, n—the ratio between the applied shear stress associated with low-temperature pumpability problems (2-7).
and rate of shear, sometimes called the coefficient of dynamic
viscosity. This value is thus a measure of the resistance to flow 6. Apparatus
of the liquid. The SI unit of viscosity is the pascal second 6.1 Mini-Rotary Viscometer5, an apparatus that consists of
(Pa·s). one or more viscometric cells in a temperature-controlled
3.2 Definitions of Terms Specific to This Standard: aluminum block. Each cell contains a calibrated rotor-stator
set. The rotor shall have a crossbar near the top of the shaft
3.2.1 calibration oils, n—those oils that establish the instru-
extending in both directions far enough to allow the locking pin
ment’s reference framework of apparent viscosity versus
(6.6) to stop rotation at successive half turns. Rotation of the
speed, from which the apparent viscosities of test oils are
rotor is achieved by an applied load acting through a string
determined.
wound around the rotor shaft.
3.2.2 test oil, n—any oil for which the apparent viscosity 6.1.1 The mini-rotary viscometric cell has the following
and yield stress are to be determined by this test method. typical dimensions:
3.2.3 used oil, n—an oil which has been used in an operating
engine.
4
The boldface numbers in parentheses refer to the list of references at the end of
3.2.4 yield stress, n—the shear stress required to initiate this standard.
flow. 5
The sole source of supply of the apparatus known to the committee at this time
is Cannon Instrument Co., P.O. Box 16, State College, PA 16804. If you are aware
3.2.4.1 Discussion—For all Newtonian fluids and some
of alternative suppliers, please provide this information to ASTM International
non-Newtonian fluids, the yield stress is zero. An oil can have Headquarters. Your comments will receive careful consideration at a meeting of the
a yield stress that is a function of its low-temperature cooling responsible technical committee,1 which you may attend.

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 D6896 − 14

Diameter of rotor 17.06 mm ± 0.08 mm Calibration Data 4 data points evenly distributed over the
Length of rotor 20.00 mm ± 0.14 mm range of –40 °C to –1 °C and included in cali-
Inside diameter of cell 19.07 mm ± 0.08 mm bration report.
Radius of shaft 3.18 mm ± 0.13 mm Calibration Report From a calibration laboratory with demon-
Radius of string 0.10 mm strated competency in temperature calibration
which is traceable to a national calibration
6.1.2 Cell Cap—A cover inserted into the top of the vis- laboratory or metrology standards body
cometer cell to minimize room air circulation into the cells is
NOTE 3—With respect to DCT probe immersion depth, a procedure to
required for thermometrically cooled instruments. The cell cap determine minimum depth can be found in Guide E2877, Section 5.3, or
is a stepped cylinder 38 mm 6 1 mm in length made of a low Test Methods E644, Section 7.
thermal conductivity material, for example, thermoplastic such
as acetyl copolymers that have known solvent resistivity and 6.4.1.1 The DCT calibration drift shall be checked at least
are suitable for use between the temperature ranges of this test annually by either measuring the ice point or against a
method. The top half is 28 mm 6 1 mm in diameter and the reference thermometer in a constant temperature bath at the
bottom half is 19 mm in diameter with a tolerance consistent prescribed immersion depth to ensure compliance with 6.4.1.
with the cell diameter. The tolerance on the bottom half is such With respect to an ice bath, Practice E563 provides guidance
that it will easily fit into cell but not allow cap to contact rotor on the preparation and use of an ice bath. However, for this use,
shaft. The piece has a center bore of 11 mm 6 1 mm. The cap variance from the specific steps, such as water source, is
is made in two halves to facilitate placement in the top of the permitted provided preparation is consistent. The basis for the
cell. variance is due to the reference being used to track change in
6.1.2.1 Cell caps shall not be used in the direct refrigeration calibration not verification.
instruments, since such use would block the flow of cold, dry NOTE 4—When a DCT’s calibration drifts in one direction over several
air into the stators to keep them frost-free. calibration checks, that is, ice point, it may be an indication of deteriora-
tion of the DCT.
6.2 Weights:
6.2.1 Yield Stress Measurement, a set of nine disks and a 6.4.2 For liquid-in-glass thermometers, LiG, two are re-
disk holder, each with a mass of 10 g 6 0.1 g. quired. One LiG shall be a calibrated 76 mm partial immersion
thermometer with a scale from +5 °C to 1 degree less than the
6.2.2 Viscosity Measurement, a mass of 150 g 6 1.0 g.
lowest test temperature in 0.2 °C subdivisions. This low
6.3 Temperature Control System, that will regulate the temperature LiG thermometer shall have a report of calibration
mini-rotary viscometer block temperature in accordance with showing the temperature deviation at each calibrated test
the temperature limits described in Table X1.1. temperature. The second LiG thermometer shall be a 76 mm
6.3.1 Temperature Profile—The temperature profile is fully partial immersion thermometer graduated from at least +20 °C
described in Table X1.1. to 90 °C in 1 °C subdivisions, which is used to verify the
preheat temperature.
6.4 Temperature Measuring Device—Use either a DCT
meeting the requirements described in 6.4.1 or liquid-in-glass 6.4.2.1 Calibration Check—Verify the low temperature
thermometers described in 6.4.2. A DCT or a calibrated low thermometer at least annually against a reference thermometer
temperature liquid-in-glass thermometer shall be used as the in a constant temperature bath or in an ice bath. The thermom-
thermometer for temperature measurement independent of the eter is to be insert to its immersion depth. If using an ice bath,
instrument’s temperature control, and shall be located in the the ice point reading is to be taken within 60 min after the
thermowell. thermometer has been at test temperature for at least 3 min. If
the corrected temperature reading deviates from the reference
NOTE 2—The display device and sensor must be correctly paired. thermometer or the ice point then repeat this calibration check.
Incorrect pairing will result in temperature measurement errors and If the thermometer deviates from the reference value on two
possibly irreversible damage to the electronics of the display. successive checks then a full thermometer recalibration is
6.4.1 Digital contact thermometer requirements: needed.
Criteria Minimum Requirements 6.4.2.2 Recalibration—A complete recalibration of the
DCT E2877 Class B liquid-in-glass thermometer, while permitted, is not necessary
Temperature range –45 °C to 100 °C
Display resolution 0.1 °C minimum, preferably 0.01 °C in order to meet the accuracy ascribed to liquid-in-glass
Sensor type RTD, such as a PRT or thermistor thermometer’s design until the thermometers corrected mea-
Sensor, 3 mm O.D. with an sensing element less than sured temperature deviates from the reference thermometer or
metal sheathed 30 mm in length to be used with a thermowell
sleeve, 6 mm O.D. × 58 mm long with a ~3 ice point by one scale division, or until five years has elapsed
mm hole in center. since the last full calibration.
Sensor, 6 mm O.D. with a sensing element less than
glass sheathed 12 mm in length 6.5 Supply of Dry Gas—A supply of dry filtered dry gas to
Display accuracy ±50 mK (±0.05 °C) for combined probe and minimize moisture condensation on the upper portions of the
sensor
Response time less than or equal to 25 s as defined in instrument.
Specification E1137 6.5.1 For thermoelectric cooled instruments, which use cell
Drift less than 50 mK (0.05 °C) per year
Calibration Error less than 50 mK (0.05 °C) over the range of caps, the dry gas supply is connected to the housing cover. The
intended use. supply of dry gas is discontinued when the cover is removed
Calibration Range –40 °C to 85 °C for the measurement phase of the test.

3
 D6896 − 14
6.6 Locking Pin—A device to keep the rotor from turning thermometer and the instrument’s measured temperature then
prematurely and able to stop the rotor at the nearest half adjust each temperature of the cooling program by the offset
revolution by interaction with the rotor crossbar. determined with the correction equation.
6.7 Sample Pre-treatment Oven, an oven capable of main- 9.2 Viscometer Cell Calibration—The calibration of each
taining a temperature of 80 °C 6 1 °C for a minimum of 2 h. viscometric cell (viscometer constants) can be determined with
the viscosity standard and the following procedure at –20 °C.
7. Reagents and Materials 9.2.1 Following the steps in 10.2 to prepare the cells for
7.1 Low Cloud-point Newtonian Oil, a calibration oil of calibration using the calibration oil as the sample.
approximately 30 Pa·s viscosity at –20 °C for calibration of the 9.2.2 Use either the calibration temperature profile for the
viscometric cells. The calibration oil shall be obtained from instrument which cools to –20 °C then holds for 2 h or,
suppliers complying with ISO Guide 34 and ISO 17025 with alternatively, the cooling profile given in Test Method D3829
traceability to a national metrology institute (NMI). for a –20 °C test temperature and follow the owner’s manual
instructions for the instrument to initiate the cooling profile
7.2 Methanol—Commercial or technical grade of dry program.
methanol is suitable for the cooling bath. 9.2.3 Place the thermometer in the thermometer well at least
7.3 Oil Solvent, commercial heptanes or similar solvent that 30 min prior to executing 9.2.5. See Note 5. This thermowell
evaporates without leaving a residue is suitable. (Warning— location is to be used for calibration and temperature monitor-
Flammable.) ing during the test procedure.
7.4 Acetone—A technical grade of acetone is suitable pro- 9.2.4 At the completion of the temperature profile and soak
vided it does not leave a residue upon evaporation. period, check that the test temperature is within 60.1 °C of the
(Warning—Flammable.) desired calibration temperature with a thermometer. If the
temperature meets the criteria remove the cell cover and
8. Sampling proceed.
9.2.5 Beginning with the cell farthest to the left, perform
8.1 A representative sample of test oil free from suspended step 10.8.
granular material and water is necessary to obtain valid 9.2.6 Repeat 9.2.5 for each of the remaining cells in
viscosity measurements. If the sample in its container is numerical order.
received below the dew-point temperature of the room, allow 9.2.7 Calculate the viscometer constant for each cell (rotor/
the sample to warm to room temperature before opening the stator combination) with the following equation:
container.
C 5 η o /t (8)
9. Calibration and Standardization where:
9.1 Temperature Control Calibration Procedure—Calibrate ηo = viscosity of the standard oil, mPa·s at –20 °C,
the MRV temperature control by comparing the instrument’s C = cell constant with 150 g mass, mPa, and
displayed temperature against a thermometer in the thermow- t = time for three complete revolutions, s.
ell. The thermometer used shall meet the requirements in 6.4. 9.2.8 If any cell has a calibration constant more than 10 %
9.1.1 Place 10 mL of a typical test fluid and rotor in each higher or lower than the average for the other cells, the fault
cell. Cell caps maybe used if available for the instrument. Place may be a problem with rotor operation. Examine rotor for
the cover on instrument. damage and recalibrate instrument.
9.1.2 Place the thermometer in the thermowell. See Note 5.
This thermowell is to be used for all temperature measurements 9.3 If corrected values for controller temperature and ther-
below 25 °C. mometer deviate by more than the tolerance, use X2.1 to assist
in determining the fault.
NOTE 5—Prior to inserting the thermometer or DCT probe in the
thermowell, place several drops (~3) of a heat transfer fluid such as 50/50 9.4 Oven—Check the calibration of the temperature sensing
water/ethylene glycol mix, CCS reference oil CL100 or a dewaxed low device by appropriate methods. The temperature should be
viscosity mineral oil in the thermowell. constant at 80 °C 6 1 °C.
9.1.3 Make at least four temperature measurements that are
at least 5 °C apart between –5 °C and the lowest test tempera- 10. Procedure
ture used to establish a calibration curve between the thermom- 10.1 Test Sample Preparation:
eter and the instrument’s temperature control. Make at least 10.1.1 Using suitable closed container, preheat the samples
two temperature measurements at every calibration tempera- in an oven to 80 °C 6 1 °C for 2.25 h. At the end of this time,
ture with at least 10 min between observations. remove the samples from the oven and allow to cool for 15 min
at room temperature.
NOTE 6—All temperatures in this test method refer to the actual
temperature as measured in the left thermowell and not necessarily the 10.1.2 Agitate each sample using vigorous mechanical or
indicated temperature. manual shaking for 60 s. Allow the samples to stand for a
9.1.4 Follow the instrument manufacturers instructions for minimum of 10 min to allow for settling.
correcting the instrument’s measured temperature. 10.2 Viscometric Cell Preparation:
Alternatively, establish a correction equation between the 10.2.1 If the cells are not clean, clean according to 10.10.

4
 D6896 − 14
10.2.2 Place 10 mL 61 mL of a test oil sample into a clean test temperature is more than 0.1 °C from the set point on two
cell. consecutive runs, the instrument’s temperature control must be
10.2.3 Repeat 10.2.2 until all test samples are in their cells. recalibrated according to 9.1.
NOTE 7—All cells should contain a fluid and rotor; if there are less than 10.6 If the temperature profile is within tolerance, proceed
a full set of samples to run, fill each of the unused cells with a typical test with measurements. If not, then abort the test and recalibrate
sample. temperature controller as in 9.1. See X2.1 – X2.3 for assistance
10.2.4 Place each rotor in its cell then place upper pivot pin in determining cause of temperature error.
in position, including those for any unused cells. 10.7 Measurement of the Yield Stress:
NOTE 8—Before inserting the rotors in the cells, inspect each rotor to be 10.7.1 Immediately prior to starting measurements, take the
sure that the shaft is straight, that the rotor surface is smooth and free from cell housing cover off the instrument.
dents, scratches, and other imperfections. For rotors with a bearing point 10.7.2 Yield Stress Determination—Starting with the cell
at the bottom of the shaft, ensure that the point is sharp and centered on
the rotor shaft. If these conditions are not met, repair or replace the rotor.
farthest to the left while facing the instrument, use the
following procedure for each cell in turn, bypassing the unused
10.2.5 Optional—Install a cell cap on all cells, including cells.
any unused cells. 10.7.3 Align the pulley wheel with the rotor shaft for the
10.2.6 For each cell, except any unused ones, place a loop of cell to be tested.
the nominal 700 mm long string over the crossbar. Hang the 10.7.4 Hang the string over the timing wheel such that the
string over the timing wheel with a small weight attached such string hangs past the front of the housing. Make sure that the
as a large paper clip. Wind the string around the shaft until the disk holder clears the edge of the bench during testing. (Do not
end is about 100 mm below the wheel. Do not overlap allow the rotor shaft to turn.)
windings. 10.7.5 For CMRV-3 and earlier models, follow the instruc-
NOTE 9—The strings can be pre-wound around the shafts before they tions in 10.7.6. For CMRV-4 or later models, if using the
are installed in 10.2.4. automatic timing devices, follow the instructions in 10.7.7. If
10.2.6.1 Engage the locking pin to prevent the rotor from manual timing measurements are used, follow the instructions
turning. in 10.7.6.
10.2.6.2 Lay the remaining string over the top of the bearing 10.7.6 Visually observe the rotor for movement of the
plate letting it hang over the back of the plate. cross-arm. (Do not measure yield stress by way of the
10.2.6.3 Repeat 10.2.6 – 10.2.6.2 until all cells with samples electronic optics.)
to be measured are prepared. 10.7.6.1 For instruments not equipped with locking pins,
10.2.7 Place the housing cover over the viscometric cells. carefully, so as not to disturb the gel structure, attach a disk
10.2.8 Connect the dry gas supply to the housing cover, as holder to the string and gently suspend the weight on the string.
noted in 6.5. Set the dry gas flow to approximately 1 L/h. Proceed to 10.7.6.3.
Increase or decrease the flow as necessary to minimize frost or 10.7.6.2 For instruments equipped with locking pins, sus-
moisture condensation around the cells. pend the disk holder on the string, then raise the locking pin.
10.7.6.3 If the end of the cross-arm does not move at least
10.3 Select the cooling profile for the desired test tempera- 3 mm in 15 s (approximately twice the diameter of the
ture and follow the instrument instructions to initiate the cross-arm or 13° of rotation) then record that the sample has
program. Table X1.2 lists the nominal times to reach a yield stress. Proceed to 10.7.6.4. If movement is detected,
particular test temperature. record weight and proceed to 10.8.
10.3.1 If the profile is not available, enter it using the 10.7.6.4 If no movement is detected, for instruments with-
custom profile part of the software program. The instrument out locking pins, hold disk holder assembly and add a disk to
manual provides instructions on adding custom profiles. The it, then proceed with 10.7.6.3. If equipped with locking pins,
entries for a custom program will be found in Table X1.3. lower the locking pin to re-engage cross-arm. Add a disk to the
10.4 Place the thermometer in the thermowell at least 30 disk holder, raise the locking pin, and proceed with 10.7.6.3.
min prior to completion of the cooling profile (see Note 5). The NOTE 10—The total amount of weight available for measurement of
same thermowell location is to be used for all measurements yield stress is normally 100 g; if no movement is detected with this
and must be the same one as was used in the calibration. weight, yield stress would be recorded as >350 Pa.
10.5 At the completion of the cooling profile, check the 10.7.7 The operator shall follow the on-screen instructions
time-temperature plot for the run to ensure that the time- adding additional disks to disk holder.
temperature profile is within tolerance and that the test tem- 10.7.7.1 For instruments with locking pins, suspend disk
perature as measured in the thermowell is within 60.2 °C of holder on string, press the flashing start button then immedi-
the final test temperature. Both of these checks may be done ately raise the locking pin and follow on-screen instructions.
automatically by the control software incorporated in some 10.7.7.2 If an additional disk is requested, capture cross-arm
instruments. Final test temperature is to be verified indepen- in locking pin, add one additional disk, and follow the
dently from the instrument’s temperature control using a on-screen instructions. Press the flashing start button, and
thermometer that has been in the thermowell for at least 30 min immediately raise the locking pin. Repeat procedure until no
prior to reaching the test temperature. See Note 5. If the final additional disks are requested. Proceed to 10.8.

5
 D6896 − 14
10.7.7.3 For instruments without locking pins, carefully 11. Calculation of Yield Stress and Apparent Viscosity
suspend and hold the disk holder on the string without jerking 11.1 Yield stress is given by the following equation:
rotor and follow on-screen instructions. Press the flashing start
button, and immediately release the disk holder. Ys 5 3.5 M (9)
10.7.7.4 If no movement is detected, carefully lift the disk where:
holder to relieve load and add a disk as indicated on computer Ys = yield stress, Pa, and
screen without pulling on string and follow on-screen instruc- M = applied mass, g.
tions. Press the flashing start button and immediately release
disk holder. Repeat procedure until no additional disks are 11.2 The apparent viscosity is given by the following
requested. Proceed with 10.8. equation when using the cell constant obtained in Eq 8:
η a 5 C t 3/r (10)
NOTE 11—When the load is first applied, some oils may show
momentary movement of the cross-arm. If there is no further movement of where:
the cross-arm for 15 s, disregard the initial movement.
ηa = apparent viscosity, mPa·s,
10.8 Measurement of Apparent Viscosity: C = cell constant obtained in Eq 8,
10.8.1 For CMRV-3 and earlier models follow the instruc- t = time for number (r) of complete revolutions of the rotor,
tions in 10.8.2. For CMRV-4 or later models, if using the and
automatic timing devices, follow the instructions in 10.8.3. If r = number of revolutions timed.
manual timing measurements are used, follow the instructions
in 10.8.2. 12. Report
10.8.2 Attach a 150 g mass to the string and slowly suspend 12.1 Apparent Viscosity and Yield Stress—For used oils,
it on the string. Start the timer when the cross-arm of the rotor report the final test temperature and both apparent viscosity and
shaft points directly forward and continue timing in accordance yield stress.
with the following constraints. 12.2 Yield Stress—Report as less than the value at which
10.8.2.1 If the first half-revolution requires less than 10 s, rotation was observed.
measure and record the time for the first three revolutions, and
proceed to 10.9. 12.3 Apparent Viscosity—Report as follows:
10.8.2.2 If the first half-revolution requires 10 s or greater, 12.3.1 If the apparent viscosity is less than 5000 mPa·s, then
measure and record the time for the first revolution and identify report the apparent viscosity as less than 5000 mPa·s.
it as the time for one revolution; then proceed to 10.9. 12.3.2 If the apparent viscosity is between 5000 mPa·s and
100 000 mPa·s, then report the apparent viscosity to the nearest
10.8.2.3 If the first revolution has not been completed in
100 mPa·s.
60 s, end the measurement. Record the time as greater than 60
12.3.3 If the apparent viscosity is between 100 000 mPa·s
s for one revolution, then proceed to 10.9, reporting that the
and 400 000 mPa·s, then report the apparent viscosity to the
viscosity is greater than the value calculated in 11.2.
nearest 1000 mPa·s.
10.8.2.4 If the time for the first three revolutions is less than
12.3.4 If the apparent viscosity is greater than 400 000
4 s, record the time as less than 4 s, then proceed to 10.9,
mPa·s, then the apparent viscosity should be reported as greater
reporting that the viscosity is less than the value calculated in
than 400 000 mPa·s.
11.2.
12.3.5 When employing software that provides three viscos-
10.8.3 Follow on-screen instructions, press start button and ity values, the first value shall be reported as the apparent
slowly suspend the weight on the string. Timing will automati- viscosity by this test method, D6896. If desired, report all three
cally begin with first movement. Do not remove the mass while values, exercising care to also report the sequence of the
the viscosity LED on the instrument is flashing. Once the time values. Never report a value that is the average of the three
and viscosity are displayed or the viscosity LED stops flashing, measured values.
proceed to 10.9.
10.9 Repeat 10.7 and 10.8 for each of the remaining cells in 13. Precision and Bias6
order from left to right. 13.1 Precision (Used Diesel Engine Oils)—The precision of
10.10 Cleaning: this test method as determined by the statistical examination of
10.10.1 After all of the cells have been completed, exit the interlaboratory test results is as follows:
cooling program and turn on the heater to warm the viscomet- 13.1.1 Yield Stress:
ric cells to room temperature or somewhat higher. The tem- 13.1.1.1 Repeatability—The difference between successive
perature shall not exceed 50 °C. results obtained by the same operator with the same apparatus
10.10.2 Remove the upper rotor pivots and the rotors. under constant operating conditions on identical test material
10.10.3 With a vacuum, remove the oil samples and rinse would, in the long run, in the normal and correct operation of
the cells with an oil solvent several times, followed by two the test method, exceed the following values only in one case
washings with acetone. Use a vacuum to remove the solvent in twenty:
from the cells after each rinse and allow the acetone to
evaporate to dryness after the final rinse. 6
Supporting data have been filed at ASTM International Headquarters and may
10.10.4 Clean the rotors in a similar manner. be obtained by requesting Research Report RR:D02-1442.

6
 D6896 − 14

Test Temperature, °C Repeatability, Pa 13.1.2.2 Reproducibility—The difference between two

–20 0.543·(X+1) single and independent results obtained by different operators
–25 0.504·(X+1)
working in different laboratories on identical test material
where: would, in the long run, exceed the following values only in one
X = mean value, Pa. case in twenty. The reproducibility as a percent of the mean
13.1.1.2 Reproducibility—The difference between two apparent viscosity is shown as follows:
single and independent results obtained by different operators Test Temperature, °C Repeatability, % of Mean
–20 0.186·X
working in different laboratories on identical test material –25 0.209·X
would, in the long run, exceed the following values only in one
case in twenty. 13.1.3 The interlaboratory program included six laborato-
Test Temperature, °C Repeatability, Pa
ries and seven test oils at the –20 °C and –25 °C test tempera-
–20 0.926·(X+1) tures. The used oils included end-of-test drain samples from
–25 0.773·(X+1) Mack T8, Mack T8E, Cummins M11-EGR and Mack T10
where: engine tests, with soot loadings (as measured by thermogravi-
X = mean value, Pa. metric analysis) ranging from approximately 5 to 9 %.7
NOTE 12—When no yield stress is detected (movement with 10 g 13.2 Bias—Since there is no accepted reference material
weight), X = 0.
suitable for determining the bias for this test method, no
13.1.2 Apparent Viscosity: statement on bias is being made.
13.1.2.1 Repeatability—The difference between successive
results obtained by the same operator with the same apparatus 14. Keywords
under constant operating conditions on identical test material
would, in the long run, in the normal and correct operation of 14.1 low temperature flow properties; low temperature vis-
the test method, exceed the following values only in one case cosity; mini-rotary viscometer; pumping viscosity; used diesel
in twenty. The repeatability as a percent of the mean apparent engine oil; viscosity; yield stress
viscosity is shown as follows:
Test Temperature, °C Repeatability, % of Mean
–20 0.0879·X 7
Supporting data have been filed at ASTM International Headquarters and may
–25 0.0616·X be obtained by requesting Research Report RR:D02-1517.

APPENDIXES

(Nonmandatory Information)

X1. TEMPERATURE PROFILES FOR TEST TEMPERATURES

X1.1 See Tables X1.1-X1.3.

7
 D6896 − 14
TABLE X1.1 Temperature Profile for Test Temperatures –20 °C to –25 °C
Segment TemperatureA Allowable
Segment Time, Temperature
h:min Final, Change,B
Beginning, °C Rate of Change, °C/h
°C °C
nominally 0:02 above 20 to 25.0
nominally 0:21 25.0 to 1.5
nominally 0:17 1.5 to 0.0
nominally 0:03 0.0 to –3.0
nominally 0:07 -3.0 to –4.0 8.5 ±0.5
nominally 0:10 -4.0 to –5.0 6.0 ±0.2
6:00 -5.0 to –8.0 0.5 ±0.2
36:00 -8.0 to –20.0 0.33 ±0.2
Hold at this point for –20 °C test temperatureC
2:00 -20.0 to –25.0 2.5 ±0.2
Hold at this point for –25 °C test temperatureC
A
If the dual control loop concept is used, the bath set point temperatures should be 5 °C below the corresponding block temperature desired. The maximum bath
temperature shall not exceed –5 °C.
B
Holding the temperature variation to less than ±0.1 °C improves the precision and reproducibility of your viscosity measurements.
C
The measurement of yield stress and apparent viscosity are to be made within 30 min of reaching the test temperature.

TABLE X1.2 Nominal Elapsed Time to Test Temperature

Test Temperature, °C Nominal Elapsed Time, h
–20 43
–25 45

TABLE X1.3 Custom Profile Values

Elapsed Temperature
Test Temperature, Test Temperature,
Time, Tolerance,
of –20.0 °C of –25.0 °C
hh:mm °C
00:02 25.0 25.0 ...
00:23 1.5 1.5 ...
00:40 0.0 0.0 ...
00:43 –3.0 –3.0 ...
00:50 –4.0 –4.0 0.5
01:00 –5.0 –5.0 0.2
07:00 –8.0 –8.0 0.2
43:00 –20.0 –20.0 0.2
45:00 –25.0 0.2

X2. SUPPORTING OPERATIONAL INFORMATION

X2.1 If the final temperature is in error in either direction by month. Other heat transfer can be used but should be similar to
more than 0.2 °C, do the following before starting another methanol in viscosity and heat capacity at the bath temperature.
analysis. X2.1.5 Is the bath refrigeration working properly?
X2.1.1 Check the thermometer calibration. For liquid in X2.1.6 If manually programmed or using a custom profile,
glass thermometers, check the ice point. An error in the ice examine the temperature profile program for an error and make
point usually indicates air in the thermometer bulb or in the the appropriate corrections.
column of liquid. X2.2 The simplest way to check a liquid in glass thermom-
X2.1.2 Check temperature sensor of the temperature con- eter calibration is to check its ice point. Other calibration
troller for accuracy, in accordance with 8.1. sources are available for both liquid in glass and electronic
temperature sensor and are appropriate if they are sufficiently
X2.1.3 Determine if the coolant is flowing and if there is accurate.
adequate coolant in the reservoir.
X2.3 The software for controlling temperature creates a
X2.1.4 For cold sources operating below –20 °C, replace temperature log during the test. Inspect the recorded cooling
methanol if wet, as indicated by ice crystals in the top of the profile temperature data for temperature deviations greater than
cold source reservoir. Cold methanol absorbs water, and as it those permitted in Table X1.1. Verify that the cooling rates
absorbs water, its cooling capacity decreases. In high humidity during the test are in conformance with those in Table X1.1 for
areas it may be necessary to change the methanol once a temperatures below –4 °C.

8
 D6896 − 14

REFERENCES

(1) Wells, J., Minutes of the Heavy Duty Engine Oil Classification Panel Pumpability,” SAE Paper No. 821206, Society of Automotive Engi-
Meeting, May 10, 2001, Orlando, FL. neers (SAE), Warrendale, PA.
(2) Stambaugh, R. L., and O’Mara, J. H., “Low Temperature Flow (5) Smith, M. F., Jr., “Better Prediction of Engine Oil Pumpability
Properties of Engine Oils,” SAE Paper No. 821247 or 820509, Through a More Effective MRV Cooling Cycle,” SAE Paper No.
Society of Automotive Engineers (SAE), Warrendale, PA. 831714, Society of Automotive Engineers (SAE), Warrendale, PA.
(3) Shaub, H., Smith, M. F., Jr., and Murphy, C. K., “Predicting Low (6) Henderson, K. O., Manning, R. E., May, C. J., and Rhodes, R. B.,
Temperature Engine Oil Pumpability with the Mini-Rotary “New Mini-Rotary Viscometer Temperature Profiles That Predict
Viscometer,” SAE Paper No. 790732, published in SAE SP-460, Engine Oil Pumpability,” SAE Paper No. 850443, Society of Auto-
Society of Automotive Engineers (SAE), Warrendale, PA and ASTM motive Engineers (SAE), Warrendale, PA.
STP-621-S4, ASTM International, W. Conshohocken, PA. (7) Shaub, Hal, Editor, Oil Flow Studies at Low Temperature in Modern
(4) Stewart, R. M., Shaub, H., Smith, M. F., Jr., and Selby, T. W., Engines, ASTM STP 1388, ASTM International, W. Conshohocken,
“Summary of ASTM Activities on Low Temperature Engine Oil PA.

SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D6896 – 12) that may impact the use of this standard. (Approved July 1, 2014.)

(1) Revised specific provisions for a digital contact thermom- (3) Revised Referenced Documents.
eter. (4) Revised definitions.
(2) Revised Calibration, Measurement, and Calculation sec- (5) Revised Materials.
tions. (6) Revised Appendix.

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