This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4684 − 20a

Standard Test Method for

Determination of Yield Stress and Apparent Viscosity of
Engine Oils at Low Temperature1
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 U.S. Department of Defense.

1. Scope* 1.5 The values stated in SI units are to be regarded as

standard. No other units of measurement are included in this
1.1 This test method covers the measurement of the yield
standard.
stress and viscosity of engine oils after cooling at controlled
1.5.1 Exception—This test method uses the SI based unit of
rates over a period exceeding 45 h to a final test temperature
milliPascal second (mPa·s) for viscosity which is equivalent to,
between –10 °C and –40 °C. The precision is stated for test
centiPoise (cP).
temperatures from –40 °C to –15 °C. The viscosity measure-
ments are made at a shear stress of 525 Pa over a shear rate of 1.6 This standard does not purport to address all of the
0.4 s–1 to 15 s–1. The viscosity as measured at this shear stress safety concerns, if any, associated with its use. It is the
was found to produce the best correlation between the tem- responsibility of the user of this standard to establish appro-
perature at which the viscosity reached a critical value and priate safety, health, and environmental practices and deter-
borderline pumping failure temperature in engines. mine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accor-
1.2 This test method contain two procedures: Procedure A dance with internationally recognized principles on standard-
incorporates several equipment and procedural modifications ization established in the Decision on Principles for the
from Test Method D4684–02 that have shown to improve the Development of International Standards, Guides and Recom-
precision of the test, while Procedure B is unchanged from Test mendations issued by the World Trade Organization Technical
Method D4684–02. Additionally, Procedure A applies to those Barriers to Trade (TBT) Committee.
instruments that utilize thermoelectric cooling technology or
direct refrigeration technology of recent manufacture for in- 2. Referenced Documents
strument temperature control. Procedure B can use the same 2.1 ASTM Standards:2
instruments used in Procedure A or those cooled by circulating D3829 Test Method for Predicting the Borderline Pumping
methanol. Temperature of Engine Oil
D8278 Specification for Digital Contact Thermometers for
1.3 Procedure A of this test method has precision stated for
Test Methods Measuring Flow Properties of Fuels and
a yield range from less than 35 Pa to 210 Pa and apparent
Lubricants
viscosity range from 4300 mPa·s to 270 000 mPa·s. The test
E563 Practice for Preparation and Use of an Ice-Point Bath
procedure can determine higher yield stress and viscosity
as a Reference Temperature
levels.
2.2 ISO Standard:3
1.4 This test method is applicable for unused oils, some- ISO 17025 General Requirements for the Competence of
times referred to as fresh oils, designed for both light duty and Testing and Calibration Laboratories
heavy duty engine applications. It also has been shown to be ISO Guide 34 General Requirements for the Competence of
suitable for used diesel and gasoline engine oils. The applica- Reference Material Producers
bility to petroleum products other than engine oils has not been
determined. 3. Terminology
3.1 Definitions:

1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, [Link], or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at service@[Link]. 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 Nov. 1, 2020. Published November 2020. Originally the ASTM website.
3
approved in 1987. Last previous edition approved in 2020 as D4684 – 20. DOI: Available from International Organization for Standardization (ISO), 1 rue de
10.1520/D4684-20A. Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland, [Link]
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*A Summary of Changes section appears at the end of this standard

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 D4684 − 20a
3.1.1 apparent viscosity, n—the determined viscosity ob- 63
γ̇ 5 (3)
tained by use of this test method. t
3.1.2 digital contact thermometer (DCT), n—an electronic 3.2.4 shear stress, n—the motivating force per unit area for
device consisting of a digital display and associated tempera- fluid flow.
ture sensing probe.
[Link] Discussion—This device consists of a temperature [Link] Discussion—For the rotary viscometer being de-
sensor connected to a measuring instrument; this instrument scribed in 6.1, the rotor surface is the area under shear or the
measures the temperature-dependent quantity of the sensor, shear area. For this test method, end effects are not considered.
computes the temperature from the measured quantity, and T r 5 9.81 M ~ R o 1R t ! 3 1026 (4)
provides a digital output. This digital output goes to a digital Tr
display and/or recording device that may be internal or external τ5
2 πR r2 h
3 109 (5)
to the device.
[Link] Discussion—The devices are often referred to as a where:
“digital thermometers,” however the term includes devices that Tr = torque applied to rotor, N·m,
sense temperature by means other than being in physical M = applied mass, g,
contact with the media. Ro = radius of the shaft, mm,
[Link] Discussion—PET is an acronym for portable elec- Rt = radius of the string, mm,
tronic thermometers, a subset of digital contact thermometers τ = shear stress at the rotor surface, Pa, and
(DCT). h = height of the rotor, mm.
3.1.3 Newtonian oil or fluid, n—an oil or fluid that at a given For the dimensions given in 6.1.1,
temperature exhibits a constant viscosity at all shear rates or T r 5 31.7 M 3 1026 (6)
shear stresses. τ 5 3.5 M (7)
3.1.4 non-Newtonian oil or fluid, n—an oil or fluid that at a
given temperature exhibits a viscosity that varies with chang- 3.2.5 test oil, n—any oil for which the apparent viscosity
ing shear stress or shear rate. and yield stress are to be determined by this test method.
3.1.5 viscosity, n—the ratio between the applied shear stress 3.2.6 unused oil, n—an oil which has not been used in an
and rate of shear which is sometimes called the coefficient of operating engine.
dynamic viscosity and is a measure of the resistance to flow of 3.2.7 used oil, n—an oil which has been used in an operating
the liquid. engine.
3.2 Definitions of Terms Specific to This Standard: 3.2.8 yield stress, n—the shear stress required to initiate
3.2.1 calibration oils, n—those oils that establish an instru- flow.
ment’s reference framework of apparent viscosity versus
[Link] Discussion—For all Newtonian fluids and many
speed, from which the apparent viscosities of test oils are
non-Newtonian fluids, the yield stress is zero. An oil can have
determined.
a yield stress that is a function of its low-temperature cooling
3.2.2 cell constant, n—the ratio of the calibration fluid rate, soak time, and temperature. Yield stress measurement by
viscosity to the time required to complete the first three this test method determines only whether the test oil has a yield
measured revolutions of the rotor. stress of at least 35 Pa; a yield stress below 35 Pa is considered
3.2.3 shear rate, n—the velocity gradient in fluid flow. to be insignificant for engine oils.
[Link] Discussion—For a Newtonian fluid in a concentric
4. Summary of Test Method
cylinder rotary viscometer in which the shear stress is mea-
sured at the inner cylinder surface (such as this apparatus, 4.1 An engine oil sample is held at 80 °C and then cooled at
described in 6.1), and ignoring any end effects, the shear rate is a programmed cooling rate to a final test temperature and held
given as follows: for a specified time period. At the end of this period, a series of
increasing low torques are applied to the rotor shaft until
2ΩR s2
γ̇ 5 (1) rotation occurs to determine the yield stress, if any is exhibited.
R 2s 2 R r2
A higher torque is then applied to determine the apparent
4πR s2 viscosity of the sample.
5 (2)
t ~ R 2s 2 R r2 !

where: 5. Significance and Use

γ̇ = shear rate at the surface of the rotor in reciprocal 5.1 When an engine oil is cooled, the rate and duration of
seconds, s−1, cooling can affect its yield stress and viscosity. In this
Ω = angular velocity, rad/s, laboratory test, a fresh engine oil is slowly cooled through a
Rs = stator radius, mm, temperature range where wax crystallization is known to occur,
Rr = rotor radius, mm, and followed by relatively rapid cooling to the final test tempera-
t = time in seconds for one revolution of the rotor. ture. These laboratory test results have predicted as failures the
For the specific apparatus being described in 6.1.1, known engine oils that have failed in the field because of lack
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 D4684 − 20a
of oil pumpability.4 These documented field failing oils all contact rotor shaft. The piece has a center bore of 11 mm 6
consisted of oils normally tested at –25 °C. These field failures 1 mm. The cap is made in two halves to facilitate placement in
are believed to be the result of the oil forming a gel structure the top of the cell.
that results in either excessive yield stress or viscosity of the [Link] Cell caps shall not be used in the direct refrigeration
engine oil, or both. instruments, since such use would block the flow of cold, dry
5.2 Cooling Profiles: air into the stators to keep them frost-free.
5.2.1 For oils to be tested at −20 °C or colder, Table X1.1 6.2 Weights:
applies. The cooling profile described in Table X1.1 is based on 6.2.1 Yield Stress Measurement—A set of nine disks and a
the viscosity properties of the ASTM Pumpability Reference disk holder, each with a mass of 10 g 6 0.1 g.
Oils (PRO). This series of oils includes oils with normal 6.2.2 Viscosity Measurement—A mass of 150 g 6 1.0 g.
low-temperature flow properties and oils that have been 6.3 Temperature Control System—Regulates the mini-rotary
associated with low-temperature pumpability problems (1-5).5 viscometer block temperature in accordance with the tempera-
Significance for the −35 °C and −40 °C temperature profiles is ture requirements described in Table X1.1 or Table X1.2.
based on the data collected from the “Cold Starting and 6.3.1 Temperature Profile—The temperature profile is fully
Pumpability Studies in Modern Engines” conducted by ASTM described in Table X1.1 and Table X1.2.
(6, 7).
5.2.2 For oils to be tested at −15 °C or −10 °C, Table X1.2 6.4 Temperature Measuring Device—Use either a DCT
applies. No significance has been determined for this tempera- meeting the requirements described in 6.4.1 or liquid-in-glass
ture profile because of the absence of appropriate reference thermometers described in 6.4.2. A calibrated DCT or cali-
oils. Similarly, precision of the test method using this profile brated low temperature liquid-in-glass thermometer shall be
for the −10 °C test temperature is unknown. The temperature used as the thermometer for temperature measurement below
profile of Table X1.2 is derived from the one in Table X1.1 and 25 °C independent of the instrument’s temperature control, and
has been moved up in temperature, relative to Table X1.1, in shall be located in the thermowell.
consideration of the expected higher cloud points of the NOTE 1—The display device and sensor must be correctly paired.
viscous oils tested at −15 °C and −10 °C. Incorrect pairing will result in temperature measurement errors and
possibly irreversible damage to the electronics of the display.
6. Apparatus 6.4.1 Digital Contact Thermometer—Use D02-DCT14
6.1 Mini-Rotary Viscometer—An apparatus that consists of listed in Specification D8278. As an alternative to the metal
one or more viscometric cells in a temperature-controlled block sheathed probe noted in Specification D8278, a glass sheathed
made of a metallic material with high thermal conductivity. DCT probe with a 6 mm O.D. is acceptable provided it meets
Each cell contains a calibrated rotor-stator set. The rotor shall the other requirements shown for D02-DCT14 in Specification
have a crossbar near the top of the shaft extending in both D8278. A DCT display resolution of 0.01 C is preferable. If
directions far enough to allow the locking pin (6.6) to stop thermowell ID is larger than the probe OD, then a metallic
rotation at successive half turns. Rotation of the rotor is sleeve must be used to fill the gap between the probe OD and
achieved by an applied force acting through a string wound thermowell ID with a length of 58 mm.
around the rotor shaft. [Link] The DCT calibration drift shall be checked at least
6.1.1 The mini-rotary viscometric cell has the following annually by either measuring the ice point or against a
dimensions: reference thermometer in a constant temperature bath at the
Diameter of rotor 17.06 mm ± 0.08 mm
prescribed immersion depth to ensure compliance with 6.4.1.
Length of rotor 20.00 mm ± 0.14 mm With respect to an ice bath, Practice E563 provides guidance
Inside diameter of cell 19.07 mm ± 0.08 mm on the preparation and use of an ice bath. However for this use
Radius of shaft 3.18 mm ± 0.13 mm
Radius of string 0.1 mm
variance from the specific steps, such as water source, is
permitted provided preparation is consistent. The basis for the
6.1.2 Cell Cap—A cover inserted into the top of the vis-
variance is due to the reference being used to track change in
cometer cell to minimize room air circulation into the cells is
calibration not verification.
required for thermometrically cooled instruments. The cell cap
is a stepped cylinder 38 mm 6 1 mm in length made of a low NOTE 2—When a DCT’s calibration drifts in one direction over several
thermal conductivity material, for example, thermoplastic such calibration checks, that is, ice point, it may be an indication of deteriora-
tion of the DCT.
as acetyl copolymers that have known solvent resistivity and
are suitable for use between the temperature ranges of this test 6.4.2 For liquid-in-glass thermometers, LiG, two are re-
method. The top half is a minimum of 25 mm in diameter and quired. One LiG shall be a calibrated 76 mm partial immersion
the bottom half is 19 mm in diameter with a tolerance thermometer with a scale from +5 °C to 1 degree less than the
consistent with the cell diameter. The tolerance on the bottom lowest test temperature in 0.2 °C subdivisions. This low
half is such that it will easily fit into cell but not allow cap to temperature LiG thermometer shall have a report of calibration
showing the temperature deviation at each calibrated test
temperature. The second LiG thermometer shall be a 76 mm
4
partial immersion thermometer graduated from at least +70 °C
Pumpability Reference Oils (PRO) 21 through 29.
5
The boldface numbers in parentheses refer to the references at the end of this to 90 °C in 1 °C subdivisions, which is used to verify the
standard.
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 D4684 − 20a
[Link] Calibration Check—Verify the low temperature Procedure A (TE Cooled and Direct Refrigeration
thermometer at least annually against a reference thermometer Instruments)
in a constant temperature bath or an ice bath. The thermometer
is to be inserted to its immersion depth. If using an ice bath, the 9. Calibration and Standardization
ice point reading is to be taken within 60 min after the
9.1 Temperature Control Calibration Procedure—Calibrate
thermometer has been at test temperature for at least 3 min. If
the MRV temperature control by comparing the instrument’s
the corrected temperature reading deviates from the reference
displayed temperature against a thermometer in the thermow-
thermometer or the ice point then repeat this calibration check.
ell. The thermometer used shall meet the requirements in 6.4.

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If the thermometer deviates from the reference value on two
9.1.1 Place 10 mL of a typical test fluid and rotor in each
successive checks then a full thermometer recalibration is
cell. If required, place cell caps over each cell then place cover
needed.
on instrument. Cell caps shall not be used on direct refrigera-
[Link] Recalibration—A complete recalibration of the tion instruments (see 6.1.2).
liquid-in-glass thermometer, while permitted, is not necessary 9.1.2 Place the thermometer in the thermowell. See Note 3.
in order to meet the accuracy ascribed to liquid-in-glass This thermowell is to be used for all temperature measurements
thermometer’s design until the thermometers corrected mea- below 25 °C.
sured temperature deviates from the reference thermometer or
ice point by one scale division, or until five years has elapsed NOTE 3—Prior to inserting the thermometer or DCT probe in the
since the last full calibration. thermowell, place several drops (~3) of a heat transfer fluid such as 50/50
water/ethylene glycol mix, CCS reference oil CL100 or a dewaxed low
6.5 Supply of Dry Gas—A supply of dry filtered dry gas to viscosity mineral oil in the thermowell.
minimize moisture condensation on the upper portions of the 9.1.3 Make these temperature measurements at 80 °C then
instrument. at least three measurements that are 5 °C apart from –5 °C to
6.5.1 For thermoelectric cooled instruments, which use cell the lowest test temperature used, including both end points to
caps, the dry gas supply is connected to the housing cover. The establish a calibration curve for this combination of thermom-
supply of dry gas is discontinued when the cover is removed eter and the instrument’s temperature control. Make at least
for the measurement phase of the test. two temperature measurements at every calibration tempera-
ture with at least 10 min between observations.
6.6 Locking Pin—A device to keep the rotor from turning
prematurely and able to stop the rotor at the nearest half NOTE 4—All temperatures in this test method refer to the actual
revolution by interaction with the rotor crossbar. temperature and not necessarily the indicated temperature.
9.1.4 Follow the instrument manufacturers instructions for
7. Reagents and Materials correcting the instrument’s measured temperature. Alterna-
7.1 Low Cloud-point Newtonian Oil—Calibration oil of tively establish a correction equation between thermometer and
approximately 30 Pa·s viscosity at –20 °C for Procedure B or the instruments’s measured temperature then adjust each tem-
60 Pa·s at –25 °C for Procedure A for calibration of the perature of the cooling program by the offset determined with
viscometric cells. The calibration oil shall be obtained from the correction equation.
suppliers complying with ISO Guide 34 and ISO 17025 with 9.2 Viscometer Cell Calibration—The calibration constant
traceability to a national metrology institute (NMI). of each rotor/stator combination is determined by conducting
7.2 Methanol—Commercial or technical grade of dry two tests at –25 °C using a viscometric standard as a test
methanol is suitable for the refrigerated cooling bath required sample.
for some units. (Warning—Flammable.) 9.2.1 Each cell shall be calibrated twice and the resulting
calibration constant is to be calculated from the average of the
7.3 Oil Solvent—Commercial heptanes or similar solvent two determinations of the time for three revolutions of the
that evaporates without leaving a residue is suitable. rotor. When the two cell calibrations are consecutive, the
(Warning—Flammable.) second test shall be on a new sample of standard with cleaning
7.4 Acetone—A technical grade of acetone is suitable pro- between the steps.
vided it does not leave a residue upon evaporation. NOTE 5—Once a set of rotors has been calibrated in an instrument,
(Warning—Flammable.) subsequent calibration checks can be single determinations if the criteria
of 9.11 are met.
8. Sampling 9.2.2 Use the same 150 g mass for both calibration and
8.1 A representative sample of test oil free from suspended viscosity measurements. However, different units may be used
solid material and water is necessary to obtain valid viscosity for calibration and viscosity measurements provided they are
measurements. If the sample in its container is received below certified to be 150 g 6 0.1 g.
the dew-point temperature of the room, allow the sample to 9.3 Following steps in 10.1, prepare the cells for calibration
warm to room temperature before opening the container. using the calibration oil as the sample.

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 D4684 − 20a
9.4 Use either the calibration temperature profile for the a full set of samples to run, fill each of the unused cells with a typical test
instrument or, alternatively, the cooling profile given in Test sample.
Method D3829 for a –25 °C test temperature, and follow the 10.1.3 Repeat 10.1.2 until all test samples are in their cells.
owner’s manual instructions for the instrument to initiate the
NOTE 8—Before inserting the rotors in the cells, inspect each rotor to be
cooling profile program. sure that the shaft is straight, that the rotor surface is smooth and free from
NOTE 6—The use of the calibration temperature profile makes it dents, scratches, and other imperfections. For rotors with a bearing point
possible to complete two cell constant determinations in one day. at the bottom of the shaft, ensure that the point is sharp and centered on
9.5 Place the thermometer in the thermometer well at least the rotor shaft. If these conditions are not met, repair or replace the rotor.
30 min prior to executing 9.7. See Note 3. This thermowell 10.1.4 Place each rotor in its cell, and place upper pivot pin
location is to be used for calibration and temperature monitor- in position, including those for any unused cells.
ing during the test procedure. 10.1.5 When use is required, install a cell cap on all cells,
9.6 At the completion of the temperature profile for cell including any unused cells.
calibration, check that the final test temperature is within 10.1.6 For each cell, except any unused ones, place a loop of
0.1 °C of the desired calibration temperature. Final test tem- the nominal 700 mm long string over the crossbar. Hang the
perature is to be verified independently of the instrument’s string over the timing wheel with a small weight attached such
temperature control with a thermometer that has been in the as a large paper clip. Wind the string around the shaft until the
thermometer well for at least the time prescribed in 9.5. See end is about 100 mm below the wheel. Do not overlap
Note 3. windings.
9.7 Beginning with the cell farthest to the left facing the NOTE 9—The strings can be pre-wound around the shafts before they
are installed in 10.1.4.
instrument, follow 10.6.3 and record the rotation time for three
revolutions. [Link] Engage the locking pin to prevent the rotor from
turning.
9.8 Repeat 9.7 for each of the remaining cells in numerical
[Link] Lay the remaining string over the top of the bearing
order.
plate letting it hang over the back of the plate.
9.9 Repeat 9.3 – 9.8 for a second set of calibration data. [Link] Repeat 10.1.6 – [Link] until all cells with samples
9.10 For each cell (rotor/stator combination) calculate the to be measured are prepared.
calibration constant using Eq 8 and 9. 10.1.7 Place the housing cover over the viscometric cells.
10.1.8 Connect the dry gas supply to the housing cover, as
t 5 ~ t 1 1t 2 ! /2 (8)
noted in 6.5. Set the dry gas flow to approximately 1 L ⁄h.
C 5 η/t (9) Increase or decrease the flow as necessary to minimize frost or
where: moisture condensation around the cells.
η = viscosity of the standard oil, mPa·s at test temperature, 10.2 Select the cooling profile for the desired test tempera-
C = cell constant with a 150 g mass, mPa, ture and follow the instrument instructions to initiate the
t1 = time of three rotor revolutions for first calibration, program. Table X1.3 lists the nominal times to reach a
t2 = time of three rotor revolutions for second calibration, particular test temperature.
and
t = average time of three rotor revolutions. 10.3 Place the thermometer in the thermowell at least
30 min prior to completion of the cooling profile (see Note 3).
9.11 After the calibration constants have been determined, The same thermowell location is to be used for all measure-
check to see if any cell has a calibration constant differing by ments and must be the same one as was used in the calibration.
more than 4 % from the average of all cells or if the difference
between t1 and t2 for any cell is greater than 4 % of the average 10.4 At the completion of the cooling profile, check the
of t1 and t2. If so, then one or both of the results should be time-temperature plot for the run to ensure that the time-
considered suspect. If these criteria are not met, examine the temperature profile is within tolerance and that the test tem-
indicated rotor for damage, repair or replacement as necessary, perature as measured in the thermowell is within 60.2 °C of
and repeat the cell calibrations. the final test temperature. Both of these checks may be done
automatically by the control software incorporated in some
9.12 If corrected values for the controller temperature and instruments. Final test temperature is to be verified indepen-
thermometer deviate by more than the tolerance (60.1 °C), use dently from the instrument’s temperature control using a
the procedure in X2.1 to assist in determining the cause and thermometer that has been in the thermowell for at least 30 min
correction. prior to reaching the test temperature. See Note 3. If the final
test temperature is more than 0.1 °C from the set point on two
10. Yield Stress and Viscosity Measurement Procedure consecutive runs, the instrument’s temperature control must be
10.1 Viscometric Cell Preparation: recalibrated according to 9.1.
10.1.1 If the cells are not clean, clean according to 10.7. 10.5 If the temperature profile is within tolerance, proceed
10.1.2 Place 10 mL 6 0.2 mL of a test oil sample into a with measurements. If not, then abort the test and recalibrate
clean cell. temperature controller as in 9.1.
NOTE 7—All cells should contain a fluid and rotor; if there are less than 10.6 Measurement of the Yield Stress:
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 D4684 − 20a
10.6.1 Immediately prior to starting measurements, take the [Link] Stop the timer after three revolutions of the rotor
cell housing cover off the instrument. from point of release. When the time for one revolution is
10.6.2 Yield Stress Determination—Starting with the cell greater than 60 s, time only one revolution.
farthest to the left while facing the instrument, use the
NOTE 12—The timing of three revolutions may be done automatically.
following procedure for each cell in turn, bypassing the unused
cells. [Link] After completing three revolutions (one revolution
[Link] Align the pulley wheel with the rotor shaft of the if the time for it is greater than 60 s), remove mass from string.
cell to be tested. [Link] Record both the time and the number of revolutions
[Link] Hang the string over the timing wheel such that the timed.
string hangs past the front of the housing. Make sure that the [Link] If no rotation occurs with the application of the
disk holder clears the edge of the bench during testing. 150 g mass, record the result for that sample as being “Too
[Link] Suspend the disk holder from the string. Viscous To Measure” (TVTM).
[Link] For instruments with automatic timing, start timing [Link] Repeat 10.6.2 – [Link] for the remaining cells to
and then release the locking pin. For manual timing, start be measured.
timing immediately after the locking pin is disengaged. 10.7 Cleaning:
[Link] Observe whether the end of the crossbar moves 10.7.1 When all measurements have been completed, set the
more than 3 mm in 15 s. (This 3 mm is approximately twice the instrument to warm to room temperature or somewhat above.
diameter of the crossbar.) An alternative procedure is the use of Cleaning cells above a temperature of 55 °C is not recom-
a marked rotation of the timing wheel equivalent to a rotor mended.
shaft rotation of 3 mm. 10.7.2 When the desired cleaning temperature is reached:
[Link] Electronic or timing wheel motion-sensing devices, [Link] For instruments with non-removable cells, remove
which are available on some instruments, are suitable alterna- strings, rotors, and cell caps, when used, then proceed with
tives to direct observation. 10.7.3.
[Link] If rotor movement of more than 3 mm, or [Link] For instruments with removable cells, either follow
alternative, in 15 s is observed in [Link], remove the disk instructions for non-removable or remove cells from instru-
holder from the end of the string, and proceed to 10.6.3. ment. The removable cells are to be cleaned by generally
[Link] If a rotor movement of less than 3 mm in 15 s is following the instructions in 10.7.3.
observed in [Link], stop timing and lift the disk holder so it 10.7.3 Cleaning Cells:
is not supported by the string. Then add an additional 10 g disk
[Link] After all of the measurements have been
to disk holder.
completed, exit the cooling program and turn on the heater to
NOTE 10—As additional disks are added to the disk holder, it is warm the viscometric cells to room temperature or somewhat
necessary to suspend the holder with the additional disks from the string higher. The temperature shall not exceed 50 °C.
and restart timing without the use of the locking pin for the remainder of
the yield stress assessment. When using software available for some
[Link] Remove the upper rotor pivots and the rotors.
instruments, ensure that the mass applied is the mass requested by the [Link] With vacuum, remove samples, then using an
program. appropriate solvent, rinse the cells at least three times with
[Link] Carefully and gently, suspend the disk holder from approximately 15 mL of an appropriate solvent for each rinse.
the string and start timing. Then rinse once with acetone.
[Link] Remove traces of residual solvent by flushing cell

--``,```,,,``,,,``,,`,`,,`,``,``-`-`,,`,,`,`,,`---
[Link] Repeat steps in [Link] and [Link] until the
accumulated mass causes rotation of the rotor. At this point, with dry air or preferably with a vacuum hose to prevent
remove the disk holder from the string. contamination with house air. (Warning—When flushing cells
[Link] If no rotation is observed with a total of 100 g, with air, be sure that the air is clean and free from oil, water and
record that the yield stress is >350 Pa, and proceed with 10.6.3. other contaminants as these could be left in the cell. House air
is frequently contaminated.)
10.6.3 Measurement of Apparent Viscosity:
[Link] Gently suspend the 150 g mass from the string. 10.7.4 Clean rotors with appropriate sample solvent, and
dry.
[Link] If the applied mass of 150 g will move the rotor, as
soon as the cross-arm is clear of the locking pin, reengage the
11. Calculation of Yield Stress and Apparent Viscosity
locking pin. Allow rotation to continue until the cross-arm
contacts the locking pin causing rotation to stop. If no 11.1 Yield stress is given by the following equation:
appreciable rotation occurs, terminate the test and proceed to Ys 5 3.5 M (10)
[Link].
where:
NOTE 11—Yield stresses exceeding the stress exerted by 150 g have
been encountered.
Ys = yield stress, Pa, and
M = applied mass, g, at which rotation was observed.
[Link] When using instruments capable of timing rotation
automatically, initiate viscosity measurement by starting 11.2 The viscosity is given by the following equation when
timing, then release the locking pin. When timing manually, using the cell constant (C) obtained in 9.10:
start timing immediately after the locking pin is disengaged. η a 5 C·t·3⁄r (11)

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 D4684 − 20a
TABLE 1 Precision—Procedure A
Yield Stress Precision
Repeatability Reproducibility
Unused Oils 35 Pa 70 Pa
Used Gasoline Engine Oils
Yield Stress # 35 Pa 35 Pa 35 Pa
Yield Stress > 35 Pa 70 Pa 70 Pa
Apparent Viscosity Precision
Repeatability Reproducibility
Unused Oils
Viscosity: 4300 to 20 000 mPa · s 6.3 % of mean 8.2 % of mean
Viscosity: >20 000 mPa · s 7.5 % of mean 14.6 % of mean
Used Gasoline Engine Oils
Yield stress # 35 Pa 11 % of mean 15 % of mean
Yield stress > 35 Pa 25 % of mean 34 % of mean

where: tested in 7 to 9 laboratories at –25 °C, –30 °C, –35 °C, and
ηa = apparent viscosity in mPa·s, –40 °C. For direct refrigeration cooled MRV’s, the program
C = cell constant obtained in Eq 9, included 20 samples tested in 6 laboratories at –25 °C, –30 °C,
t = time in seconds for number (r) of complete revolutions –35 °C, and –40 °C. These samples consisted of multigrade
of the rotor in [Link], and engine oils and base stocks that had a yield stress range of less
r = number of revolutions timed; either one or three than 35 Pa to 210 Pa and a apparent viscosity range from
revolutions. 4300 mPa·s to 270 000 mPa·s.
The precision of this test method for used gasoline engine
12. Report oils was determined by the statistical examination of interlabo-
12.1 Apparent Viscosity and Yield Stress—Report the final ratory test results at –25 °C and –30 °C.
test temperature, apparent viscosity, and yield stress by Test 13.1.1 Repeatability—In Table 1, the difference between
Method D4684, Procedure A. successive results obtained by the same operator with the same
apparatus under constant operating conditions on identical test

--``,```,,,``,,,``,,`,`,,`,``,``-`-`,,`,,`,`,,`---
12.2 Yield Stress—Report as less than the value at which
rotation was observed; that is, if rotation was observed with a materials would, in the long run, in the normal and correct
mass of 20 g, report the yield stress as <70 Pa (20 g × 3.5). If operation of the test method, exceed the following values only
the rotor did not move with the application of 100 g of total in 1 case in 20.
weight, report the yield stress as >350 Pa. 13.1.2 Reproducibility—In Table 1, the difference between
two single and independent results obtained by different
NOTE 13—If the rotation was observed with a mass of 10 g, the operators working in different laboratories on identical test
minimum mass, report the yield stress as <35 Pa rather than as 0 Pa. materials would, in the long run, exceed the following values
12.3 Apparent Viscosity—Report as follows: only in 1 case in 20.
12.3.1 If the apparent viscosity is less than 5000 mPa·s, then 13.2 Bias:
report the apparent viscosity as less than 5000 mPa·s. 13.2.1 Bias (Unused Gasoline Engine Oils)—No statement
12.3.2 If the apparent viscosity is between 5000 mPa·s and on bias is being made for this test method, because there is no
100 000 mPa·s, then report the apparent viscosity to the nearest accepted reference material suitable for determining absolute
100 mPa·s. bias.
12.3.3 If the apparent viscosity is between 100 000 mPa·s 13.2.2 Relative Biases:
and 400 000 mPa·s, then report the apparent viscosity to the [Link] Yield Stress—There was no significant relative bias
nearest 1000 mPa·s. between yield stresses measured by Procedure A and those
12.3.4 If the apparent viscosity is greater than measured by Procedure B for oils with a yield stresses less than
400 000 mPa·s, then the apparent viscosity should be reported 105 Pa. No statement can be made with those with yield stress
as greater than 400 000 mPa·s. greater than 105 Pa.
12.3.5 If the rotor did not move with the application of the [Link] Viscosity—There is no statistically significant rela-
150 g weight, report that the sample was “Too Viscous To tive bias between the viscosities as measured by either Proce-
Measure” (or “TVTM”). dure A or Procedure B.
13. Precision and Bias6 13.2.3 Bias (Used Gasoline Engine Oils)—Since there is no
accepted reference material suitable for determining the bias
13.1 Precision—The precision of this test method for un- for this test method, no statement on bias in being made.
used oils was determined by the statistical examination of
results from an interlaboratory program. For the thermoelec- Procedure B (Methanol cooled MRV Instruments and
trically cooled MRV’s, the program included 10 to 11 samples those used for Procedure A)
14. Calibration and Standardization
6
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Reports RR:D02-1404, D02–1612, D02–1613, 14.1 Temperature Control Calibration Procedure—
and D02–1654. Contact ASTM Customer Service at service@[Link]. Calibrate the MRV temperature control by comparing the

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 D4684 − 20a
instrument’s displayed temperature against a thermometer in T = time in seconds for three complete revolutions obtained
the thermowell. The thermometer used shall meet the require- in 15.4.1.
ments in 6.4.
14.2.9 If any cell has a calibration constant more than 10 %
14.1.1 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. If required, place cell caps over each cell then place cover
may be a problem with rotor operation. Examine rotor for
on instrument. Cell caps shall not be used on direct refrigera-
damage, and recalibrate the instrument.
tion instruments (see 6.1.2).
14.1.2 Place the thermometer in the thermowell. See Note 3. 14.3 If corrected temperature values shown by the instru-
This thermowell is to be used for all measurements below ment’s temperature control and thermometer deviate by more
25 °C. than 60.1 °C, use X2.1 to assist in determining the fault.
14.1.3 Make these temperature measurements at 80 °C then
at least three measurements that are 5 °C apart from –5 °C to 15. Procedure
the lowest test temperature used, including both end points to 15.1 Program the temperature controller to control the
establish a calibration curve for this combination of thermom- mini-rotary viscometer block temperature as outlined in Table
eter and the instrument’s temperature control. Make at least X1.1 or Table X1.2. The programmed temperature is the
two temperature measurements at every calibration tempera- temperature in Table X1.1 or Table X1.2 plus the appropriate
ture with at least 10 min between observations. temperature correction factor determined in 14.1. Table X1.3
NOTE 14—All temperatures in this test method refer to the actual lists the nominal times to reach a particular test temperature.
temperature and not necessarily the indicated temperature. 15.2 Test Sample and Viscometric Cell Preparation:
14.1.4 Follow the instrument manufacturers instructions for 15.2.1 Remove the nine rotors from the viscometric cells
correcting the instrument’s measured temperature.

--``,```,,,``,,,``,,`,`,,`,``,``-`-`,,`,,`,`,,`---
and ensure that both the cells and rotors are clean. See 15.6 for
Alternatively, establish a correction equation between ther- the cleaning procedure.
mometer and the instruments’s measured temperature then 15.2.2 Place a 10 mL 6 1.0 mL oil sample in each cell.
adjust each temperature of the cooling program by the offset
NOTE 15—All cells should contain a fluid and rotor; if there are less
determined with the correction equation. than a full set of samples to run, fill each of the unused cells with a typical
14.2 Viscometer Cell Calibration—The calibration of each test sample.
viscometric cell (viscometer constants) can be determined with NOTE 16—Before inserting the rotors in the cells, inspect each rotor to
be sure that the shaft is straight, that the rotor surface is smooth and free
the viscosity standard and the following procedure at –20 °C: from dents, scratches, and other imperfections. For rotors with a bearing
14.2.1 Use steps in 15.2 – 15.2.5. point at the bottom of the shaft, ensure that the point is sharp and centered
14.2.2 Use either the calibration temperature profile for the on the rotor shaft. If these conditions are not met, repair or replace the
instrument or, alternatively, the cooling profile given in Test rotor.
Method D3829 for a –20 °C test temperature and follow the 15.2.3 Install the rotors in the proper stators and install the
owner’s manual instructions for the instrument to initiate the upper pivots.
cooling profile program. 15.2.4 Place the loop of the 700 mm long string over the
14.2.3 Place the thermometer in the thermometer well at cross-arm at the top of the rotor shaft and wind all but 200 mm
least 30 min prior to continuing. See Note 3. This thermowell of the length of the string around the shaft. Do not overlap
location is to be used for calibration and temperature monitor- strings. Loop the remaining end of the string over the top
ing during the test procedure. Allow the oil in the cells to soak bearing cover. Orient the rotor such that an end of the
at –20 °C 6 0.2 °C for at least 1 h, making small temperature cross-arm at the top of the rotor shaft is pointing directly
adjustments, if necessary, to maintain the test temperature. forward. If available, secure cross-arm with locking pin. If the
14.2.4 At the completion of the temperature profile for cell rotations are manually timed, it is helpful to color one end of
calibration, check that the final test temperature is within the cross-arm.
0.1 °C of the desired calibration temperature. Final test tem- NOTE 17—The string may be prewound around the shaft before
perature is to be verified independently of the instrument’s installation of the rotor in 15.2.3.
temperature control with a thermometer that has been in the
15.2.5 Place the housing cover over the viscometric cells.
thermometer well for at least the time prescribed in 14.2.3. See
This is to minimize the formation of frost on the cold metal
Note 3.
parts exposed to air. In some climates, it may be necessary to
14.2.5 Proceed to 15.3.1 – 15.3.3.
flush the cover with a dry gas (for example, dry air or nitrogen)
14.2.6 Perform step in 15.4.1. to minimize the frost formation.
14.2.7 Repeat 14.2.5 and 14.2.6 for each of the remaining 15.2.6 Select the cooling profile for the desired test tem-
cells, taking the cells in order from left to right. perature and follow the instrument instructions to initiate the
14.2.8 Calculate the viscometer constant for each cell program. Table X1.3 lists the nominal times to reach a
(rotor/stator combination) with the following equation: particular test temperature.
C 5 η o /T (12) 15.2.7 Place the thermometer in the thermowell at least
30 min prior to completion of the temperature profile. The
ηo = Viscosity of the standard oil, mPa·s at –20 °C, thermowell used, should be the same one that was used during
C = cell constant with 150 g mass, mPa, and
calibration. (See Note 3.)

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 D4684 − 20a
15.2.8 At the completion of the temperature profile, the cross-arm or 13° of rotation) then record that the sample has
temperature of the block should be within 0.2 °C of the desired yield stress. Proceed to [Link]. If movement is detected,
test temperature when measured by a thermometer other than record the mass and proceed to 15.4.
the temperature controller in the same thermometer well used [Link] If no movement is detected, for instruments with-
during calibration. If the block temperature is within this range, out locking pins, hold weight assembly and add a disk, then
proceed with the yield stress and viscosity measurements proceed with [Link]. If equipped with locking pins, lower the
within 30 min of the completion of the temperature profile (see locking pin to re-engage cross-arm. Add a disk to the disk
15.3). holder, raise the locking pin, and proceed with [Link].
[Link] If the final temperature of the block is 0.2 °C to
0.5 °C warmer than the desired temperature, proceed as fol- Model CMRV-4 or Later Model MRV
lows. Set the temperature controller to bring the block tem- [Link] The operator shall follow the on-screen instructions
perature to the correct test temperature and then hold at the for the addition of weight increments.
correct test temperature for 30 min before proceeding. This [Link] For instruments with locking pins: suspend disk
entire temperature correction should not take longer than 1 h. holder on string, press the flashing start button, then immedi-
The data obtained in this way are considered valid test results, ately raise the locking pin and follow the on-screen instruc-
otherwise the test is invalid. tions.
[Link] If the final test temperature is more than 0.2 °C [Link] If additional mass is requested, capture cross-arm
cooler or more than 0.5 °C warmer than the preselected test in locking pin, then add one additional disk, and follow the
temperature, then the test is NOT VALID for the preselected on-screen instructions. Press the flashing start button, then
temperature. For Information Only, the yield stress and viscos- immediately raise the locking pin. Repeat procedure until no
ity may be measured without further temperature adjustment. additional mass is requested. Proceed to 15.4.
These results are characteristic of the actual temperature, not [Link] For instruments without locking pins: carefully
the preselected one. suspend and hold the disk holder on the string without jerking
15.2.9 If the final temperature as noted in 15.2.8 is in error rotor, and follow the on-screen instructions. Press the flashing
in either direction by more than 0.2 °C, see X2.1 before starting start button, and immediately release the disk holder.
another test. [Link] If no movement is detected, then carefully support
15.2.10 With models CMRV-4 and higher, if the program the disk holder. Add a disk as indicated on the computer screen,
reports cooling profile out of tolerance, the operation of the without pulling on the string, and follow the on-screen instruc-
instrument shall be thoroughly reviewed for correct operation. tions. Press the flashing start button, and immediately release
With models earlier than CMRV-4, check the logged data for disk holder. Repeat procedure until no additional disks are
excessive temperature deviation. See X2.1 and X2.2. requested. Proceed with 15.4.
15.3 Measurement of the Yield Stress: NOTE 19—When the load is first applied, some oils may show
momentary movement of the cross-arm. If there is no further movement of
15.3.1 Beginning with the cell farthest to the left of the
the cross-arm for 15 s, disregard the initial movement.
instrument, follow this procedure for each cell in turn.
15.3.2 Align the pulley wheel with the rotor shaft for the 15.4 Measurement of Apparent Viscosity:
cell to be tested, such that the string hangs past the front of the 15.4.1 Follow the instrument model specific instructions.
housing. Make sure that the disk holder clears the edge of the For CMRV-3 or Earlier
bench during testing.
[Link] Attach a 150 g mass to the string and slowly
15.3.3 Remove the string from the upper bearing support suspend it on the string. Start the timer when the cross-arm of
and carefully place it over the pulley wheel so as not to disturb the rotor shaft points directly forward and continue timing in
the test oil. (Do not allow the rotor shaft to turn.) accordance with the following constraints.
15.3.4 Follow the instrument model specific instructions: [Link] If the first half-revolution requires less than 10 s,
NOTE 18—For users with CMRV-4 or newer instruments wishing to measure and record the time for the first three revolutions.
manually time yield stress and viscosity, follow the instructions in [Link] [Link] If the first half-revolution requires 10 s or greater,
and [Link], respectively. measure and record the time for the first revolution and identify
Model CMRV-3 or Earlier it as the time for one revolution.
[Link] If the first revolution has not been completed in
[Link] Visually observe the rotor for movement of the 60 s, end the measurement. Record the time as greater than 60 s
cross-arm. (Do not measure yield stress by way of the for one revolution. Report that the viscosity is greater than the
electronic optics.) value calculated in 16.2.
[Link] For instruments not equipped with locking pins: [Link] If the time for the first three revolutions is less than
carefully, so as not to disturb the gel structure, attach a disk 4 s, record the time as less than 4 s. Report that the viscosity is
holder to the string and gently suspend it on the string. Proceed less than the value calculated in 16.2.
to [Link].
[Link] For instruments equipped with locking pins: sus- For CMRV-4 and Later
pend the disk holder on the string, then raise the locking pin. [Link] Follow the on-screen instructions, press the start
[Link] If the end of the cross-arm does not move at least button, and slowly suspend the 150 g mass on the string.
3 mm in 15 s (approximately twice the diameter of the Timing will automatically begin with the first movement. Do
--``,```,,,``,,,``,,`,`,,`,``,``-`-`,,`,,`,`,,`---

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 D4684 − 20a
not remove mass while viscosity LED on instrument is 17.3.5 When employing software that provides three vis-
flashing. The time and viscosity will be displayed. Proceed to cosity values, the first value shall be reported as the apparent
15.5. viscosity by Test Method D4684. If desired, report all three
15.5 Repeat 15.3–15.4 for each of the remaining cells in values, taking care to also report the sequence of the values.
order from left to right. Never report a value that is the average of the three measured
values.
15.6 Cleaning:
15.6.1 After all of the measurements have been completed, 18. Precision and Bias7
exit the cooling program and turn on the heater to warm the
viscometric cells to room temperature or somewhat higher. The 18.1 Precision (Unused Oils)—The precision of this test
temperature shall not exceed 50 °C. method as determined by the statistical examination of inter-
15.6.2 Remove the upper rotor pivots and the rotors. laboratory test results is as follows:
15.6.3 With a vacuum, remove the oil samples and rinse the 18.1.1 Yield Stress—In the case of pass-fail data, no gener-
cells with an oil solvent several times, followed by two ally accepted method for determining precision is currently
washings with acetone. Use a vacuum to remove the solvent available.
from the cells after each rinse and allow the acetone to 18.1.2 Apparent Viscosity:
evaporate to dryness after the final rinse. [Link] Repeatability—The difference between successive
15.6.4 Clean the rotors in a similar manner. results obtained by the same operator with the same apparatus
under constant operating conditions on identical test material
16. Calculation of Yield Stress and Apparent Viscosity would, in the long run, in the normal and correct operation of
the test method, exceed the following values only in 1 case in
16.1 Yield stress is given by the following equation:
20. The repeatability as a percent of the mean apparent
Ys 5 3.5 M (13) viscosity is shown as follows:
where: Test Temperature, °C Repeatability, Percent
of Mean
Ys = yield stress, Pa, and –15 4.2
M = applied mass, g, recorded in 15.3. –20 7.3
–25 11.7
16.2 The viscosity is given by the following equation when –30 9.3
using the cell constant obtained in 14.2.8: –35 13.2
–40 19.8
η a 5 C t 3/r (14)
[Link] Reproducibility—The difference between two
where: single and independent results obtained by different operators
ηa = apparent viscosity in mPa·s, working in different laboratories on identical test material
C = cell constant obtained for a 150 g mass in Eq 12, would, in the long run, exceed the following values only in 1
t = time for number (r) of complete revolutions of the rotor case in 20. The reproducibility as a percent of the mean
recorded in 15.4, and apparent viscosity is shown as follows:
r = number of revolutions timed in 15.4. Test Temperature, °C Reproducibility, Percent

--``,```,,,``,,,``,,`,`,,`,``,``-`-`,,`,,`,`,,`---
of Mean
17. Report –15 8.4
–20 12.1
17.1 Apparent Viscosity and Yield Stress—For unused oils, –25 17.5
report the final test temperature and either the apparent –30 18.4
–35 35.8
viscosity or the existence of yield stress, but not both, by Test –40 34.1
Method D4684, Procedure B. For used oils, report both 18.1.3 The interlaboratory program included nine test oils at
apparent viscosity and yield stress by Test Method D4684, the –15 °C test temperature with eleven laboratories participat-
Procedure B. ing. Nine test oils were included at the –20 °C test temperature
17.2 Yield Stress—Report as less than the value at which with eleven laboratories participating. The –25 °C test tem-
rotation was observed. perature included 18 test oils with 14 laboratories participating.
17.3 Apparent Viscosity—Report as follows: Nine test oils were evaluated at –30 °C in 13 laboratories. At
17.3.1 If the apparent viscosity is less than 5000 mPa·s, then the –35 °C and –40 °C test temperatures, six test oils were
report the apparent viscosity as less than 5000 mPa·s. evaluated in twelve laboratories.
17.3.2 If the apparent viscosity is between 5000 mPa·s and 18.2 Precision (Used Diesel Engine Oils)—The precision of
100 000 mPa·s, then report the apparent viscosity to the nearest this test method as determined by the statistical examination of
100 mPa·s. interlaboratory test results is as follows:
17.3.3 If the apparent viscosity is between 100 000 mPa·s 18.2.1 Yield Stress:
and 400 000 mPa·s, then report the apparent viscosity to the
nearest 1000 mPa·s.
17.3.4 If the apparent viscosity is greater than 7
Supporting data have been filed at ASTM International Headquarters and may
400 000 mPa·s, then the apparent viscosity should be reported be obtained by requesting Research Reports RR:D02-1212, D02-1249, D02-1277,
as greater than 400 000 mPa·s. and D02-1517. Contact ASTM Customer Service at service@[Link].

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 D4684 − 20a
[Link] Repeatability—The difference between successive 20. The repeatability as a percent of the mean apparent
results obtained by the same operator with the same apparatus viscosity is shown as follows:
under constant operating conditions on identical test material Test Temperature, °C Repeatability, Percent of Mean
would, in the long run, in the normal and correct operation of –20 14.3
–25 10.3
the test method, exceed the following values only in 1 case in
20: [Link] Reproducibility—The difference between two
Test Temperature, °C Repeatability, Pa
single and independent results obtained by different operators
–20 1.735 · (X + 1) working in different laboratories on identical test material
–25 1.014 · (X + 1) would, in the long run, exceed the following values only in 1
where:
X = mean value in Pa
case in 20. The reproducibility as a percent of the mean
apparent viscosity is shown as follows:
NOTE 20—When no yield stress is detected (movement with 10 g Test Temperature, °C Reproducibility, Percent of Mean
weight), X = 0. –20 21.1
–25 20.8
[Link] Reproducibility—The difference between two
single and independent results obtained by different operators [Link] The interlaboratory program included nine labora-
working in different laboratories on identical test material tories and nine test oils at the –20 °C and –25 °C test
would, in the long run, exceed the following values only in 1 temperatures. The used oils included end-of-test drain samples
case in 20. from Mack T8, Mack T8E, Cummins M11-EGR and Mack T10
engine tests, with soot loadings (as measured by thermogravi-
Test Temperature, °C Reproducibility, Pa
–20 2.993 · (X + 1)
metric analysis) ranging from approximately 5 % to 9 % (see
–25 2.976 · (X + 1) RR:D02-1517).7
where:
X = mean value in Pa 18.3 Bias—Since there is no accepted reference material
suitable for determining the bias for this test method, no
18.2.2 Apparent Viscosity: statement on bias is being made.
[Link] Repeatability—The difference between successive
results obtained by the same operator with the same apparatus 19. Keywords
under constant operating conditions on identical test material 19.1 low temperature flow properties; low temperature vis-
would, in the long run, in the normal and correct operation of cosity; mini-rotary viscometer; pumping viscosity; used diesel
the test method, exceed the following values only in 1 case in engine oil; viscosity; yield stress

APPENDIXES

(Nonmandatory Information)

X1. TEMPERATURE PROFILES FOR TEST TEMPERATURES

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

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 D4684 − 20a
TABLE X1.1 Temperature Profile for Test Temperatures −20 °C to −40 °C
Segment TemperatureA Allowable
Segment Time Temperature
h:min Rate of Change ChangeB
Beginning °C Final °C
°C/h °C
nominally 0:20 above 20 to 80
2:00 80 to 80 ±1.0
nominally 0:20 80 to 0
nominally 0:03 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 temperature.C
2:00 −20.0 to −25.0 2.5 ±0.2
Hold at this point for −25 °C test temperature.C
2:00 −25.0 to −30.0 2.5 ±0.2
Hold at this point for −30 °C test temperature.C
2:00 −30.0 to −35.0 2.5 ±0.2
Hold at this point for −35 °C test temperature.C
2:00 −35.0 to −40.0 2.5 ±0.2
Hold at this point for −40 °C test temperature.C
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 Temperature Profile for Test Temperatures −10 °C and −15 °C
Segment TemperatureA Allowable
Segment Time Rate of Change Temperature
Beginning °C Final °C
h:min °C/h ChangeB °C
nominally 0:20 above 20 to 80
2:00 80 to 80 ±1.0
nominally 0:20 80 to 10
nominally 0:03 10 to 7.0
nominally 0:07 7.0 to 6.0 8.5 ±0.5
nominally 0:10 6.0 to 5.0 6.0 ±0.2
6:00 5.0 to 2.0 0.5 ±0.2
36:00 2.0 to −10.0 0.33 ±0.2
Hold at this point for − 10 °C test temperature.C
2:00 −10.0 −15.0 2.5 ±0.2
Hold at this point for − 15 °C test temperature.C
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 X1.3 Nominal Elapsed Time to Test Temperature

Test Temperature, Nominal Elapsed Time,
°C h
−10 45
−15 47
−20 45
−25 47
−30 49
−35 51
−40 53
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 D4684 − 20a

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 it should be similar
more than 0.2 °C, do the following before starting another to methanol in viscosity and heat capacity at the bath tempera-
analysis: ture.
X2.1.1 Check the thermometer calibration. For liquid-in- X2.1.4 Check to see that the refrigeration system is working
glass thermometers, check the ice point. An error in the ice properly. The instrument manual in conjunction with the bath
point usually indicates separation of the liquid at some point in manufacturer will be sources of appropriate information.
the thermometer. X2.1.5 If manually programmed or using a custom profile,
X2.1.2 Check temperature sensor of the temperature con- examine the temperature profile program for an error and make
troller for accuracy, in accordance with 9.1. the appropriate corrections.

X2.1.3 For those instrument that require external liquid X2.2 For some instruments, the software controlling tem-
circulation: perature creates a temperature log during the test. For other
instruments a sensor connected to a strip chart recorder will
X2.1.3.1 Check whether the coolant is flowing or whether
provide the information to determine if temperature deviations
there is adequate coolant in the reservoir.
are greater than those permitted in Table X1.1 or Table X1.2
X2.1.3.2 For cold sources operating below –20 °C, replace and correct accordingly.
methanol if wet, as indicated by ice crystals in the top of the
cold source reservoir. Cold methanol absorbs water, and as it X2.3 Verify that the preheat program for 80 °C lasts for a
absorbs water, its cooling capacity decreases. In high humidity minimum of 2 h. If not, correct accordingly to the owner’s
areas, it may be necessary to change the methanol once a manual or through the instrument manufacturer.

REFERENCES

(1) Stambaugh, R. L., and O’Mara, J. H., “Low Temperature Flow (5) Henderson, K. O., Manning, R. E., May, C. J., and Rhodes, R. B.,
Properties of Engine Oils,” SAE Paper No. 821247 or 820509. “New Mini-Rotary Viscometer Temperature Profiles That Predict
(2) Shaub, H., Smith, M. F., Jr., and Murphy, C. K., “Predicting Low Engine Oil Pumpability,” SAE Paper No. 850443.
Temperature Engine Oil Pumpability with the Mini-Rotary (6) ASTM Research Report RR:D02-1442, “Cold Starting and Pumpabil-
Viscometer,” SAE Paper No. 790732, published in SAE SP-460 and ity Studies in Modern Engines,” ASTM International, W.
ASTM STP-621-S4. Conshohocken, PA, 1999 (order #COLDSTART).
(3) Stewart, R. M., Shaub, H., Smith, M. F., Jr., and Selby, T. W.,
--``,```,,,``,,,``,,`,`,,`,``,``-`-`,,`,,`,`,,`---

(7) Shaub, Harold, Editor, “Oil Flow Studies at Low Temperature in

“Summary of ASTM Activities on Low Temperature Engine Oil Modern Engines,” ASTM STP 1388, ASTM International, W.
Pumpability,” SAE Paper No. 821206. Conshohocken, PA, 2000.
(4) Smith, M. F., Jr., “Better Prediction of Engine Oil Pumpability
Through a More Effective MRV Cooling Cycle,” SAE Paper No.
831714.

SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D4684 – 20) that may impact the use of this standard. (Approved Nov. 1, 2020.)

(1) Revised subsections 2.1, 3.1.2, and 6.4.

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D4684 – 18) that may impact the use of this standard. (Approved June 1, 2020.)

(1) Revised definition for viscosity in subsection 3.1.5.

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 D4684 − 20a
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