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: E3116 − 18

Standard Test Method for

Viscosity Measurement Validation of Rotational
Viscometers1
This standard is issued under the fixed designation E3116; 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 E2161 Terminology Relating to Performance Validation in

1.1 This test method provides procedures for validating Thermal Analysis and Rheology
viscosity measurements by rotational viscometers of Newto- E2975 Test Method for Calibration or Calibration Verifica-
nian fluids. Performance parameters determined include vis- tion of Concentric Cylinder Rotational Viscometers
cosity repeatability (precision), detection limit, quantitation
limit, linearity, and bias. 3. Terminology
1.2 Validation of apparatus performance and analytical 3.1 Definitions:
methods is requested or required for quality initiatives or where 3.1.1 Technical terms used in this standard are defined in
results may be used for legal purposes. Practice E177 and in Terminologies E473, E1142, and E2161
including analyte, calibration, Celsius, detection limit,
1.3 The values stated in SI units are to be regarded as
linearity, Newtonian, non-Newtonian, precision, quantitation
standard. No other units of measurement are included in this
limit, reference materials, relative standard deviation,
standard.
repeatability, shear, slope, standard deviation, validation,
1.4 This standard does not purport to address all of the viscometer, and viscosity.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4. Summary of Test Method
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 4.1 Viscosity is the primary dependent parameter and either
1.5 This international standard was developed in accor- torque or rotational speed is the primary independent parameter
dance with internationally recognized principles on standard- measured by rotational viscometry. Viscosity is strongly de-
ization established in the Decision on Principles for the pendent upon temperature and so temperature is usually held
Development of International Standards, Guides and Recom- constant.
mendations issued by the World Trade Organization Technical 4.2 Viscosity is validated by the direct measurement using a
Barriers to Trade (TBT) Committee. concentric cylinder rotational viscometer at an isothermal
temperature using reference materials of known viscosity as an
2. Referenced Documents
analyte.
2.1 ASTM Standards:2
4.3 Alternatively, validation of a rotational viscometry
E177 Practice for Use of the Terms Precision and Bias in
method based upon viscosity measurement may be performed
ASTM Test Methods
using a specific test specimen as the analyte.
E473 Terminology Relating to Thermal Analysis and Rhe-
ology 4.4 The viscosity of three or more specimens, nominally
E1142 Terminology Relating to Thermophysical Properties representing the minimum, midpoint and maximum of the
E1970 Practice for Statistical Treatment of Thermoanalytical range of the test method, are measured at least in triplicate.
Data
NOTE 1—Repeatability is determined by performing a sufficient number
of determinations to calculate statistically valid estimates of the standard
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal deviation or relative standard deviation of the measurements.
Measurements and is the direct responsibility of Subcommittee E37.08 on Rheol-
ogy.
4.4.1 Viscosity linearity and bias are determined from the
Current edition approved Jan. 1, 2018. Published January 2018. DOI: 10.1520/ linear regression (best-fit) straight-line correlation of the results
E3116-18. from measurements of the three or more specimens.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.4.2 Viscosity repeatability, detection limits and quantita-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on tion limits are determined from the standard deviation of the
the ASTM website. measurement of three or more analyte-containing specimens.

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 E3116 − 18
4.5 A spindle is rotated in a Newtonian fluid at a known (or 7.1.3 A cylindrical rotational element, spindle, geometry, or
measured) speed. The viscosity drag experienced by the tool, composed of a material inert to the material being tested,
immersed spindle is measured (or known) as a torque. Viscos- to fix the specimen between the coupling shaft and a stationary
ity may then be determined from these properties (torque and position.
rotational speed) and the dimensions of the spindle by equa- 7.1.4 A sensor to measure the torque within 61 % of full
tions such as Eq 1 and Eq 2. scale developed by the specimen.
η5τ S ⁄ ω (1) 7.1.5 A temperature sensor to provide an indication of the
2 2 2 2
specimen temperature over the range of 19 to 26°C to within
S 5 ~r 2 r ! ⁄ ~4 π r r L! (2)
c s c s 60.1°C.
where: 7.1.6 A data collection device, to provide a means of
η = viscosity, Pa-s, acquiring, storing, and displaying measured or calculated
ω = rotational speed, r/min, signals, or both. The minimum output signals required are
τ = torque, N-m, torque, rotational speed, temperature, and time.
rc = radius of the cylindrically shaped container, m, 7.1.7 A stand, to support, level, lower, and raise the drive
rs = radius of the cylindrically shaped spindle, m, motor, shaft and rotational element.
L = length of the cylindrically shaped spindle, m, and 7.2 A specimen container, cylindrical or disk in shape, to
S = instrument or experimental calibration constant, m-3.
2
contain the test specimen during testing.
NOTE 2—1 Pa = 1 N/m ; 60 s = 1 min.
NOTE 4—The specific container may depend upon the rotational
5. Significance and Use element being used (see vendor’s recommendations). In the absence of
other information, a low form Griffin beaker of 600-mL capacity shall be
5.1 This test method may be used to validate the perfor- used.
mance of a specific rotational viscometer apparatus. 7.3 A temperature bath and controller to provide a con-
5.2 This test method may be used to validate the perfor- trolled isothermal temperature environment for the specimen
mance of a specific method based upon the measurement of within the range of 19 to 26°C constant to within 60.1°C.
viscosity using rotational viscometer apparatus. 7.4 Auxiliary instrumentation considered useful in conduct-
5.3 This test method may be used to determine the repeat- ing this test method includes:
ability of a specific apparatus, operator, or laboratory. 7.4.1 Data analysis capability to provide viscosity, stress or
other useful quantities derived from the measured signals.
5.4 This test method may be used for specification or 7.4.2 A level to indicate the vertical plumb of the drive
regulatory compliance purposes. motor, shaft and rotational element.

6. Interferences 8. Reagents and Materials

6.1 Viscosity is highly dependent upon temperature. Mate- 8.1 Three or more viscosity reference fluids (with accom-
rials may change by as much as 7 % per Celsius degree. For panying certificates) representing the minimum, midpoint and
this reason, all measurements shall be made in the same maximum viscosity range to be validated by the procedure.
temperature controlled environment. NOTE 5—Viscosity reference materials are typically available from the
viscometer supplier.
6.2 This test method assumes that the analyte exhibits
Newtonian behavior, that is viscosity is linearly dependent 9. Preparation of Apparatus
upon shear rate (rotational speed) and a linear applied force
(torque). Many materials of interest, however, are non- 9.1 Perform any viscometer preparation or calibration pro-
Newtonian in nature where the measured viscosity varies with cedures described in the apparatus operations manual or
shear rate. Care shall be exercised in the selection of a according to Test Method E2975.
reference material analyte for this test method that is Newto- 9.2 Operate the viscometer in air with a connected rotational
nian in nature. element in place. The indicator shall be stable and indicate a
zero value.
7. Apparatus 9.3 Set the temperature bath at 25°C and equilibrate for 30
7.1 Viscometer, Rotational—The essential instrumental re- min. Measure the temperature bath and ensure that it is 25 6
quired providing the minimum rotational viscometer analytical 0.2°C.
capabilities for this test method include: NOTE 6—Other temperatures may be used but shall be reported.
7.1.1 A drive motor, to apply a rotational displacement to
the specimen at a rate of 0.2 r/min to 200 r/min constant to 10. Procedure
60.2 % of full scale. 10.1 Place the required amount of medium viscosity refer-
7.1.2 A coupling shaft or other means, to transmit the ence material in the specimen container. Record the reference
rotational displacement from the motor to the specimen. viscosity value from its certificate as ηmedREF.
NOTE 3—It is convenient to have a mark on the shaft to indicate the NOTE 7—The amount of viscosity reference material needed varies with
fluid level of the test specimen appropriate for the measurement. each rotational element and container combination. See the instrument

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 E3116 − 18
operation’s manual for the correct amount of liquid for each element- 10.13 Determine the mean viscosity value for ηmax and its
container pair. standard deviation σmax.
NOTE 8—Pour the reference material slowly down the side of specimen
container taking care to prevent incorporation of air bubbles into the 10.14 Repeat steps 10.1 through 10.10 for (nmin = 3) the
material. minimum viscosity reference material recording ηminREF,
10.2 Place the container with its reference material in the ηmin1, ηmin2, ηmin3, ωmin1, ωmin2, ωmin3, Tmin1, Tmin2, and
temperature bath at 25 6 0.2°C and equilibrate for 30 minutes. Tmin3.
NOTE 9—Other temperatures may be used but shall be reported. 10.15 Calculate the mean viscosity value for ηmin and its
10.3 Vertically align and level the viscometer motor, shaft standard deviation σmin.
and rotational element on its supporting stand over the speci- 10.16 Using the values from 10.11, 10.13, and 10.15 and Eq
men container. 3, calculate the viscosity relative standard deviation for
10.4 Slowly lower the rotational element into the test RSDmin, RSDmed, and RSDmax.
specimen until the fluid reaches the appropriate level indicated 10.17 Using the values from 10.11, 10.13, 10.15, and 10.16
in the operation’s manual. and Eq 4, calculate the repeatability value r.
NOTE 10—The shaft may have a mark to indicate the appropriate fluid 10.18 Calculate the detectability limit (DL) using Eq 5.
level for the measurement.
NOTE 11—Ensure that no air bubbles are trapped under the rotational 10.19 Calculate the quantitation limit (QL) using Eq 6.
element. 10.20 Using the reference viscosity values (ηxREF) for the
10.5 Initiate the rotation of the rotational element at 0.5 minimum (min), medium (med) and maximum (max) viscosity
r/min for 30 min. reference material from steps 10.1, 10.12, and 10.14 as the
10.6 Increase (or decrease) the rotational speed to that independent (X) values and the three (or more) determined
required to produce a reading nearest the midpoint of the scale. mean viscosity values from steps 10.11, 10.13, and 10.15 as the
dependent (Y) values, determine by linear regression the slope
10.7 Stop the rotation of the element and wait for 1 min.
(m), and intercept (b) of a correlation best-fit line (see Practice
10.8 Restart the rotational at the same rotational speed (or E1970).
torque) and allow at least 5 revolutions of the element.
NOTE 13—The value of m will be close to unity. b has the units of
10.9 Measure and record the observed viscosity ηmed1 (or viscosity (nominally Pa-s).
torque τmed1), rotational speed ωmed1 and temperature Tmed1.
10.21 Determine the deviation values (δYmin, δYmed, and
NOTE 12—If the temperature is not 25.0 6 0.2°C, discard the δYmax) for each of the mean minimum, medium, and maximum
measurement, allow the test specimen to equilibrate for an additional 30 viscosity values using Eq 7 and the values of m and b from
min or until the desired temperature range and stability is observed, and
remeasure.
10.20.
10.10 Repeat steps 10.7 through 10.9 two more times, 10.22 Determine which deviation value from step 10.21 has
measuring the indicated viscosity as ηmed2 and ηmed3 (or the largest absolute value and identify it as δYlargest.
torque τmed2 and τmed3), rotational speed ωmed2 and ωmed3, and 10.23 Determine linearity (L) using Eq 8.
temperature Tmed2 and Tmed3.
10.24 Determine the bias using Eq 9.
10.11 Using the three (nmed = 3) values for viscosity from
steps 10.9 and 10.10, calculate the mean value for ηmed and 11. Calculations
σmed (see Practice E1970).
11.1 Relative standard deviation (RSD) is given by Eq 3 (see
10.12 Repeat steps 10.1 through 10.11 for (nmax = 3) the Practice E1970):
maximum viscosity reference material recording ηmaxREF,
ηmax1, ηmax2, ηmax3, ωmax1, ωmax2, ωmax3, Tmax1, Tmax2, and RSD 5 σ 3 100 % ⁄ mean value (3)
Tmax3. 11.2 The repeatability (r) value is given by Eq 4:

r 5 s f h s n min 2 1 d RSD min

2
j 1 h s n med 2 1 d RSD med
2
j 1 h s n max 2 1 d RSD max
2
j g ⁄ f s n min 2 1 d 1 s n med 2 1 d 1 s n max 2 1 d g d 1⁄2 (4)

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 E3116 − 18
11.3 The detection limit (DL) is given by Eq 5: ηminREF = 200.0 mPa-s
DL 5 3.3 r η min ⁄ 100 % (5) ηmedREF = 500.0 mPa-s
ηmaxREF = 800.0 mPa-s
11.4 The quantitation limit (QL) is given by Eq 6: ηmin = 190.0 mPa-s
QL 5 10 r η min ⁄ 100 % (6) ηmed = 487.5 mPa-s
11.5 Correlation slope (m) and intercept (b) are obtained ηmax = 800.0 mPa-s
nmin = 3
from a display of the measured viscosity values from 10.10,
nmed = 3
10.12, and 10.14 on the Y-axis and reference viscosity values nmax = 3
from 10.11, 10.13, and 10.15 on the X-axis such as that shown σmin = 2.0 mPa-s
in Fig. 1. Using linear regression (see Practice E1970) deter- σmed = 5.0 mPa-s
mine the slope (m) and intercept (b) of the correlation line. σmax = 5.4 mPa-s
11.6 Deviation is given by Eq 7: 12.1.1 Relative Standard Deviation:
?
δY 5 η 2 m ηREF 2 b ? (7)
RSDmin = 2.0 mPa-s × 100 % / 190.0 mPa-s = 1.05 %
where: RSDmed = 5.0 mPa-s × 100 % / 487.5 mPa-s = 1.03 %
η = the experimentally determined mean viscosity value RSDmax = 5.4 mP-s × 100 % / 800.0 mPa-s = 0.68 %
(from steps 10.11, 10.13, and 10.15), and
ηREF = the corresponding known viscosity reference value. 12.1.2 Repeatability:
11.6.1 Select the largest δY value as δYlargest. r = {(3 – 1) × (1.05 %)2} + {(3 – 1) × (1.03 %)2} + {(3 – 1)
11.7 Percent linearity (L) is given by: × (0.68 %)2} / {(3 – 1) + (3 – 1) + (3 – 1)}]1/2
= [{(2 × 1.103 %2) + (2 × 1.061 %2) + (2 × 0.462 %2)} /
L 5 @ ~ 100 % 3 δY largest! ⁄ ~ m 3 η max REF 1 b ! # (8) {2 + 2 + 2}]1/2
11.8 Bias (Bias) is given by: = [{2.206 + 2.122 + 0.924} / 6]1/2 %
= [5.252 / 6]1/2 % = 0.87531/2 %
Bias 5 b (9)
= 0.94 %
12. Example Calculations
12.1 For the example calculations described below, the
following experimental values are used:

FIG. 1 Correlation of Measured Viscosity with Reference Viscosity

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 E3116 − 18
12.1.3 Detection Limit: 12.1.8 Bias:
DL = 3.3 × 0.94 % × 190.0 mPa-s / 100 % Bias = –15.8 mPa-s
= 21 mPa-s
13. Report
12.1.4 Quantitation Limit:
13.1 A complete description of the apparatus including the
QL = 10 × 0.94 % × 190.0 mPa-s / 100 % manufacturer, model number, spindle type and configuration
= 21 mPa-s and container.
12.1.5 Correlation Slope and Intercept from Fig. 1: NOTE 14—The cylindrical spindle may be generically described using
the radius and length; the container by its inside diameter.
m = 1.0167 13.2 Some or all of the performance parameters described
b = –15.8 mPa-s by this test method useful for the application at hand including:
12.1.6 Deviations: 13.2.1 Viscosity range (ηminREF to ηmaxREF),
13.2.2 Temperature,
δYmin = |(190.9 mPa-s – 1.0167 × 200.0 mPa-s) – (–15.8 13.2.3 Viscosity repeatability (r), detection limit (DL), and
mPa-s)| quantitation limit (QL),
= |(190.9 – 203.3 + 15.8) mPa-s| 13.2.4 Viscosity linearity (L), and
= 3.4 mPa-s 13.2.5 Viscosity bias (Bias).
δYmed = 5.05 mPa-s
δYmax = 2.44 mPa-s 14. Precision and Bias
12.1.7 Linearity: 14.1 Precision and bias are determined by the procedures in
this standard. No separate precision and bias information is
L = [100 % × 5.05 mPa-s] / [(1.0167 × 800.0 mPa-s + (–15.8 required.
mPa-s)]
15. Keywords
= [505 %] / [813.4 – 15.8]
= 505 % / 797.6 15.1 detection limit; linearity; precision; quantitation limit;
= 0.63 % range; repeatability; rheology; rotational viscometry; valida-
tion; viscosity

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