ASTM E3116-23

Standard Test Method for Viscosity Measurement Validation of Rotational Viscometers

SIGNIFICANCE AND USE
5.1 This test method may be used to validate the performance of a specific rotational viscometer apparatus.  
5.2 This test method may be used to validate the performance of a specific method based upon the measurement of viscosity using rotational viscometer apparatus.  
5.3 This test method may be used to determine the repeatability of a specific apparatus, operator, or laboratory.  
5.4 This test method may be used for specification or regulatory compliance purposes.
SCOPE
1.1 This test method provides procedures for validating viscosity measurements by rotational viscometers of Newtonian fluids. Performance parameters determined include viscosity repeatability (precision), detection limit, quantitation limit, linearity, and bias.  
1.2 Validation of apparatus performance and analytical methods is requested or required for quality initiatives or where results may be used for legal purposes.  
1.3 The values stated in SI units are the standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

General Information

• Status: Published
• Publication Date: 31-May-2023
• ICS: 17.060 - Measurement of volume, mass, density, viscosity
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.08 - Rheology

Relations

• Refers: ASTM E1142-23b - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Oct-2023
• Refers: ASTM E473-23b - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 01-Oct-2023
• Refers: ASTM E2975-16 - Standard Test Method for Calibration or Calibration Verification of Concentric Cylinder Rotational Viscometers
• Effective Date: 01-Dec-2016
• Refers: ASTM E2161-15 - Standard Terminology Relating to Performance Validation in Thermal Analysis and Rheology
• Effective Date: 01-Sep-2015
• Refers: ASTM E2975-15 - Standard Test Method for Calibration of Concentric Cylinder Rotational Viscometers
• Effective Date: 01-Sep-2015
• Refers: ASTM E1142-15 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-May-2015
• Refers: ASTM E1142-14b - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 15-Aug-2014
• Refers: ASTM E473-14 - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 15-Aug-2014
• Refers: ASTM E2975-14 - Standard Test Method for Calibration of Concentric Cylinder Rotational Viscometers
• Effective Date: 01-Aug-2014
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E1142-14a - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Apr-2014
• Refers: ASTM E1142-14 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 15-Feb-2014
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E2161-13 - Standard Terminology Relating to Performance Validation in Thermal Analysis
• Effective Date: 01-Mar-2013
• Refers: ASTM E1142-12 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Sep-2012

Overview

ASTM E3116-23 is the Standard Test Method for Viscosity Measurement Validation of Rotational Viscometers. Developed by ASTM, this international standard outlines robust procedures for validating viscosity measurements using rotational viscometers, specifically for Newtonian fluids. The test method establishes protocols for determining key performance parameters such as viscosity repeatability (precision), detection limit, quantitation limit, linearity, and bias. These benchmarks support laboratories and manufacturers in delivering reliable, reproducible, and regulatory-compliant viscosity data-critical in industries including pharmaceuticals, chemicals, food, and materials science.

Key Topics

• Performance Validation: The standard enables validation of specific rotational viscometer apparatus and methods, ensuring equipment and procedures yield accurate viscosity measurements.
• Repeatability Assessment: Used to evaluate repeatability across apparatus, operators, or laboratories, enhancing quality control programs.
• Comprehensive Parameter Determination:
  • Viscosity repeatability
  • Detection limit and quantitation limit
  • Linearity of response and measurement bias
• Reference Materials: Uses certified reference fluids covering the operational viscosity range, promoting measurement traceability and confidence.
• Temperature Control: Strong emphasis is placed on isothermal measurement conditions, as viscosity can vary significantly with temperature.

Applications

• Laboratory Quality Assurance: Laboratories use ASTM E3116-23 to validate viscometer performance and analytical methods during instrument setup, operator training, and routine QC checks.
• Regulatory and Specification Compliance: The method aligns with requirements for validated results in industrial quality assurance as well as regulatory submissions where viscosity data may be a legal or compliance requirement.
• Method Transfer and Inter-Lab Comparisons: Facilitates data comparability when transferring methods between laboratories or evaluating new equipment, supporting robust inter-lab consistency.
• Materials Characterization: Applied in the characterization of Newtonian fluids-such as oils, polymers, and specialty chemicals-where certified viscosity measurements are essential to production, formulation, or research processes.
• Performance Documentation: Supports documentation and reporting of apparatus configuration, test conditions, and validation outcomes, aiding in audits and traceability.

Related Standards

ASTM E3116-23 references several complementary ASTM standards that enhance its applicability and precision:

• ASTM E177: Practice for Use of Precision and Bias Terms in ASTM Test Methods
• ASTM E473: Terminology Relating to Thermal Analysis and Rheology
• ASTM E1142: Terminology Relating to Thermophysical Properties
• ASTM E1970: Practice for Statistical Treatment of Thermoanalytical Data
• ASTM E2161: Terminology Relating to Performance Validation in Thermal Analysis and Rheology
• ASTM E2975: Test Method for Calibration or Calibration Verification of Concentric Cylinder Rotational Viscometers

Practical Value

Implementing ASTM E3116-23 supports:

• Consistent Viscosity Validation: Assures that rotational viscometric analyses are trustworthy for Newtonian fluid measurements.
• Operational Excellence: Enhances equipment utilization, reduces downtime due to invalid measurements, and streamlines troubleshooting.
• Traceable Reporting: Standardized reporting and calculation frameworks help laboratories demonstrate measurement capability and compliance.

By following ASTM E3116-23, organizations can foster greater confidence in viscosity data, meeting industry and regulatory expectations for measurement quality, repeatability, and transparency across global operations.

Standards Content (Sample)

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 − 23
Standard Test Method for
Viscosity Measurement Validation of Rotational
Viscometers
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
Thermal Analysis and Rheology
1.1 This test method provides procedures for validating
E2975 Test Method for Calibration or Calibration Verifica-
viscosity measurements by rotational viscometers of Newto-
tion of Concentric Cylinder Rotational Viscometers
nian fluids. Performance parameters determined include vis-
cosity repeatability (precision), detection limit, quantitation
3. Terminology
limit, linearity, and bias.
3.1 Definitions:
1.2 Validation of apparatus performance and analytical
3.1.1 Technical terms used in this standard are defined in
methods is requested or required for quality initiatives or where
Practice E177 and in Terminologies E473, E1142, and E2161
results may be used for legal purposes.
including analyte, calibration, Celsius, detection limit,
1.3 The values stated in SI units are the standard. No other
linearity, Newtonian, non-Newtonian, precision, quantitation
units of measurement are included in this standard.
limit, reference materials, relative standard deviation,
1.4 This standard does not purport to address all of the
repeatability, shear, slope, standard deviation, validation,
safety concerns, if any, associated with its use. It is the
viscometer, and viscosity.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Summary of Test Method
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
Barriers to Trade (TBT) Committee.
4.2 Viscosity is validated by the direct measurement using a
concentric cylinder rotational viscometer at an isothermal
2. Referenced Documents
temperature using reference materials of known viscosity as an
2.1 ASTM Standards:
analyte.
E177 Practice for Use of the Terms Precision and Bias in
4.3 Alternatively, validation of a rotational viscometry
ASTM Test Methods
method based upon viscosity measurement may be performed
E473 Terminology Relating to Thermal Analysis and Rhe-
using a specific test specimen as the analyte.
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
1 of determinations to calculate statistically valid estimates of the standard
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 June 1, 2023. Published June 2023. Originally
linear regression (best-fit) straight-line correlation of the results
approved in 2018. Last previous edition approved in 2018 as E3116 – 18. DOI:
10.1520/E3116-23.
from measurements of the three or more specimens.
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 [e-mail]. For Annual Book of ASTM
tion limits are determined from the standard deviation of the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. measurement of three or more analyte-containing specimens.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E3116 − 23
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.
7.1.5 A temperature sensor to provide an indication of the
η 5 τ S ⁄ ω (1)
specimen temperature over the range of 19 °C to 26 °C to
2 2 2 2
S 5 ~r 2 r ! ⁄ ~4 π r r L! (2)
c s c s
within 60.1 °C.
7.1.6 A data collection device, to provide a means of
where:
acquiring, storing, and displaying measured or calculated
η = viscosity, Pa-s,
signals, or both. The minimum output signals required are
ω = rotational speed, r/min,
torque, rotational speed, temperature, and time.
τ = torque, N-m,
r = radius of the cylindrically shaped container, m, 7.1.7 A stand, to support, level, lower, and raise the drive
c
r = radius of the cylindrically shaped spindle, m, motor, shaft and rotational element.
s
L = length of the cylindrically shaped spindle, m, and
7.2 A specimen container, cylindrical or disk in shape, to
-3
S = instrument or experimental calibration constant, m .
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
element being used (see vendor’s recommendations). In the absence of
5. Significance and Use
other information, a low form Griffin beaker of 600-mL capacity shall be
used.
5.1 This test method may be used to validate the perfor-
mance of a specific rotational viscometer apparatus.
7.3 A temperature bath and controller to provide a con-
trolled isothermal temperature environment for the specimen
5.2 This test method may be used to validate the perfor-
within the range of 19 °C to 26 °C constant to within 60.1 °C.
mance of a specific method based upon the measurement of
viscosity using rotational viscometer apparatus.
7.4 Auxiliary instrumentation considered useful in conduct-
ing this test method includes:
5.3 This test method may be used to determine the repeat-
7.4.1 Data analysis capability to provide viscosity, stress or
ability of a specific apparatus, operator, or laboratory.
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.
8. Reagents and Materials
6. Interferences
8.1 Three or more viscosity reference fluids (with accom-
6.1 Viscosity is highly dependent upon temperature. Mate-
panying certificates) representing the minimum, midpoint and
rials may change by as much as 7 % per Celsius degree. For
maximum viscosity range to be validated by the procedure.
this reason, all measurements shall be made in the same
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
9.1 Perform any viscometer preparation or calibration pro-
(torque). Many materials of interest, however, are non-
cedures described in the apparatus operations manual or
Newtonian in nature where the measured viscosity varies with
according to Test Method E2975.
shear rate. Care shall be exercised in the selection of a
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
min. Measure the temperature bath and ensure that it is 25 °C
7.1 Viscometer, Rotational—The essential instrumental re-
6 0.2 °C.
quired providing the minimum rotational viscometer analytical
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
10. Procedure
the specimen at a rate of 0.2 r/min to 200 r/min constant to
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
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E3116 − 18 E3116 − 23
Standard Test Method for
Viscosity Measurement Validation of Rotational
Viscometers
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
1.1 This test method provides procedures for validating viscosity measurements by rotational viscometers of Newtonian fluids.
Performance parameters determined include viscosity repeatability (precision), detection limit, quantitation limit, linearity, and
bias.
1.2 Validation of apparatus performance and analytical methods is requested or required for quality initiatives or where results may
be used for legal purposes.
1.3 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E473 Terminology Relating to Thermal Analysis and Rheology
E1142 Terminology Relating to Thermophysical Properties
E1970 Practice for Statistical Treatment of Thermoanalytical Data
E2161 Terminology Relating to Performance Validation in Thermal Analysis and Rheology
E2975 Test Method for Calibration or Calibration Verification of Concentric Cylinder Rotational Viscometers
3. Terminology
3.1 Definitions:
3.1.1 Technical terms used in this standard are defined in Practice E177 and in Terminologies E473, E1142, and E2161 including
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.08 on Rheology.
Current edition approved Jan. 1, 2018June 1, 2023. Published January 2018June 2023. Originally approved in 2018. Last previous edition approved in 2018 as E3116 – 18.
DOI: 10.1520/E3116-18.10.1520/E3116-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E3116 − 23
analyte, calibration, Celsius, detection limit, linearity, Newtonian, non-Newtonian, precision, quantitation limit, reference
materials, relative standard deviation, repeatability, shear, slope, standard deviation, validation, viscometer, and viscosity.
4. Summary of Test Method
4.1 Viscosity is the primary dependent parameter and either torque or rotational speed is the primary independent parameter
measured by rotational viscometry. Viscosity is strongly dependent upon temperature and so temperature is usually held constant.
4.2 Viscosity is validated by the direct measurement using a concentric cylinder rotational viscometer at an isothermal temperature
using reference materials of known viscosity as an analyte.
4.3 Alternatively, validation of a rotational viscometry method based upon viscosity measurement may be performed using a
specific test specimen as the analyte.
4.4 The viscosity of three or more specimens, nominally representing the minimum, midpoint and maximum of the range of the
test method, are measured at least in triplicate.
NOTE 1—Repeatability is determined by performing a sufficient number of determinations to calculate statistically valid estimates of the standard deviation
or relative standard deviation of the measurements.
4.4.1 Viscosity linearity and bias are determined from the linear regression (best-fit) straight-line correlation of the results from
measurements of the three or more specimens.
4.4.2 Viscosity repeatability, detection limits and quantitation limits are determined from the standard deviation of the
measurement of three or more analyte-containing specimens.
4.5 A spindle is rotated in a Newtonian fluid at a known (or measured) speed. The viscosity drag experienced by the immersed
spindle is measured (or known) as a torque. Viscosity may then be determined from these properties (torque and rotational speed)
and the dimensions of the spindle by equations such as Eq 1 and Eq 2.
η 5 τ S ⁄ ω (1)
2 2 2 2
S 5 r 2 r ⁄ 4 π r r L (2)
~ ! ~ !
c s c s
where:
η = viscosity, Pa-s,
ω = rotational speed, r/min,
τ = torque, N-m,
r = radius of the cylindrically shaped container, m,
c
r = radius of the cylindrically shaped spindle, m,
s
L = length of the cylindrically shaped spindle, m, and
-3
S = instrument or experimental calibration constant, m .
NOTE 2—1 Pa = 1 N/m ; 60 s = 1 min.
5. Significance and Use
5.1 This test method may be used to validate the performance of a specific rotational viscometer apparatus.
5.2 This test method may be used to validate the performance of a specific method based upon the measurement of viscosity using
rotational viscometer apparatus.
5.3 This test method may be used to determine the repeatability of a specific apparatus, operator, or laboratory.
5.4 This test method may be used for specification or regulatory compliance purposes.
E3116 − 23
6. Interferences
6.1 Viscosity is highly dependent upon temperature. Materials may change by as much as 7 % per Celsius degree. For this reason,
all measurements shall be made in the same temperature controlled environment.
6.2 This test method assumes that the analyte exhibits Newtonian behavior, that is viscosity is linearly dependent upon shear rate
(rotational speed) and a linear applied force (torque). Many materials of interest, however, are non-Newtonian in nature where the
measured viscosity varies with shear rate. Care shall be exercised in the selection of a reference material analyte for this test
method that is Newtonian in nature.
7. Apparatus
7.1 Viscometer, Rotational—The essential instrumental required providing the minimum rotational viscometer analytical
capabilities for this test method include:
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 60.2 %
of full scale.
7.1.2 A coupling shaft or other means, to transmit the rotational displacement from the motor to the specimen.
NOTE 3—It is convenient to have a mark on the shaft to indicate the fluid level of the test specimen appropriate for the measurement.
7.1.3 A cylindrical rotational element, spindle, geometry, or tool, composed of a material inert to the material being tested, to fix
the specimen between the coupling shaft and a stationary position.
7.1.4 A sensor to measure the torque within 61 % of full scale developed by the specimen.
7.1.5 A temperature sensor to provide an indication of the specimen temperature over the range of 19 to 26°C to within
60.1°C.19 °C to 26 °C to within 60.1 °C.
7.1.6 A data collection device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.
The minimum output signals required are torque, rotational speed, temperature, and time.
7.1.7 A stand, to support, level, lower, and raise the drive motor, shaft and rotational element.
7.2 A specimen container, cylindrical or disk in shape, to contain the test specimen during testing.
NOTE 4—The specific container may depend upon the rotational element being used (see vendor’s recommendations). In the absence of other information,
a low form Griffin beaker of 600-mL capacity shall be used.
7.3 A temperature bath and controller to provide a controlled isothermal temperature environment for the specimen within the
range of 19 to 26°C19 °C to 26 °C constant to within 60.1°C.60.1 °C.
7.4 Auxiliary instrumentation considered useful in conducting this test method includes:
7.4.1 Data analysis capability to provide viscosity, stress or other useful quantities derived from the measured signals.
7.4.2 A level to indicate the vertical plumb of the drive motor, shaft and rotational element.
8. Reagents and Materials
8.1 Three or more viscosity reference fluids (with accompanying certificates) representing the minimum, midpoint and maximum
viscosity range to be validated by the procedure.
NOTE 5—Viscosity reference materials are typically available from the viscometer supplier.
E3116 − 23
9. Preparation of Apparatus
9.1 Perform any viscometer preparation or calibration procedures described in the apparatus operations manual or according to
Test Method E2975.
9.2 Operate the viscometer in air with a connected rotational element in place. The indicator shall be stable and indicate a zero
value.
...