ASTM E2509-21

Standard Test Method for Temperature Calibration of Rheometers in Isothermal Mode

SIGNIFICANCE AND USE
5.1 Rheological properties such as viscosity and storage and loss modulus change rapidly with temperature. High quality determinations of these properties depend upon a stable and well-known temperature of the measuring apparatus.  
5.2 This test method may be used for research, quality assurance, specification acceptance, and regulatory compliance.
SCOPE
1.1 This test method describes the temperature calibration or conformance of rheometers. The applicable temperature range is 0 °C to 80 °C however other ranges may be selected for the purpose at hand.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
1.4 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: 30-Sep-2021
• 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 E1142-15 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-May-2015
• Refers: ASTM E473-14 - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 15-Aug-2014
• Refers: ASTM E1142-14b - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 15-Aug-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 E1142-12 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Sep-2012
• Refers: ASTM E1142-11b - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Aug-2011
• Refers: ASTM E473-11a - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 15-Jun-2011
• Refers: ASTM E1142-11a - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 15-Jun-2011
• Refers: ASTM E473-11 - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 01-Apr-2011
• Refers: ASTM E1142-11 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Apr-2011
• Refers: ASTM E473-10 - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 01-Mar-2010
• Refers: ASTM E473-09 - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 01-Aug-2009

Overview

ASTM E2509-21, titled Standard Test Method for Temperature Calibration of Rheometers in Isothermal Mode, is an internationally recognized standard developed by ASTM International. This standard specifies the procedures for calibrating the temperature of rheometers used in isothermal mode, ensuring accurate and repeatable measurements of rheological properties such as viscosity, storage, and loss modulus. Accurate temperature calibration is essential because these properties are highly sensitive to temperature fluctuations. The standard is applicable within a temperature range of 0 °C to 80 °C, but may be adapted for other ranges as needed.

Key Topics

• Temperature Calibration of Rheometers: Provides detailed procedures for calibrating rheometers to ensure the temperature of the test specimen is both stable and known.
• Calibration Methods: Outlines single-point, two-point, and multi-point calibration techniques, allowing flexibility based on the user's requirements and the desired accuracy.
• Apparatus Requirements: Specifies the use of electronic thermometers, dummy test specimens, and rheometers with specific performance capabilities in temperature control and measurement.
• Precision and Bias: Presents guidance on evaluating the accuracy (bias) and repeatability (precision) of temperature calibration, supporting laboratories in quality assurance.
• Reporting Criteria: Defines the necessary details to report calibration results, such as instrument description, method used, calibration values, and test conditions.

Applications

ASTM E2509-21 is widely used in:

• Research Laboratories: Accurate measurement of rheological properties under isothermal conditions is vital for experimentation in material science, polymer research, and thermal analysis.
• Quality Assurance and Control: Manufacturers depend on reliable rheometer calibration to ensure consistency and regulatory compliance in product testing, particularly for polymers, rubbers, pharmaceuticals, and food products.
• Regulatory Compliance: The standard supports industries in meeting regulatory requirements related to product quality, reproducibility, and traceability.
• Specification Acceptance: Enables organizations and clients to validate equipment performance as part of acceptance criteria for new instruments or during routine audits.

Related Standards

For a comprehensive approach to rheological and thermal analysis, the following ASTM standards are referenced or closely related:

• ASTM E473: Terminology Relating to Thermal Analysis and Rheology - Provides definitions for terms used in ASTM E2509-21, such as rheometer and rheometry.
• ASTM E1142: Terminology Relating to Thermophysical Properties - Offers additional standardized terminology critical for interpreting rheological measurement results.

Practical Value

Complying with ASTM E2509-21 ensures the reliability, accuracy, and comparability of rheological measurements critical in research, manufacturing, and quality assurance environments. The standard’s procedures help minimize variability due to temperature discrepancies, supporting product development, quality control, and regulatory adherence through proven calibration methodologies.

Keywords

• Temperature calibration of rheometers
• Isothermal mode calibration
• Rheological property measurement
• ASTM E2509-21
• Quality assurance in rheology
• Thermal analysis standards
• Viscosity measurement accuracy

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: E2509 − 21
Standard Test Method for
Temperature Calibration of Rheometers in Isothermal Mode
This standard is issued under the fixed designation E2509; 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 the torque applying instrument plates of a rheometer at
constant (isothermal) temperature. The difference between the
1.1 This test method describes the temperature calibration
rheometer set temperature and that indicated by the thermom-
or conformance of rheometers. The applicable temperature
eter is used to calibrate the rheometer temperature signal.
range is 0 °C to 80 °C however other ranges may be selected
for the purpose at hand.
5. Significance and Use
1.2 The values stated in SI units are to be regarded as
5.1 Rheological properties such as viscosity and storage and
standard. No other units of measurement are included in this
loss modulus change rapidly with temperature. High quality
standard.
determinations of these properties depend upon a stable and
1.3 This standard does not purport to address all of the
well-known temperature of the measuring apparatus.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.2 This test method may be used for research, quality
priate safety, health, and environmental practices and deter-
assurance, specification acceptance, and regulatory compli-
mine the applicability of regulatory limitations prior to use.
ance.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
6. Interferences
ization established in the Decision on Principles for the
6.1 In many rheological experiments, temperature is varied
Development of International Standards, Guides and Recom-
with time. The calibration in this test method is made under
mendations issued by the World Trade Organization Technical
stable and isothermal temperature conditions. Thus the effects
Barriers to Trade (TBT) Committee.
of changes in temperature with time are not addressed. This
2. Referenced Documents
isothermal calibration does not provide any information about
the specimen under temperature scanning conditions.
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rhe-
7. Apparatus
ology
E1142 Terminology Relating to Thermophysical Properties
7.1 An electronic thermometer that includes:
7.1.1 Temperature sensor, (such as a thermocouple, plati-
3. Terminology
num resistance thermometer, thermistor, etc.) with an accuracy
3.1 Definitions—Specific technical terms found in this stan-
(traceable to a known absolute standard) and resolution of
dard are defined in Terminologies E473 and E1142, including
60.1 °C and a range of 0 °C to 80 °C.
rheometer and rheometry.
NOTE 1—Sensors with other temperature ranges may be used at the
4. Summary of Test Method
operator’s convenience.
NOTE 2—Some sensors are available already affixed with dummy test
4.1 An electronic thermometer of known characteristics is
specimens from section 7.2
placed in the center of a dummy test specimen in contact with
7.1.2 Temperature indicator, to convert the signal presented
by the temperature sensor into a digital electronic temperature
This test method is under the jurisdiction ofASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.08 on Rheol-
display with the accuracy and precision indicated in section
ogy.
7.1.1.
Current edition approved Oct. 1, 2021. Published November 2021. Originally
approved in 2008. Last previous edition approved in 2014 as E2509 – 14. DOI:
7.2 Dummy test specimen,twopolymersheetseach1mmin
10.1520/E2509-21.
thickness of such a diameter to fill the space (that is, gap)
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM between the instrument plates.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. NOTE 3—The dummy test specimen may be composed of the material
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2509 − 21
to be tested or some other representative polymer material. Polydimeth-
8. Preparation of Apparatus
ylsiloxane (PDMS) (for example, “Silly Putty” ) may be used for this
8.1 Turn on the rheometer and allow it to equilibrate for at
purpose.
least 30 minutes prior to temperature calibration.
NOTE 4—Polydimethylsiloxane may leave a residue of silicone oil on
the surfaces of the instrument plates. This oil should be removed prior to
8.2 Assemble the rheometer with the instrument plates to be
subsequent use.
used during subsequent tests.
7.3 Rheometer, the essential instrumentation required pro-
viding the minimum rheological analytical capabilities for this
9. Calibration and Standardization
test method include:
9.1 Perform any temperature calibration procedures recom-
7.3.1 A drive actuator, to apply torque or displacement to
mended by the rheometer manufacturer as described in the
the specimen in a periodic manner capable of frequencies of
instruments operations manual.
oscillation from 0.01 rad/s to 10 rad/s (1.6 mHz to 1.6 Hz).
This actuator may also be capable of providing static force or
10. Procedure
transient step or displacement of the test specimen.
10.1 Insert the temperature sensor so that it is located at the
7.3.2 Acoupling shaft, or other means to transmit the torque
vertical and radial center of the dummy test specimen.
or displacement from the actuator to the specimen.
7.3.3 A geometry, tools or plates, to fix the specimen
NOTE 5—This may be accomplished by placing the sensor between two
sheets of the dummy test specimen.
between the coupling shaft and a stationary position. For the
purposes of this test, parallel plates are the preferred configu-
10.2 Mount the dummy test specimen between the instru-
ration
ment plates. Close the gap to the dimension to be used for the
7.3.4 Either a torque sensor, to measure force developed by
test specimen, keeping the temperature sensor centered verti-
the specimen or a position sensor to measure the angular
cally and radially.
displacement, either one being capable of measuring within
NOTE 6—Other gaps and plate diameters may be used but shall be
limits appropriate to the specimen and test being performed.
reported.
7.3.5 A temperature sensor, to provide an indication of the
NOTE7—Itisnotnecessarytotrimthedummytestspecimenbutalarge
specimen temperature readable to within 60.1 °C.
excess of material beyond the edges of the plates should be avoided.
7.3.6 A furnace or heating/cooling element, to provide
10.3 Heat (or cool) the plates to the desired calibration
controlled heating or cooling of a specimen to a constant
temperature and equilibrate until the indicated temperature
temperature constant to within 60.1 °C over the temperature
changes by less than 60.1 °C in 5 min.
range of interest.
10.4 Measure and record the temperature indicated by the
7.3.7 A temperature controller, capable of executing a
thermometer as T and that of set temperature of the rheometer
o
specific temperature program by operating the furnace or
as T .
s
heating/cooling element between selected temperature limits
10.5 Determine the temperature calibration value according
constant to within 60.1 °C.
7.3.8 A stress or stain controller, capable of executing a to Section 11.
specific unidirectional or oscillatory stress or strain program
NOTE 8—Depending upon the needs of the user, a single-point
between selected stress or strain limits capable of controlling
temperature calibration may be adequate. In this case, a single offset
within limits appropriate to the specimen and test being calibration value is determined. Others may prefer a two-point tempera-
ture calibration where the temperature values of interest are selected to
performed.
encompass all test temperatures. Here, a linear interpolation of results
7.3.9 A data collecting device, to provide a means of
between the two temperature calibration points may be used. Some users
acquiring, storing, and displaying measured or calculated
may wish to calibrate the apparatus at temperature interv
...

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: E2509 − 14 E2509 − 21
Standard Test Method for
Temperature Calibration of Rheometers in Isothermal Mode
This standard is issued under the fixed designation E2509; 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 describes the temperature calibration or conformance of rheometers. The applicable temperature range is 0
°C to 80°C 80 °C however other ranges may be selected for the purpose at hand.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 There are no ISO equivalents to this standard.
1.3 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.
1.4 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 and health practices and determine the applicability of regulatory
limitations prior to use.
1.4 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:
E473 Terminology Relating to Thermal Analysis and Rheology
E1142 Terminology Relating to Thermophysical Properties
3. Terminology
3.1 Definitions—Specific technical terms found in this standard are defined in Terminologies E473 and E1142, including
rheometer and rheometry.
4. Summary of Test Method
4.1 An electronic thermometer of known characteristics is placed in the center of a dummy test specimen in contact with the torque
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 Aug. 1, 2014Oct. 1, 2021. Published August 2014November 2021. Originally approved in 2008. Last previous edition approved in 20082014
as E2509 – 08.E2509 – 14. DOI: 10.1520/E2509-14.10.1520/E2509-21.
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
E2509 − 21
applying instrument plates of a rheometer at constant (isothermal) temperature. The difference between the rheometer set
temperature and that indicated by the thermometer is used to calibrate the rheometer temperature signal.
5. Significance and Use
5.1 Rheological properties such as viscosity and storage and loss modulus change rapidly with temperature. High quality
determinations of these properties depend upon a stable and well-known temperature of the measuring apparatus.
5.2 This test method may be used for research, quality assurance, specification acceptance, and regulatory compliance.
6. Interferences
6.1 In many rheological experiments, temperature is varied with time. The calibration in this test method is made under stable and
isothermal temperature conditions. Thus the effects of changes in temperature with time are not addressed. This isothermal
calibration does not provide any information about the specimen under temperature scanning conditions.
7. Apparatus
7.1 An electronic thermometer that includes:
7.1.1 Temperature sensor, (such as a thermocouple, platinum resistance thermometer, thermistor, etc.) with an accuracy (traceable
to a known absolute standard) and resolution of 60.1°C 60.1 °C and a range of 0 °C to 80°C. 80 °C.
NOTE 1—Sensors with other temperature ranges may be used at the operator’s convenience.
NOTE 2—Some sensors are available already affixed with dummy test specimens from section 7.2
7.1.2 Temperature indicator, to convert the signal presented by the temperature sensor into a digital electronic temperature display
with the accuracy and precision indicated in section 7.1.1.
7.2 Dummy test specimen, two polymer sheets each 1 mm in thickness of such a diameter to fill the space (that is, gap) between
the instrument plates.
NOTE 3—The dummy test specimen may be composed of the material to be tested or some other representative polymer material. Polydimethylsiloxane
(PDMS) (for example, “Silly Putty” ) may be used for this purpose.
NOTE 4—Polydimethylsiloxane may leave a residue of silicone oil on the surfaces of the instrument plates. This oil should be removed prior to subsequent
use.
7.3 Rheometer, the essential instrumentation required providing the minimum rheological analytical capabilities for this test
method include:
7.3.1 A drive actuator, to apply torque or displacement to the specimen in a periodic manner capable of frequencies of oscillation
from 0.01 rad/s to 10 rad/s (0.0016 (1.6 mHz to 1.6 Hz). This actuator may also be capable of providing static force or transient
step or displacement of the test specimen.
7.3.2 A coupling shaft, or other means to transmit the torque or displacement from the actuator to the specimen.
7.3.3 A geometry, tools or plates, to fix the specimen between the coupling shaft and a stationary position. For the purposes of
this test, parallel plates are the preferred configuration
7.3.4 Either a torque sensor, to measure force developed by the specimen or a position sensor to measure the angular displacement
, displacement, either one being capable of measuring within limits appropriate to the specimen and test being performed.
7.3.5 A temperature sensor, to provide an indication of the specimen temperature readable to within 60.1°C.60.1 °C.
The trademark Silly Putty is registered to Crayola Properties, inc., Easton, PA, 18042.
E2509 − 21
7.3.6 A furnace or heating/cooling element, to provide controlled heating or cooling of a specimen to a constant temperature
constant to within 60.1°C 60.1 °C over the temperature range of interest.
7.3.7 A temperature controller, capable of executing a specific temperature program by operating the furnace or heating/cooling
element between selected temperature limits constant to within 60.1°C.60.1 °C.
7.3.8 A stress or stain controller, capable of executing a specific unidirectional or oscillatory stress or strain program between
selected stress or strain limits capable of controlling within limits appropriate to the specimen and test being performed.
7.3.9 A data collecting device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.
The minimum output signals required include applied force, position or frequency or calculated signal (such as viscosity, storage
modulus, loss modulus, or tangent delta) using a linear or logarithmic scale and the independent experimental parameters (such
as temperature, time, stress, strain, or frequency of oscillation).
7.3.10 Auxiliary instrumentation considered necessary or useful in conducting this test method includes:
7.3.10.1 A cooling capability to hasten cool down from elevated temperatures, to provide constant cooling rates, or to sustain an
isothermal subambient temperature.
7.3.10.2 Data analysis capability, to provide determined signals (such as viscosity, storage, or loss modulus) or other useful
parameters derived from the measured signals.
8. Preparation of Apparatus
8.1 Turn on the rheometer and allow it to equilibrate for at least 30 minutes prior to temperature calibration.
8.2 Assemble the rheometer with the instrument plates to be used during subsequent tests.
9. Calibration and Standardization
9.1 Perform any temperature calibration procedures recommended by the rheometer manufacturer as described in the instruments
operations manual.
10. Procedure
10.1 Insert the temperature sensor so that it is located at the vertical and radial center of the dummy test specimen.
NOTE 5—This may be accomplished by placing the sensor between two sheets of the dummy test specimen.
10.2 Mount the dummy test specimen between the instrument plates. Close the gap to the dimension to be used for the test
specimen, keeping the temperatu
...