ASTM E3277-23a
(Test Method)Standard Test Method for Determining the Liquid or Solid State of a Material by Rheometry
Standard Test Method for Determining the Liquid or Solid State of a Material by Rheometry
SIGNIFICANCE AND USE
5.1 Shipping regulations often require the identification of a material as either a liquid or a solid. This test method may be used to make that determination for regulatory purposes. (See also Test Method D4359.)
5.2 For liquid thermosetting resin, as cure progresses, the liquid resin becomes a solid. A thermosetting resin is more easily worked or shaped while in the liquid-like form and becomes more difficult to do so as the cure advances. The point at which the solid-like character becomes dominant is called the gel point and is considered to be the end of the period where the thermosetting resin is workable. Gel point is identified as that point where tan δ = 1 as determined in Test Method D4473.
Note 1: Gel point at ambient temperature is seldom a useful parameter. Use of this test method at the more useful elevated temperatures requires capabilities readily available but outside of 7.2.6, 7.2.7, and Section 10.
5.3 This test method may be used in research, development, and for regulatory compliance.
SCOPE
1.1 Using rheometry, this test method determines, for regulatory purposes, whether a viscose viscous material is a liquid or a solid. Very small amounts of material (typically less than 3 g) may be used for this measurement.
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.
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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: E3277 − 23a
Standard Test Method for
Determining the Liquid or Solid State of a Material by
1
Rheometry
This standard is issued under the fixed designation E3277; 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* 3. Terminology
3.1 Definitions—Technical terms used in this test method
1.1 Using rheometry, this test method determines, for regu-
are defined in Terminologies D4092 and E473 including
latory purposes, whether a viscose viscous material is a liquid
dynamic mechanical analyzer, loss modulus, phase angle,
or a solid. Very small amounts of material (typically less than
rheometer, shear, storage modulus, strain, stress, and tan delta.
3 g) may be used for this measurement.
3.1.1 dissipative, adj—in dynamic mechanical analysis, the
1.2 The values stated in SI units are to be regarded as
irrecoverably loss of mechanical energy usually as heat.
standard. No other units of measurement are included in this
3.1.2 gel point, n—the stage at which a liquid begins to
standard.
exhibit pseudo-elastic properties.
1.3 This standard does not purport to address all of the
3.1.3 slip, wall, n—in rheology, the lack of adhesion be-
3
safety concerns, if any, associated with its use. It is the
tween the test specimen and the shearing surface.
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 Viscoelastic materials exhibit both solid-like and liquid-
1.4 This international standard was developed in accor-
like characteristics. The loss modulus of a material is a measure
dance with internationally recognized principles on standard-
of its liquid-like characteristic while the storage modulus of a
ization established in the Decision on Principles for the
material indicates its solid-like characteristics. When the loss
Development of International Standards, Guides and Recom-
modulus is greater than the storage modulus, a material is said
mendations issued by the World Trade Organization Technical
to be predominantly a liquid. When the storage modulus is
Barriers to Trade (TBT) Committee.
greater than the loss modulus, the material is said to be
predominantly a solid. The ratio of loss modulus to storage
2. Referenced Documents
modulus is known as tangent angle delta (tan δ).
2
4.2 Loss modulus and storage modulus of a material is
2.1 ASTM Standards:
measured using a cone-and-plate or parallel plate rheometer at
D4092 Terminology for Plastics: Dynamic Mechanical
ambient temperature conditions and tan δ is then calculated.
Properties
Materials with a tan δ greater than unity (tan δ ≥ 1.0) are
D4359 Test Method for Determining Whether a Material Is
identified as liquids. Those materials with a tan δ less than
a Liquid or a Solid
unity are identified as solids.
D4473 Test Method for Plastics: Dynamic Mechanical Prop-
erties: Cure Behavior
5. Significance and Use
E473 Terminology Relating to Thermal Analysis and Rhe-
5.1 Shipping regulations often require the identification of a
ology
material as either a liquid or a solid. This test method may be
used to make that determination for regulatory purposes. (See
also Test Method D4359.)
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.08 on Rheol-
5.2 For liquid thermosetting resin, as cure progresses, the
ogy.
liquid resin becomes a solid. A thermosetting resin is more
Current edition approved Oct. 1, 2023. Published November 2023. Originally
easily worked or shaped while in the liquid-like form and
approved in 2021. Last previous edition approved in 2023 as E3277 – 23. DOI:
becomes more difficult to do so as the cure advances. The point
10.1520/E3277-23A.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Bingham, E. C., Fluidity and Plasticity, McGraw-Hill, New York, NY, 1922, p.
the ASTM website. 231.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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E3277 − 23a
been found suita
...
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: E3277 − 23 E3277 − 23a
Standard Test Method for
Determining the Liquid or Solid State of a Material by
1
Rheometry
This standard is issued under the fixed designation E3277; 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 Using rheometry, this test method determines, for regulatory purposes, whether a viscose viscous material is a liquid or a solid.
Very small amounts of material (typical(typically less than 3 g) may be used for this measurement.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D4092 Terminology for Plastics: Dynamic Mechanical Properties
D4359 Test Method for Determining Whether a Material Is a Liquid or a Solid
D4473 Test Method for Plastics: Dynamic Mechanical Properties: Cure Behavior
E473 Terminology Relating to Thermal Analysis and Rheology
3. Terminology
3.1 Definitions—Technical terms used in this test method are defined in Terminologies D4092 and E473 including dynamic
mechanical analyzer, loss modulus, phase angle, rheometer, shear, storage modulus, strain, stress, and tan delta.
3.1.1 dissipative, adj—in dynamic mechanical analysis, the irrecoverably loss of mechanical energy usually as heat.
3.1.2 gel point, n—the stage at which a liquid begins to exhibit pseudo-elastic properties.
3
3.1.3 slip, wall, n—in rheology, the lack of adhesion between the test specimen and the shearing surface.
1
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 June 1, 2023Oct. 1, 2023. Published June 2023November 2023. Originally approved in 2021. Last previous edition approved in 20222023 as
E3277 – 22. DOI: 10.1520/E3277-23.23. DOI: 10.1520/E3277-23A.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 the ASTM website.
3
Bingham, E. C., Fluidity and Plasticity, McGraw-Hill, New York, NY, 1922, p. 231.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E3277 − 23a
4. Summary of Test Method
4.1 Viscoelastic materials exhibit both solid-like and liquid-like characteristics. The loss modulus of a material is a measure of its
liquid-like characteristic while the storage modulus of a material indicates its solid-like characteristics. When the loss modulus is
greater than the storage modulus, a material is said to be predominantly a liquid. When the storage modulus is greater than the loss
modulus, the material is said to be predominantly a solid. The ratio of loss modulus to storage modulus is known as tangent angle
delta (tan δ).
4.2 Loss modulus and storage modulus of a material is measured using a cone-and-plate or parallel plate rheometer at ambient
temperature conditions and tan δ is then calculated. Materials with a tan δ greater than unity (tan δ ≥ 1.0) are identified as liquids.
Those materials with a tan δ less than unity are identified as solids.
5. Significance and Use
5.1 Shipping regulations often require the identification of a material as either a liquid or a solid. This test method may be used
to make that determination for regulatory purposes. (See also Test Method D4359.)
5.2 For liquid thermosetting resin, as cure progresses, the liquid resin becomes a soli
...
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