ASTM E3277-21

Standard Test Method for Determining Whether a Material is a Liquid or a Solid 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.  
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 (typical 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.

General Information

• Status: Historical
• Publication Date: 28-Feb-2021
• ICS: 17.060 - Measurement of volume, mass, density, viscosity
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.08 - Rheology

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E3277 − 21
Standard Test Method for
Determining Whether a Material is a Liquid or a Solid 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 shear, storage modulus, strain, stress, and tan delta.
3.1.1 dissipative, adj—in dynamic mechanical analysis, the
1.1 Using rheometry, this test method determines, for regu-
irrecoverably loss of mechanical energy usually as heat.
latory purposes, whether a viscose viscous material is a liquid
3.1.2 gel point, n—the stage at which a liquid begins to
or a solid. Very small amounts of material (typical less than
exhibit pseudo-elastic properties.
3 g) may be used for this measurement.
1.2 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard. No other units of measurement are included in this
4.1 Viscoelastic materials exhibit both solid-like and liquid-
standard.
likecharacteristics.Thelossmodulusofamaterialisameasure
1.3 This standard does not purport to address all of the
of its liquid-like characteristic while the storage modulus of a
safety concerns, if any, associated with its use. It is the
material indicates its solid-like characteristics. When the loss
responsibility of the user of this standard to establish appro-
modulus is greater than the storage modulus, a material is said
priate safety, health, and environmental practices and deter-
to be predominantly a liquid. When the storage modulus is
mine the applicability of regulatory limitations prior to use.
greater than the loss modulus, the material is said to be
1.4 This international standard was developed in accor-
predominantly a solid. The ratio of loss modulus to storage
dance with internationally recognized principles on standard-
modulus is known as tangent angle delta (tan δ).
ization established in the Decision on Principles for the
4.2 Loss modulus and storage modulus of a material is
Development of International Standards, Guides and Recom-
measured using a cone-and-plate or parallel plate rheometer at
mendations issued by the World Trade Organization Technical
ambient temperature conditions and tan δ is then calculated.
Barriers to Trade (TBT) Committee.
Materials with a tan δ greater than unity (tanδ≥ 1.0) are
identified as liquids. Those materials with a tan δ less than
2. Referenced Documents
unity are identified as solids.
2
2.1 ASTM Standards:
D4092 Terminology for Plastics: Dynamic Mechanical 5. Significance and Use
Properties
5.1 Shipping regulations often require the identification of a
D4473 Test Method for Plastics: Dynamic Mechanical Prop-
material as either a liquid or a solid. This test method may be
erties: Cure Behavior
used to make that determination for regulatory purposes.
E473 Terminology Relating to Thermal Analysis and Rhe-
5.2 For liquid thermosetting resin, as cure progresses, the
ology
liquid resin becomes a solid. A thermosetting resin is more
3. Terminology easily worked or shaped while in the liquid-like form and
becomes more difficult to do so as the cure advances.The point
3.1 Definitions—Technical terms used in this standard are
at which the solid-like character becomes dominant is called
defined in Terminologies D4092 and E473 including dynamic
the gel point and is considered to be the end of the period
mechanical analyzer, loss modulus, phase angle, rheometer,
where the thermosetting resin is workable. Gel point is
identified as that point where tan δ = 1 as determined in Test
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal
Method D4473.
Measurements and is the direct responsibility of Subcommittee E37.08 on Rheol-
ogy. NOTE 1—Gel point at ambient temperature is seldom a useful param-
Current edition approved March 1, 2021. Published April 2021. DOI: 10.1520/ eter. Use of this test method at the more useful elevated temperatures
E3277-21.
requires capabilities readily available but outside of 7.2.6, 7.2.7, and
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Section 10.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.3 This test method may be used in research, development,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. and for regulatory compliance.
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E3277 − 21
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