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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.

A Designation: E473 - 23
�u 117
INTERNATIONAL

Standard Terminology Relating to


Thermal Analysis and Rheology 1

This standard is issued under the fixed designation E473; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope ture Measurement Validation of Thermogravimetric Ana­


1.1 This terminology is a compilation of definitions of terms lyzers
used in ASTM documents relating to thermal analysis and E2918 Test Method for Performance Validation of Thermo-
rheology. This terminology includes only those terms for which mechanical Analyzers
ASTM either has standards or is contemplating some action. It 3. Terminology
is not intended to be an all-inclusive listing of terms related to
adiabatic, adj - no heat exchange with the surroundings.
thermal analysis and rheology.
1.2 This terminology specifically supports the single-word bifilar, adj-involving a thread or wire doubled back upon
form for terms using thermo as a prefix, such as thermoana­ itself.
lytical or thermomagnetometry, while recognizing that for calorimeter, n-apparatus for measuring quantities of ab­
some terms a two-word form can be used, such as thermal sorbed or evolved heat.
analysis. This terminology does not support, nor does it
recommend, use of the grammatically incorrect, single-word combined, adj - the application of two or more techniques to
form using thermal as a prefix, such as, thermalanalytical or different samples at the same time.
thermalmagnetometry. controlled-rate thermal analysis (CRTA), n-a family of
1.3 A definition is a single sentence with additional infor­ techniques that monitors the temperature versus time profile
mation included in a Discussion area. It is reviewed every five needed to maintain a chosen, fixed rate of change of a
years. property of a substance.
D1scuss10N-Compared to controlled-temperature experiments,
1.4 This international standard was developed in accor­
where the reaction rate tends to increase exponentially and the rate can
dance with internationally recognized principles on standard­
become limited by heat or mass transfer, CRTA experiments are more
ization established in the Decision on Principles for the likely to involve the chemical reaction as the limiting step. This
Development of International Standards, Guides and Recom­ technique can also improve the resolution of multiple reactions. For
mendations issued by the World Trade Organization Technical example, in controlled rate experiments, power to the furnace is

Barriers to Trade (TBT) Committee. controlled to ensure a fixed rate of mass loss (or gain).

controlled-temperature program, n-the temperature history


2. Referenced Documents
experienced by a sample during the course of a thermal
2.1 ASTM Standards:2 analysis experiment.
E1142 Terminology Relating to Thermophysical Properties D1scuss10N-ln contrast to controlled-rate experiments, power to the
E2161 Terminology Relating to Performance Validation in furnace is controlled to ensure a fixed rate of temperature change for

Thermal Analysis and Rheology controlled-temperature experiments. The program may include heating
or cooling segments in which the temperature is changed at a fixed rate,
E2253 Test Method for Temperature and Enthalpy Measure­
isothermal segments in which time becomes the explicit independent
ment Validation of Differential Scanning Calorimeters
variable, or any sequence of these individual segments. If the atmo­
E2402 Test Method for Mass Loss, Residue, and Tempera- sphere (or vacuum) around the sample is changed by some external
action (depending on the independent variable only-temperature or
time) during the course of the experiment, that too becomes part of the
1 This terminology is under the jurisdiction of ASTM Committee E37 on controlled-temperature program.
Thermal Measurements and are the direct responsibility of Subcommittee E37.03 on
Nomenclature and Definitions. curve, thermal, n-the plot or display of a dependent param­
Current edition approved July 15, 2023. Published July 2023. Originally eter against an independent parameter such as temperature or
approved in 1973. Last previous edition approved in 2022 as E473 - 22d. DOI:
time.
I0.1520/E0473-23.
D1scuss10N-ln thermal analysis, the term thermogram is inappro­
2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM priately used as a synonym for thermal curve. Its use is deprecated to
Standards volume information, refer to the standard's Document Summary page on avoid confusion with a visual image that maps the temperature pattern
the ASTM website. of an object.

Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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derivative, adj-pertaining to the first derivative (mathemati­ evolved gas analysis (EGA), n-a technique in which the
cal) of any curve with respect to temperature or time. nature or amount, or both, of gas or vapor evolved by a
substance is subjected to a controlled-temperature program.
dielectric analysis (DEA), n-a technique in which the dielec­
D1scuss10N-Some specific forms of EGA have become established
tric constant (permittivity or capacitance) and dielectric loss for investigating different aspects of catalysis, such as reduction,
(conductance) of a substance under oscillating electric field oxidation, or desorption. In this context, EGA in a hydrogen atmo­
are measured as a function of temperature or time while the sphere is known as temperature-programmed reduction (TPR); EGA in
substance is subjected to a controlled-temperature program an oxygen atmosphere is temperature-programmed oxidation (TPO);

in a specified atmosphere. and EGA in the absence of decomposition, in an inert atmosphere or


vacuum, is temperature-programmed desorption (TPD). For each
differential, adj-pertaining to a difference in measured or technique the method used for gas identification and quantification

measurable quantities usually between a substance and some should always be clearly stated.

reference or standard material.


exotherm, n-in thermal analysis, the thermal record of a
differential scanning calorimetry (DSC), n- a technique in transition or reaction where heat is released by a material or
which the heat flow difference into a substance and a reaction.
reference material is measured as a function of temperature
extrapolated onset value, n-the value of the independent
while the substance and reference material are subjected to a
parameter found by extrapolating the dependent parameter
controlled-temperature program.
baseline prior to the event and a tangent constructed at the
D1scuss10N-The record is the differential scanning calorimetric or
DSC curve. Two modes, power compensation differential scanning
inflection point on the leading edge to their intersection.
calorimetry, and heat flux differential scanning calorimetry can be
first-deviation-from-baseline (FDFB), n-on a thermal curve,
distinguished, depending on the method of measurement used.
the point that is first observed to depart from the baseline
D1scuss10N-Two conventions exist in thermal analysis. In the before a transition.
physicist's convention, exothermic behavior increases downward on
D1scuss10N-The first-deviation-from-baseline is often determined
the thermal curve. In the chemist's convention, exothermic behavior
E37 takes no
as the first point that differs from the baseline by more than the
increases upward on the thermal curve. Committee
detection limit at the onset to a sustainable change from one state to
E2161 and Test Methods E2253, E2402, and
position on which convention shall be used. To aid the user, the
another (see Terminology
direction of exothermic (or conversely, endothermic) behavior shall be
E2918).
indicated on each thermal curve.

D1scuss10N-Transition onset is a synonym. The transition onset is


differential thermal analysis (DTA), n-a technique in which
differentiated from the extrapolated onset.
the temperature difference between the substance and a
reference material is measured as a function of temperature, guard heater/cooler, thermal, n-a heated or cooled barrier
while the substance and reference material are subjected to a that surrounds internal components to limit heat flow be­
controlled-temperature program. tween the internal components and the surroundings.
D1scuss10N-The term quantitative differential thermal analysis
covers those uses of DTA where the equipment is designed to produce high-pressure (HP...) , adj-a prefix for different thermoana­
quantitative results. lytical techniques in which the pressure in the apparatus is
above ambient.
dilatometry, n-see thermodilatometry.
D1scuss10N-As an example, high-pressure thermogravimetric analy­
dynamic mechanical analysis (DMA), n-a technique in
sis is designated HPTGA.
which the storage modulus (elastic response) and loss
modulus (viscous response) of a substance under oscillatory isothermal, adj-at constant temperature.
load is measured as a function of temperature, time, or
frequency of oscillation, while the substance is subjected to modulated temperature, adj-a prefix applied to the tech­

a controlled-temperature program in a specified atmosphere. nique named to indicate that temperature modulation has
been applied to the temperature program.
electrobalance, n- an analytical balance where the specimen D1scuss10N-As an example, a DSC experiment carried out with a
weight is balanced by the torque produced by a current in a modulated temperature program would be Modulated Temperature
coil in a magnetic field (that is, a torque motor) with the Differential Scanning Calorimetry (MTDSC).

torque proportional to the current.


D1scuss10N-Other modulated techniques are possible, such as

endotherm, n-in thermal analysis, the thermal record of a modulated force TMA.

transition where heat is absorbed by the specimen. D1scuss10N-The use of the prefix MT is preferred to TM.

enthalpic relaxation, n-the process of reaching equilibrium


nonreversing, adj-in modulated temperature experiments,
after aging, accompanied by absorption or release of energy.
responding to the value of the temperature or time, or both.
D1scuss10N-The enthalpic relaxation is often observed, upon
heating, as an exothermic peak following the onset of a glass transition offset, temperature, n-in thermal analysis, the difference
or an endothermic peak after the midpoint.
between the measured specimen temperature and the actual
D1scuss10N-Synonyms for enthalpic relaxation include enthalpic specimen temperature arising from the temperature sensor
overshoot, enthalpy, or enthalpic release. being in fixed proximity, but external, to the specimen.

2
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� E473 - 23
onset point (temperature or time), n-the temperature or temperature or time while the substance is subjected to a
time at which a deflection is first observed from the controlled-temperature program.
established baseline prior to the thermal event.
thermal lag, T, n-the change in indicated temperature (f,.D
peak, n-that portion of a thermal curve characterized by a with a change in heating or cooling rate (!}.�).
deviation from the established baseline, a maximum depen­ DISCUSSION-Thermal lag ('r) is given by 1 =ti.Till.�.
dent parameter deflection, and a reestablishment of a base­
thermoanalytical, adj-of, or pertaining to, thermal analysis.
line not necessarily identical to that before the peak.

peak value, n-the value of the independent parameter corre­ thermodilatometry, n-a technique in which a dimension of a

sponding to the maximum (or minimum) deflection from the substance under negligible load is measured as a function of
baseline of the dependent parameter curve. temperature while the substance is subjected to a controlled­
temperature program in a specified atmosphere.
plateau, n- a region of little or no change in a graphical D1scuss10N-Linear thermodilatometry and volume thermodilatom­
representation. etry are distinguished on the basis of the dimension measured.

pulse, n-a transient step-hold-return variation of a parameter thermogravimetric analysis (TGA), n-a technique in which
that is normally constant where the intensity and duration are the mass of a substance is measured as a function of
specified. temperature or time while the substance is subjected to a
rate constant, k, n-in chemistry, a coefficient of proportion­
controlled-temperature program in a specified atmosphere.
D1scuss10N-The record is the thermogravimetric or TG curve.
ality relating to the rate of a chemical reaction at a given
temperature to the concentration of the reactant, for a thermogravimetry (TG), n-see thermogravimetric analy­
unimolecular reaction, or to the product of the concentra­ sis.
tions of reactants for a multimolecular reaction. thermomagnetometry, n-a family of thermoanalytical tech­

reversing, adj-in modulated temperature experiments, re­


niques in which a magnetic characteristic of a substance is
sponding to the rate of change of the temperature. measured as a function of temperature or time while the
substance is subjected to a controlled-temperature program
rheometer, n-an instrument for measuring rheological prop­ in a specified atmosphere.
erties with a controlled temperature, shear rate, or stress D1scuss10N-Thermogravimetric analysis with a magnetic field act­
program. ing on the specimen is the most common example.

rheometry, n-a technique in which viscosity, storage thermomechanical analysis (TMA), n-a technique in which
modulus, and loss modulus of a material are measured as a the deformation of a substance under nonoscillatory load is
function of temperature, time, shear rate, or stress while the measured as a function of temperature or time while the
material is subjected to controlled temperature, shear rate, or substance is subjected to a controlled-temperature program
stress program. in a specified atmosphere.
D1scuss10N-The load on the substance may be compressive, tensile,
shear, n--deformation when parallel planes of a material move
flexural, or torsional. When the applied load is too low to cause
parallel to each other. deformation, TMA measures a dimension of the substance and in this
thermodilatometry.
shear rate, y, n-time rate of change of shear strain.
mode is called

valley, n-a region of minimum values in a graphical repre­


shear stress,T, n-force per unit area in shear.
sentation bordered by higher values.
simultaneous, adj-the application of two or more techniques
to the same sample at the same time. viscometer, n-an instrument for measuring viscosity at fixed
D1scuss10N-A hyphen is used to separate the abbreviations of the temperature, shear rate, or stress.
techniques; for example, simultaneous thermogravimetric analysis and
differential scanning calorimetry would be TGA-DSC.
viscometry, n-a technique in which viscosity of a material is
measured at fixed temperature, shear rate, or stress.
stochastic, adj-random.
viscosity, rotational, n-a measure of viscosity (see Terminol­
tan () , n-is the dimensionless ratio of energy lost to energy ogy E1142) in which a rotational element (spindle) is
returned during one cycle of a periodic process. Tan 8 is unidirectionally rotated in a measured fluid.
normally calculated by dividing the loss component of the D1scuss10N-Brookfield viscosity is an obsolete and deprecated
property measured by a periodic method by the storage synonym for rotational viscosity.
component (for example, tan 8 E;E' as used in DMA). =

4. Keywords
thermal analysis (TA), n-a group of techniques in which a
physical property of a substance is measured as a function of 4.1 definitions; rheology; terminology; thermal analysis

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� E473 - 23
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