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Plastics – Determination of dynamic mechanical properties – Part 1: General principles (ISO 6721­1:2019)

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100% found this document useful (1 vote)
386 views32 pages

Dineniso6721-1 2019-09 en

Plastics – Determination of dynamic mechanical properties – Part 1: General principles (ISO 6721­1:2019)

Uploaded by

Daeryun Kim
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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September 2019

DIN EN ISO 6721-1


D
ICS 83.080.01 Supersedes
DIN EN ISO 6721­1:2011­08

Plastics –
Determination of dynamic mechanical properties –
Part 1: General principles (ISO 6721­1:2019);
English version EN ISO 6721­1:2019,
English translation of DIN EN ISO 6721-1:2019-09

Kunststoffe –
Bestimmung dynamisch­mechanischer Eigenschaften –
Teil 1: Allgemeine Grundlagen (ISO 6721­1:2019);
Englische Fassung EN ISO 6721­1:2019,
Englische Übersetzung von DIN EN ISO 6721-1:2019-09
Plastiques –
Détermination des propriétés mécaniques dynamiques –
Partie 1: Principes généraux (ISO 6721­1:2019);
Version anglaise EN ISO 6721­1:2019,
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Traduction anglaise de DIN EN ISO 6721-1:2019-09

Document comprises 32 pages

Translation by DIN-Sprachendienst.
In case of doubt, the German-language original shall be considered authoritative.

© DIN Deutsches Institut für Normung e. V. (German Institute for Standardization) is the owner of all
non­exclusive rights of exploitation, irrespective of the form and procedure.
Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale.
www.din.de
www.beuth.de
!&,6Q"
09.19 3091946
DIN EN ISO 6721-1:2019-09

A comma is used as the decimal marker.

National foreword
This document (EN ISO 6721-1:2019) has been prepared by Technical Committee ISO/TC 61 “Plastics” in
collaboration with Technical Committee CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium).

The responsible German body involved in its preparation was DIN-Normenausschuss Kunststoffe
(DIN Standards Committee Plastics), Working Committee NA 054-01-03 AA “Physical, rheological and
analytical test methods”.

DIN EN ISO 6721 consists of the following parts, under the general title Plastics — Determination of dynamic
mechanical properties:

 Part 1: General principles

 Part 2: Torsion-pendulum method

 Part 3: Flexural vibration — Resonance-curve method

The DIN documents corresponding to the international documents referred to in this document are as
follows:

ISO 291 DIN EN ISO 291


ISO 293 DIN EN ISO 293
ISO 294 (all parts) DIN EN ISO 294 (all parts)
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ISO 295 DIN EN ISO 295


ISO 472 DIN EN ISO 472
ISO 2818 DIN EN ISO 2818
ISO 4593 DIN ISO 4593
ISO 6721-2 DIN EN ISO 6721-2
ISO 6721-3 DIN EN ISO 6721-3

Amendments

This standard differs from DIN EN ISO 6721-1:2011-08 as follows:

a) normative references have been updated;

b) Figure 1 has been corrected;

c) subclause 5.3 “Temperature-controlled enclosure” has been updated;

d) in subclauses 5.6 and 9.2, limits of error have been indicated in absolute and percentage values;

e) the standard has been editorially revised.

2
DIN EN ISO 6721-1:2019-09

Previous editions

DIN 53445-1: 1959-09


DlN 53445: 1965-11, 1986-08
DIN 53520: 1969-01
DIN 53440-1: 1973-04, 1984-01
DIN 53440-2: 1973-04, 1984-01
DIN 53440-3: 1973-04, 1984-01
DIN EN ISO 6721-1: 1996-12, 2003-01, 2011-08
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3
DIN EN ISO 6721-1:2019-09

National Annex NA
(informative)

Bibliography

DIN EN ISO 291, Plastics — Standard atmospheres for conditioning and testing

DIN EN ISO 293, Plastics — Compression moulding of test specimens of thermoplastic materials

DIN EN ISO 294 (all parts), Plastics — Injection moulding of test specimens of thermoplastic materials

DIN EN ISO 295, Plastics — Compression moulding of test specimens of thermosetting materials

DIN EN ISO 472, Plastics — Vocabulary

DIN EN ISO 2818, Plastics — Preparation of test specimens by machining

DIN EN ISO 6721-2, Plastics — Determination of dynamic mechanical properties — Part 2: Torsion-pendulum
method

DIN EN ISO 6721-3, Plastics — Determination of dynamic mechanical properties — Part 3: Flexural
vibration — Resonance-curve method

DIN ISO 4593, Testing of plastics films — Determination of the thickness by mechanical scanning
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4
EUROPEAN STANDARD EN ISO 6721-1
NORME EUROPÉENNE
EUROPÄISCHE NORM May 2019

ICS 83.080.01 Supersedes EN ISO 6721-1:2011

English Version

Plastics —
Determination of dynamic mechanical properties —
Part 1: General principles
(ISO 6721-1:2019)
Plastiques — Kunststoffe —
Détermination des propriétés mécaniques dynamiques — Bestimmung dynamisch-mechanischer Eigenschaften —
Partie 1: Principes généraux Teil 1: Allgemeine Grundlagen
(ISO 6721-1:2019) (ISO 6721-1:2019)

This European Standard was approved by CEN on 8 June 2018.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by
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translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION


COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 6721-1:2019 E
worldwide for CEN national Members.
DIN EN ISO 6721-1:2019-09
EN ISO 6721-1:2019 (E)

Contents
Page

European foreword....................................................................................................................................................... 3
Foreword .......................................................................................................................................................................... 4
Introduction .................................................................................................................................................................... 5
1 Scope .................................................................................................................................................................... 6
2 Normative references .................................................................................................................................... 6
3 Terms and definitions ................................................................................................................................... 7
4 Principle .......................................................................................................................................................... 14
5 Test apparatus............................................................................................................................................... 17
5.1 Type................................................................................................................................................................... 17
5.2 Mechanical, electronic and recording systems ................................................................................. 17
5.3 Temperature-controlled enclosure ....................................................................................................... 17
5.4 Gas supply ....................................................................................................................................................... 17
5.5 Temperature-measurement device ...................................................................................................... 17
5.6 Devices for measuring test specimen dimensions ........................................................................... 17
6 Test specimens .............................................................................................................................................. 17
6.1 General ............................................................................................................................................................. 17
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6.2 Shape and dimensions................................................................................................................................ 18


6.3 Preparation .................................................................................................................................................... 18
7 Number of test specimens ......................................................................................................................... 18
8 Conditioning................................................................................................................................................... 18
9 Procedure........................................................................................................................................................ 18
9.1 Test atmosphere ........................................................................................................................................... 18
9.2 Measurement of specimen cross-section ............................................................................................ 18
9.3 Mounting the test specimens ................................................................................................................... 18
9.4 Varying the temperature ........................................................................................................................... 18
9.5 Varying the frequency ................................................................................................................................ 19
9.6 Varying the dynamic-strain amplitude ................................................................................................ 19
10 Expression of results................................................................................................................................... 19
11 Precision .......................................................................................................................................................... 20
12 Test report ...................................................................................................................................................... 20
Annex A (informative) Resonance curves ........................................................................................................ 21
Annex B (informative) Deviations from linear behaviour ......................................................................... 27
Bibliography ................................................................................................................................................................. 28

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DIN EN ISO 6721-1:2019-09
EN ISO 6721-1:2019 (E)

European foreword
This document (EN ISO 6721-1:2019) has been prepared by Technical Committee ISO/TC 61 “Plastics”
in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by
NBN.

This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by November 2019, and conflicting national standards
shall be withdrawn at the latest by November 2019.

Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 6721-1:2011.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.

Endorsement notice
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The text of ISO 6721-1:2019 has been approved by CEN as EN ISO 6721-1:2019 without any
modification.

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DIN EN ISO 6721-1:2019-09
EN ISO 6721-1:2019 (E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www​.iso​
.org/iso/foreword​.html.
This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-
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chemical properties.
This fourth edition cancels and replaces the third edition (ISO 6721-1:2011), which has been technically
revised. The main changes compared to the previous edition are as follows:
— the document has been revised editorially;
— normative references have been changed to undated and added as references into Tables 4 and 5.
A list of all parts in the ISO 6721 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www​.iso​.org/members​.html.

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DIN EN ISO 6721-1:2019-09
EN ISO 6721-1:2019 (E)

Introduction
The methods specified in the first nine parts of ISO 6721 can be used for determining storage and
loss moduli of plastics over a range of temperatures or frequencies by varying the temperature of the
specimen or the frequency of oscillation. Plots of the storage or loss moduli, or both, are indicative
of viscoelastic characteristics of the specimen. Regions of rapid changes in viscoelastic properties at
particular temperatures or frequencies are normally referred to as transition regions. Furthermore,
from the temperature and frequency dependencies of the loss moduli, the damping of sound and
vibration of polymer or metal-polymer systems can be estimated.
Apparent discrepancies may arise in results obtained under different experimental conditions. Without
changing the observed data, reporting in full (as described in the various parts of ISO 6721) the
conditions under which the data were obtained will enable apparent differences observed in different
studies to be reconciled.
The definitions of complex moduli apply exactly only to sinusoidal oscillations with constant amplitude
and constant frequency during each measurement. On the other hand, measurements of small phase
angles between stress and strain involve some difficulties under these conditions. Because these
difficulties are not involved in some methods based on freely decaying vibrations and/or varying
frequency near resonance, these methods are used frequently (see ISO 6721-2 and ISO 6721-3). In these
cases, some of the equations that define the viscoelastic properties are only approximately valid.
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EN ISO 6721-1:2019 (E)

1 Scope
The various parts of ISO 6721 specify methods for the determination of the dynamic mechanical
properties of rigid plastics within the region of linear viscoelastic behaviour. This document specifies
the definitions and describes the general principles including all aspects that are common to the
individual test methods described in the subsequent parts.
Different deformation modes can produce results that are not directly comparable. For example, tensile
vibration results in a stress which is uniform across the whole thickness of the specimen, whereas
flexural measurements are influenced preferentially by the properties of the surface regions of the
specimen.
Values derived from flexural-test data will be comparable to those derived from tensile-test data only at
strain levels where the stress-strain relationship is linear and for specimens which have a homogeneous
structure.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 291, Plastics — Standard atmospheres for conditioning and testing
ISO 4593, Plastics — Film and sheeting — Determination of thickness by mechanical scanning
ISO 6721-2, Plastics — Determination of dynamic mechanical properties — Part 2: Torsion-pendulum method
ISO 6721-3, Plastics — Determination of dynamic mechanical properties — Part 3: Flexural vibration —
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Resonance-curve method
ISO 6721-4, Plastics — Determination of dynamic mechanical properties — Part 4: Tensile vibration —
Non-resonance method
ISO 6721-5, Plastics — Determination of dynamic mechanical properties — Part 5: Flexural vibration —
Non-resonance method
ISO 6721-6, Plastics — Determination of dynamic mechanical properties — Part 6: Shear vibration — Non-
resonance method
ISO 6721-7, Plastics — Determination of dynamic mechanical properties — Part 7: Torsional vibration —
Non-resonance method
ISO 6721-8, Plastics — Determination of dynamic mechanical properties — Part 8: Longitudinal and shear
vibration — Wave-propagation method
ISO 6721-9, Plastics — Determination of dynamic mechanical properties — Part 9: Tensile vibration —
Sonic-pulse propagation method

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EN ISO 6721-1:2019 (E)

ISO 6721-10, Plastics — Determination of dynamic mechanical properties — Part 10: Complex shear
viscosity using a parallel-plate oscillatory rheometer
ISO 6721-12, Plastics — Determination of dynamic mechanical properties — Part 12: Compressive
vibration — Non-resonance method

3 Terms and definitions


For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:​//www​.iso​.org/obp
— IEC Electropedia: available at http:​//www​.electropedia​.org/
NOTE Some of the terms defined here are also defined in ISO 472. The definitions given here are not strictly
identical with, but more detailed than those in ISO 472.

3.1
complex modulus
M*
ratio of dynamic stress, given by σ(t) = σA exp(i2πft) and dynamic strain, given by ε(t) = εAexp[i(2πft – δ)],
of a viscoelastic material that is subjected to a sinusoidal vibration, where σA and εA are the amplitudes of
the stress and strain cycles, f is the frequency, δ is the phase angle between stress and strain and t is time
Note 1 to entry: It is expressed in Pascals (Pa).

Note 2 to entry: The phase angle (3.5), δ, is shown in Figure 1.


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Note 3 to entry: Depending on the mode of deformation, the complex modulus might be one of several types: E∗,
G∗, K∗ or L∗ (see Table 3).

M* = M’ + i M”

where i = ( −1 )
1
2 = −1 and M’ and M” are as defined in 3.2 and 3.3 respectively.

For the relationships between the different types of complex modulus, see Table 1.

Note 4 to entry: For isotropic viscoelastic materials, only two of the elastic parameters G∗, E∗, K∗, L∗ and µ∗ are
independent (µ∗ is the complex Poisson's ratio, given by µ∗ = µ′ + iµ″).

Note 5 to entry: The most critical term containing Poisson's ratio µ is the “volume term” 1 − 2µ, which has values
between 0 and 0,4 for µ between 0,5 and 0,3. The relationships in Table 1 containing the “volume term” 1 − 2µ can
only be used if this term is known with sufficient accuracy.

It can be seen from Table 1 that the “volume term” 1 − 2µ can only be estimated with any confidence from a
knowledge of the bulk modulus K or the uniaxial-strain modulus L and either E or G. This is because K and L
measurements involve deformations when the volumetric strain component is relatively large.

Note 6 to entry: Up to now, no measurement of the dynamic mechanical bulk modulus K, and only a small number
of results relating to relaxation experiments measuring K(t), have been described in the literature.

Note 7 to entry: The uniaxial-strain modulus L is based upon a load with a high hydrostatic-stress component.
Therefore, values of L compensate for the lack of K values, and the “volume term” 1 − 2µ can be estimated with
sufficient accuracy based upon the modulus pairs (G, L) and (E, L). The pair (G, L) is preferred, because G is based
upon loads without a hydrostatic component.

Note 8 to entry: The relationships given in Table 1 are valid for the complex moduli as well as their magnitudes (3.4).

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EN ISO 6721-1:2019 (E)

Note 9 to entry: Most of the relationships for calculating the moduli given in the other parts of this International
Standard are, to some extent, approximate. They do not take into account, for example “end effects” caused by
clamping the specimens, and they include other simplifications. Using the relationships given in Table 1 therefore
often requires additional corrections to be made. These are given in the literature (see e.g. References [7] and [8]
in the Bibliography).

Note 10 to entry: For linear-viscoelastic behaviour, the complex compliance C∗ is the reciprocal of the complex
modulus M∗, i.e.

          M* = (C*)−1

Thus

C '− iC ''
M '+ iM '' =
(C ') 2 + (C '') 2
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a)   Phase shift δ/2πf between the stress σ and strain ε b)   Relationship between the storage
in a viscoelastic material subjected to sinusoidal oscil- modulus M′, the loss modulus M″, the
lation (σA and εA are the respective amplitudes, f is the phase angle δ and the magnitude [M]
frequency) of the complex modulus M*

Figure 1 — Phase angle and complex modulus

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EN ISO 6721-1:2019 (E)

Table 1 — Relationships between moduli for uniformly isotropic materials


G and µ E and µ K and µ G and E G and K E and K G and La
Poisson's ratio, E G/K E 1
µ 1 − 2µ = b 3−
G 1 + G / 3K 3K L/G −1
Shear modulus, E 3K ( 1 − 2 µ ) E
G=
2(1 + µ ) 2(1 + µ ) 3 − E / 3K

Tensile 2G(1 + μ ) 3K(1 − 2μ) 3G 3G (1 − 4G / 3L )


modulus, E =
1 + G / 3K 1−G / L
Bulk modulus,
2G (1 + µ ) E G 4G
K=c L−
3(1 − 2 µ ) 3(1 − 2 µ ) 3(3G / E − 1 ) 3

Unaxial-strain
2G (1 − µ ) E (1 − µ ) 3K ( 1 − µ ) G ( 4G / E − 1 ) 4G K ( 1 + E / 3K )
or longitudi- K+
nal-wave 1 − 2µ (1 + µ ) (1 − 2 µ ) 1+ µ 3G / E − 1 3 1 − E / 9K
modulus, L =
a See 3.1, Note 7 to entry
b See 3.1, Note 5 to entry.
c See 3.1, Note 6 to entry.

3.2
storage modulus
M′
real part of the complex modulus M∗
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Note 1 to entry: The storage modulus is expressed in pascals (Pa).

Note 2 to entry: The storage modulus M' is shown in Figure 1 b).

Note 3 to entry: It is proportional to the maximum energy stored during a loading cycle and represents the
stiffness of a viscoelastic material.

Note 4 to entry: The different types of storage modulus, corresponding to different modes of deformation, are:
E t' tensile storage modulus, E f' flexural storage modulus, G s' shear storage modulus, G to
'
torsional storage
modulus, K′ bulk storage modulus, L'c uniaxial-strain storage modulus and L'w longitudinal-wave storage
modulus.

3.3
loss modulus
M″
imaginary part of the complex modulus
Note 1 to entry: The loss modulus is expressed in pascals (Pa).

Note 2 to entry: The loss modulus M” is shown in Figure 1 b).

Note 3 to entry: It is proportional to the energy dissipated (lost) during one loading cycle. As with the storage
modulus (3.2), the mode of deformation is designated as in Table 3, e.g. E t'' is the tensile loss modulus.

3.4
magnitude of the complex modulus
[M]
root mean square value of the storage and the loss moduli as given by the formula
[M]2 = (M′)2 + (M′′)2 = (σA / εA)2

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EN ISO 6721-1:2019 (E)

where σA and εA are the amplitudes of the stress and the strain cycles, respectively
Note 1 to entry: The complex modulus is expressed in pascals (Pa).

Note 2 to entry: The relationship between the storage modulus M′, the loss modulus M″, the phase angle δ, and
the magnitude [M] of the complex modulus is shown in Figure 1 b). As with the storage modulus, the mode of
deformation is designated as in Table 3, e.g. [Et] is the magnitude of the tensile complex modulus.

3.5
phase angle
δ
phase difference between the dynamic stress and the dynamic strain in a viscoelastic material
subjected to a sinusoidal oscillation
Note 1 to entry: The phase angle is expressed in radians (rad).

Note 2 to entry: The phase angle δ is shown in Figure 1.

Note 3 to entry: As with the storage modulus (3.2), the mode of deformation is designated as in Table 3, e.g. δt is
the tensile phase angle.

3.6
loss factor
tan δ
ratio between the loss modulus and the storage modulus given by the formula
tan δ = M′′ / M′

where δ is the phase angle between the stress and the strain
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Note 1 to entry: The loss factor is expressed as a dimensionless number.

Note 2 to entry: The ratio between loss modulus M” and storage modulus M' is shown in Figure 1 b).

Note 3 to entry: The loss factor tan δ is commonly used as a measure of the damping in a viscoelastic system. As with
the storage modulus (3.2), the mode of deformation is designated as in Table 3, e.g. tan δt is the tensile loss factor.

3.7
stress-strain hysteresis loop
stress expressed as a function of the strain in a viscoelastic material subject to sinusoidal vibrations
Note 1 to entry: Provided the viscoelasticity is linear in nature, this curve is an ellipse (see Figure 2).

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Figure 2 — Dynamic stress-strain hysteresis loop for a linear-viscoelastic material subject to


sinusoidal tensile vibrations

3.8
damped vibration
time-dependent deformation or deformation rate X(t) of a viscoelastic system undergoing freely
decaying vibrations, given by the formula
X(t) = X0exp(−βt) × sin2πfdt

where

X0 is the magnitude, at zero time, of the envelope of the cycle amplitudes;

fd is the frequency of the damped system;

β is the decay constant (3.9)


Note 1 to entry: A typical curve of freely decaying damped vibrations is shown in Figure 3.

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EN ISO 6721-1:2019 (E)

Key
X is the time-dependent deformation or deformation rate
Xq is the amplitude of the qth cycle
X0 and β define the envelope of the exponential decay of the cycle amplitudes — see formula in 3.8

Figure 3 — Damped-vibration curve for a viscoelastic system undergoing freely decaying


vibrations
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3.9
decay constant
β
coefficient that determines the time-dependent attenuation of damped free vibrations, i.e. the time
dependence of the amplitude Xq of the deformation or deformation
Note 1 to entry: The decay constant is expressed in reciprocal seconds (s−1).

Note 2 to entry: The decay constant β of freely decaying damped vibrations is shown in Figure 3.

3.10
logarithmic decrement
Λ
natural logarithm of the ratio of two successive amplitudes, in the same direction, of damped free
oscillations of a viscoelastic system given by the formula
Λ = ln(Xq / Xq + 1)

where Xq and Xq + 1 are two successive amplitudes of deformation or deformation rate in the same
direction
Note 1 to entry: The logarithmic decrement is expressed as a dimensionless number.

Note 2 to entry: Successive amplitudes used for calculation of the logarithmic decrement Λ are shown in Figure 3.

Note 3 to entry: It is used as a measure of the damping in a viscoelastic system.

Note 4 to entry: Expressed in terms of the decay constant β and the frequency fd, the logarithmic decrement is
given by the following formula

Λ = β/fd

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Note 5 to entry: The loss factor tan δ is related to the logarithmic decrement by the approximate formula.

tan δ ≈ Λ/π

Note 6 to entry: Damped freely decaying vibrations are especially suitable for analysing the type of damping in
the material under test (i.e. whether the viscoelastic behaviour is linear or nonlinear) and the friction between
moving and fixed components of the apparatus (see Annex B).

3.11
resonance curve
curve representing the frequency dependence of the deformation amplitude DA or deformation-rate
amplitude RA of an inert viscoelastic system subjected to forced vibrations at constant load amplitude
LA and at frequencies close to and including resonance
Note 1 to entry: A typical resonance curve is shown in Figure 4.

Note 2 to entry: More detailed information on resonance curves is given in Annex A.


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Figure 4 — Resonance curve for a viscoelastic system subjected to forced vibrations


(Deformation-rate amplitude RA versus frequency f at constant load amplitude; logarithmic
frequency scale)

3.12
resonance frequencies
fri
frequencies of the peak amplitudes in a resonance curve
Note 1 to entry: The subscript i refers to the order of the resonance vibration.

Note 2 to entry: Resonance frequencies are expressed in hertz (Hz).

Note 3 to entry: Resonance frequencies for viscoelastic materials derived from measurements of displacement
amplitude will be slightly different from those obtained from displacement-rate measurements, the difference
being larger the greater the loss in the material (see Annex A). Storage and loss moduli are accurately related
by simple expressions to resonance frequencies obtained from displacement-rate curves. The use of resonance
frequencies based on displacement measurements leads to a small error which is only significant when the
specimen exhibits high loss. Under these conditions, resonance tests are not suitable.

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3.13
width of a resonance peak
Δf i
difference between the frequencies f 1 and f 2 of the ith-order resonance peak, where the height RAh of
the resonance curve at f 1 and f 2 is related to the peak height RAMi of the ith mode by

R Ah = 2 − 1/2 R AM = 0 , 707 R AM

Note 1 to entry: The width Δf i is expressed in hertz (Hz).

Note 2 to entry: The data used for the calculation of the width of a resonace peak Δf i are shown in Figure 4.

Note 3 to entry: It is related to the loss factor tan δ by the formula

tan δ = Δf i / fri

Note 4 to entry: If the loss factor does not vary markedly over the frequency range defined by Δf i, the formula
holds exactly when the resonance curve is based on the deformation-rate amplitude (see also Annex A).

4 Principle
A specimen of known geometry is subjected to mechanical oscillation, described by two characteristics:
the mode of vibration and the mode of deformation.
Four oscillatory modes, I to IV, are possible, depending on whether the mode of vibration is non-
resonant, natural (resonant) or near-resonant. These modes are described in Table 2.
The particular type of modulus depends upon the mode of deformation (see Table 3).
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Table 4 indicates ways in which the various types of modulus are commonly measured. Table 5 gives a
summary of the methods covered by the various parts of ISO 6721.

Table 2 — Oscillatory modes


Mode of oscillation I II III IVa
Damped, freely decay-
Forced vibration
ing amplitude
Constant Resonance Resonance
frequency frequency curve
Frequency Non-resonance Resonance (natural) Sweep, near Approximately resonant
resonance
Load amplitude One of the two Constantb Constant
Deformation constant, the other Measured Measured Excitation pulse
amplitude measured
Inertial mass None Specimen and/or additional masses, depending on frequency range
NOTE Terms written in bold type give the designation of the mode; terms in normal type provide additional
information.
a The type of torsion pendulum used shall be indicated by adding the relevant letter, A or B (see ISO 6721-2).
b The load must be in phase with the deformation rate.

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Table 3 — Type of modulus (mode of deformation)


Designation Type of modulus
Et Tensile
Ef Flexural
Gs Shear
Gto Torsion
K Bulk compression
Lc Uniaxial compression (of thin sheets)
Lw Longitudinal bulk wave

Table 4 — Commonly used test arrangements


Type of
modulus and International Typical frequency,
Test arrangement Inertial mass
mode of Standard Hz
oscillation

Inertial mem-
Gto IV ISO 6721-2 0,1 to 10
ber
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Ef III ISO 6721-3 Specimen 10 to 1 000

Ef I ISO 6721-5

None 10−3 to 100

Gto I ISO 6721-7

Key
1 clamps, pivots or supports
2 specimen
3 inertial member

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Table 4 (continued)
Type of
modulus and International Typical frequency,
Test arrangement Inertial mass
mode of Standard Hz
oscillation

ISO 6721-4,
Et I ISO 6721-9,
ISO 6721-12

ISO 6721-6, 10−3 to 100


Gs I
ISO 6721-10

Lc I — None
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Ef I — 10−3 to 10

Specimen and
Ef II — 3 to 60
arms

Key
1 clamps, pivots or supports
2 specimen
3 inertial member

Table 5 — Methods covered by the various parts of the ISO 6721 series
Mode of Type of modulus (see Table 3)
oscillation Et Ef Gs Gto K Lc Lw
(see Table 2)
I ISO 6721-4,
ISO 6721-6,
ISO 6721-9, ISO 6721-5 ISO 6721-7 ISO 6721-8
ISO 6721-10
ISO 6721-12
II
III ISO 6721-3
IV ISO 6721-2

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5 Test apparatus

5.1 Type
The apparatus used is specified in detail in the relevant part of the ISO 6721 series (see the Introduction
and Clause 4).

5.2 Mechanical, electronic and recording systems


See the relevant part of the ISO 6721 series.

5.3 Temperature-controlled enclosure


The test specimen and the clamps or supports shall be enclosed in a temperature-controlled enclosure
containing air or a suitable inert gas.
The enclosure shall be designed so that its temperature can be varied over a range sufficient for the
material under test (e.g. −100 °C to +300 °C). It is recommended that the chamber be equipped with
temperature-programming facilities.
The temperature in the enclosure shall be uniform to within ± 1 K along the length of the specimen and
measured close to its length. If the constant-temperature procedure is used (see 9.5), the temperature
shall be constant to within ± 1 K during the test. When a constant rate of increase (or decrease) in
temperature is used (see 9.4), the rate shall not be greater than 120 K/h.

5.4 Gas supply


Supply of air or a suitable inert gas for purging purposes.
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5.5 Temperature-measurement device


The device for measuring the temperature of the air surrounding the specimen shall be capable
of determining the temperature to ±0,5 °C. The use of a thermometer with a low-inertia sensor is
recommended.

5.6 Devices for measuring test specimen dimensions


For the purposes of the various parts of the ISO 6721 series, the test specimen dimensions used for
calculating moduli are measured at room temperature only. For the measurements of the temperature
dependence of moduli, therefore, the effects of thermal expansion are not taken into account.
The devices used for measuring the length, width and thickness of the specimen (in accordance with
ISO 4593) shall be capable of determining these quantities to ±0,5 % or ±0,05 mm, whichever is smaller.

6 Test specimens

6.1 General
The parameters measured by these methods are sensitive to dimensional non-uniformity of the
specimen and to differences in its physical state (e.g. degree of crystallinity, orientation or internal
stress). These factors should be considered when choosing the dimensions and tolerances, methods of
preparation and conditioning procedures for specimens of a particular material.
The specimens (homogeneous specimens, laminated bars or strips) shall have negligible shrinkage or
warpage within the temperature range of the measurements.

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6.2 Shape and dimensions


See the relevant part of the ISO 6721 series.

6.3 Preparation
For the purposes of these methods, whether carried out on starting materials or finished products,
the test specimens shall be prepared in accordance with the relevant material standard. They may be
machined (according to ISO 2818) from compression-moulded plates [according to ISO 293, ISO 295
or ISO 1268 (all parts)] or from the finished product. Alternatively, the specimens may be injection-
moulded (according to ISO 294).

7 Number of test specimens


At least three test specimens shall be used for single-point measurements, i.e. measurements at a single
temperature and frequency. If the temperature and/or the frequency is varied over a more-or-less wide
range for quality-control purposes, one specimen is sufficient. In all other cases, at least two specimens
shall be tested.

8 Conditioning
The test specimens shall be conditioned as specified in the International Standard for the material to
be tested. In the absence of this information, the most appropriate conditions from ISO 291 shall be
selected, unless otherwise agreed upon by the interested parties.

9 Procedure
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9.1 Test atmosphere


The test temperature (or the dependence of the temperature on time), the gas supply (air or inert gas) and
the relative humidity shall be chosen according to the specific type of test and the purpose of the test.

9.2 Measurement of specimen cross-section


Before the test, measure the thickness and width of each specimen to ± 0,5 % or ± 0,05 mm, whichever
is smaller, at five points along its length. All specimens with visible irregularities, e.g. sink marks, or
variations in thickness and/or width greater than 3 % of the average shall be rejected. With specimens
of non-uniform thickness, e.g. finished parts, only the loss factor can be determined.
The procedure for measuring the dimensions of specimens of other shapes shall be agreed upon by the
interested parties.

9.3 Mounting the test specimens


According to the relevant part of the ISO 6721 series.

9.4 Varying the temperature


If temperature is the independent variable, the temperature of the test specimen shall be varied
from the lowest to the highest temperature of interest while measuring the viscoelastic properties.
The frequency of vibration may be fixed (oscillation mode I), decreased naturally with increasing
temperature (oscillation modes II and IV) or swept (oscillation mode III) (see Table 2).
Tests conducted over a range of temperatures shall be performed at incremental temperature steps
or at a rate of change of temperature slow enough to allow temperature equilibrium to be reached
throughout the entire specimen. The time to reach equilibrium will depend on the mass of the particular

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specimen and the apparatus being used. Temperature rates of 1 °C/min to 2 °C/min or 2 °C to 5 °C step
intervals held for 3 min to 5 min have been found suitable. For oscillation mode III, step intervals of
10 min are recommended.
The dynamic moduli of polymers are influenced in general by the state of physical ageing of the
specimen at the time of measurement. The age state depends upon the thermal history of the specimen
and changes with time at temperatures below the temperature θα corresponding to the centre of the
α-relaxation region. The α-relaxation is the highest-temperature mechanical relaxation mechanism and
in amorphous polymers is assigned to the glass to rubber transition. Changes in the physical age state
influence the molecular mobility and hence the response of the polymer to a time-dependent load or
deformation.
When measurements are made with increasing temperature, changes in age state will begin to occur
within the time scale of the test as the temperature approaches θα. Subsequent cooling will in general
establish a different state of physical ageing, and further measurements of dynamic properties will not
reproduce previous values. Meaningful measurements of high accuracy will therefore require a record of
the thermal history of the specimen and the heating rate if tests at elevated temperatures are carried out.

9.5 Varying the frequency


If vibrational frequency is the independent variable, the test temperature shall be fixed at the desired
temperature. The vibrational frequency of the specimen shall be varied while measuring the viscoelastic
properties.

9.6 Varying the dynamic-strain amplitude


If the test method allows measurements to be made over a range of strain amplitudes, it is good practice
to present results for the variation of storage modulus with dynamic-strain amplitude εA to reveal the
strain limit for linear viscoelastic behaviour. Measurements should start with the lowest strain for
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which accurate measurements are possible and proceed to higher strain values. These measurements
should be made at a low frequency, preferably around 1 Hz.
NOTE Under dynamic loading, the temperature of viscoelastic materials can increase significantly owing
to the dissipation of mechanical energy in the specimen as heat. If the temperature rise is significant, properties
will change with time under load. The temperature rise increases with the loss modulus of the material, the
dynamic-strain amplitude and the frequency. If the data-processing electronics is capable of analysing results
within the first few cycles, the influence of any temperature rise will be minimized. Subsequent measurements
will then change with time as the specimen temperature continues to rise, and such observations will indicate
the need to exercise some caution in the interpretation and presentation of the results.

10 Expression of results
Prepare a table of results, using the designation of the moduli as indicated in Table 3 for the relevant
deformation mode, plus the designation of the type of oscillation as in Table 2, e.g.

E f'' (III) — Flexural loss modulus measured using resonance curves

Average values and, if requested and possible, standard deviations for the storage modulus and the loss
modulus shall be reported to two significant figures.
If the test method allows measurements to be made over a range of strain amplitude, present results of
storage modulus plotted against strain amplitude.
Also prepare plots of the storage modulus and loss modulus versus temperature at different frequencies
or plots of the storage modulus and loss modulus versus frequency at different temperatures, using
logarithmic scales for the modulus and frequency axes.
For further details, see the relevant part of the ISO 6721 series.

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11 Precision
See the relevant part of the ISO 6721 series.

12 Test report
The test report shall include the following information:
a) a reference to the relevant part of the ISO 6721 series;
b) all details necessary for complete identification of the material tested, including type, source,
manufacturer's code number, form and previous history where these are known;
c) for sheets, the thickness of the sheet and, if applicable, the direction of the major axes of the
specimens in relation to some feature of the sheet;
d) the date of the test;
e) the shape and dimensions of the specimens;
f) the method of preparing the specimens;
g) details of the conditioning of the specimens;
h) the number of specimens tested;
i) details of the test atmosphere if other than air;
j) a description of the apparatus used for the test;
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k) the temperature programme used for the test, including the initial and final temperatures as well
as the rate of linear change in temperature or the size and duration of the temperature steps;
l) the table of data prepared as specified in Clause 10;
m) the modulus versus temperature or modulus versus frequency plots prepared as specified in
Clause 10;
n) where possible, a plot of storage modulus against dynamic-strain amplitude at a single frequency
as specified in Clause 10.

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Annex A
(informative)

Resonance curves

A.1 If a mechanically inert viscoelastic system is subjected to a vibrational force with varying frequency
and constant amplitude, it shows single- or multiple-resonance behaviour. This can be described in terms
of the deformation amplitude DA or deformation-rate amplitude RA of the system.

A.2 In vibration tests, resonance behaviour is usually presented as plots of the deformation amplitude
DA of the system versus the frequency f. The characteristics of this type of resonance DA(f) are as given in
A.2.1 to A.2.4.

A.2.1 For a single vibrational order at low frequencies, DA tends to a limiting “static” amplitude DA0
(f = 0) and, at high frequencies, to a limiting slope of −2 (−40 dB/decade) when plotted using the same
logarithmic scale along both axes (see Figure A.1).
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Key
DA deformation amplitude DA0 limiting static amplitude
RA deformation-rate amplitude DAM resonance deformation amplitude
f frequency RAM resonance deformation-rate amplitude
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1 deformation amplitude DA versus frequency f fRD deformation peak amplitude


2 deformation-rate amplitude RA versus frequency f frR deformation-rate peak amplitude
a Slope = 1. fn natural frequency (peak frequency without
b Slope = −2. damping, at tan δ = 0)
c Slope = −1.

NOTE Deformation amplitude and deformation-rate amplitudes plotted for the first vibrational order
assuming a loss factor tan δ of 0,6.

Figure A.1 — Resonance curves

A.2.2 The resonance frequency fRD at the peak amplitude DAM differs from the natural frequency fn
(of the same system but without damping). This last parameter, however, determines the value of the
storage component M′ of the complex modulus. M′ can therefore only be calculated approximately from
DA(f) curves.

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A.2.3 Within a series of vibrational orders i, the resonance amplitudes DAMi decrease markedly,
approximately in proportion to (fRi)−2 (see Figure A.2).
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Key
  single orders i = 1, 2, 3, ..
  sum of the single orders (multiple-resonance curve)
fn1   natural frequency for first-order oscillations
DA   deformation amplitude
DAi   deformation amplitude of ith oscillational order
a   Slope = −2.

Figure A.2 — Resonance curves plotted for the deformation amplitudes DA of oscillational order
i = 1, 2, 3 for a flexurally vibrating specimen with both ends free and for tan δ = 0,1

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A.2.4 A complex expression exists for the frequency width Δf (see 3.13) of the DA(f) resonance curve,
from which the loss factor tan δ can only be estimated approximately (see Table A.1).

Table A.1 — Formulae involving deformation resonance DA( f ) and deformation-rate resonance
RA( f ) (single vibrational order)
Deformation-rate amplitude
Deformation amplitude DA
RA
Reso-
( )
2
nance-curve  D AM 
2 1 − x 2 / tan 2δ + x 2 2
 R AM 
( )
2
−1
formula, where   =   =1+ x + x / tan 2δ
x = f/fn  DA  1
1 − tan 2δ R
 A 
4
Natural −1/2
frequency,  1 
f n = f RD  1 − tan 2δ  f n = f rR
where M′ ∝ f n2  2 
Width Δf and
Δf 2, where a
( )
1/2 1/2
∆f 2
( )
is the relative 1/2  1   1  1/2
= tanδ × a 2 − 1 ×  1 + tan 2δ  ×  1 − tan 2δ  ∆f / f n = tanδ × a 2 − 1
decrease in 2( f RD )
2  4   2 
amplitude (at-
tenuation)a
a The recommended value of a is 2 (≈3 dB), i.e. (a2 − 1)1/2 = 1. In this case, Δf is commonly referred to as the half-width.

A.3 Resonance curves may also be presented as deformation-rate amplitude RA(f) plots. Compared
with the DA(f) plot described above, this type shows many advantages, given in A.3.1 to A.3.4.
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A.3.1 For a single vibrational order, when plotted using the same logarithmic scale along both axes, the
RA(f) resonance curve is symmetrical in shape and approaches slopes of +1 and −1 (±20 dB/decade) at
low and high frequencies.

A.3.2 The resonance frequency frR at the peak amplitude RAM coincides with the natural frequency
fn. This gives an exact formula for the storage component M′ of the complex modulus (see Note 3 to
definition 3.12).

A.3.3 Within a series of vibrational orders, the resonance amplitude RAMi decreases in proportion
to (fni)−1 only. This gives a considerably wider range of vibrational orders (see Figure A.3) and better
resolution at the higher orders (i > 1) for highly damping materials (see Figure A.4).

A.3.4 The simple relationship between the frequency width Δf and the loss factor holds exactly
(see Table A.1 and 3.13).

A.4 For most types of measuring apparatus, deformation-rate amplitudes are recorded, as they
operate with induction-type vibration detectors. (With a carrier-frequency system, deformation
amplitudes are measured.)

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A.5 As can be seen from the formulae given in Table A.1, the differences betwen the relations for
deformation-type or resonance curves and those for deformation-rate-type resonance curves can be
neglected at loss factors ≤ 0,1.
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Key
RA deformation-rate amplitude
a Slope = −1.

Figure A.3 — Resonance curves as in Figure A.2 but plotted as a function


of the deformation-rate amplitude, RA

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Key
DA deformation amplitude
RA deformation-rate amplitude
fn1 natural frequency for first-order oscillations
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Figure A.4 — Multiple-resonance curves as in Figures A.2 and A.3 with tan δ = 0,6

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Annex B
(informative)

Deviations from linear behaviour

Figure B.1 shows semi-logarithmic plots of freely decaying amplitude Xq versus time t. This type of plot
provides a good test of linearity of damping properties. Initial amplitudes beyond the range of linear
behaviour of the material under test generally show over-exponential decay (crosses in Figure B.1).
Similar behaviour is observed if the damping of the specimen is extremely low and damping of the
oscillating system by the ambient air becomes significant. The points indicated by triangles, however,
give a curve with the opposite curvature which tends to a linear amplitude versus time plot instead
of an exponential one. This type of plot indicates friction between the moving and fixed parts of
the apparatus. Both types of deviation from linear viscoelastic behaviour can only be detected by
measurements of freely decaying vibrations. With forced vibrations, only extremely faint non-harmonic
deformations are generated.
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Key
Xq logarithm of freely decaying amplitude
t time
1 linear viscoelastic behaviour with exponential decay
2 nonlinear viscoelastic behaviour (initial over-exponential decay)
3 friction between moving and fixed parts — linear decay

Figure B.1 — Logarithm of freely decaying amplitude, Xq, versus time, t

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Bibliography

[1] ISO 472, Plastics — Vocabulary


[2] ISO 293, Plastics — Compression moulding of test specimens of thermoplastic materials
[3] ISO 294 (all parts), Plastics — Injection moulding of test specimens of thermoplastic materials
[4] ISO 295, Plastics — Compression moulding of test specimens of thermosetting materials
[5] ISO 1268 (all parts), Fibre-reinforced plastics — Methods of producing test plates
[6] ISO 2818, Plastics — Preparation of test specimens by machining
[7] Nederveen C.J., & Van Der Wal C.W. Rheol. Acta, 6 (4), p. 316 (1967)
[8] Read B.E., & Dean G.D. The Determination of Dynamic Properties of Polymers and Composites,
Adam Hilger, Bristol, 1978
[9] Gradin P., Howgate P.G., Selden R. in Comprehensive Polymer Science, Vol. 2, C. Booth and C.
Price, Eds
[10] McCrum N.G., Read B.E., Williams G. Anelastic and Dielectric Effects in Polymer Solids, Wiley
and Sons, London, 1967
[11] Nielsen L.E. Mechanical Properties of Polymers and Composites, Marcel Dekker, New York, 1974
[12] Ward I.M., & Sweeney J. Mechanical Properties of Solid Polymers, Third Edition, John Wiley &
Sons, 2013
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