This document specifies a method for the separation of overlapping thermal transitions of plastics related to reversing and non-reversing heat flow rate, using temperature modulated differential scanning calorimetry.

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This document specifies a bending-vibration method based upon resonance curves for determining the flexural complex modulus E*f of homogeneous plastics and the damping properties of laminated plastics intended for acoustic insulation, for example systems consisting of a metal sheet coated with a damping plastic layer, or sandwich systems consisting of two sheet-metal layers with an intermediate plastic layer. For many purposes, it is useful to determine these properties as a function of temperature and frequency.

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This document specifies the characteristics of non-adiabatic fast differential scanning calorimeters, also covered by the general abbreviation FSC having an open specimen geometry in which specimens are placed directly onto active measurement areas of chip sensors based on Micro-Electro-Mechanical Systems (MEMS) membrane technology, without encapsulation in closed crucibles and ovens. Due to the open specimen geometry, this document is applicable to very small specimens having masses of not greater than 1 µg only. The occurrence of high temperature gradients during measurements can be prevented by keeping specimen thicknesses as small as possible. The use of very low specimen masses enables achievement of very high scanning rates in the order of several thousand K/s, both in heating and cooling mode whereby lower specimen masses and thicknesses allow higher heating and cooling rates. Typically, low scanning rates of FSC overlap with high scanning rates of conventional DSC covered by ISO 11357‑1, thus enabling connection to conventional DSC results. NOTE 1 Due to the sensor layout FSC is also called chip calorimetry. NOTE 2 FSC stands for Fast Scanning Calorimetry but also for Fast Scanning Calorimeter. In practice from the context the choice can be made quite easily. FSC is suitable for thermal analysis of fast kinetic effects of polymers, polymer blends and composites, such as: — thermoplastics (polymers, moulding compounds and other moulding materials, with or without fillers, fibres or reinforcements); — thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements); — elastomers (with or without fillers, fibres or reinforcements). This document specifies methods for qualitative and quantitative analysis of fast physical and chemical processes showing changes in heat flow rate. This includes measurement of characteristic temperatures as well as caloric values of both, solid and liquid materials. This document is particularly applicable for the observation of fast kinetics of thermal effects such as: — physical transitions (glass transition, phase transitions such as melting and crystallization, polymorphic transitions, etc.); — metastability and related processes like reorganization, (re)crystallization, annealing, ageing, amorphization; — chemical reactions (hydration, oxidation, polymerisation, crosslinking and curing of elastomers and thermosets, decomposition, etc.); — isothermal measurements of fast crystallising systems or chemical reactions. It is also applicable for the determination of heat capacity and related changes of thermodynamic functions. FSC provides a technique to analyse material behaviour at similarly high heating or cooling rates used in industrial polymer processing. FSC can also enable separation of overlapping thermal effects with different kinetics such as: — melting and decomposition: higher heating rates can shift decomposition to higher temperatures and allow unperturbed measurement of melting; — glass transition and cold crystallisation of polymers: higher heating rates can suppress cold crystallisation resulting in unperturbed measurement of glass transition as a function of cooling / heating rates; — reorganisation of amorphous or semi-crystalline polymers upon cooling and heating: depending on the cooling rate used specimens with different crystallinities can be generated and their reorganisation upon heating analysed using different scanning rates. This document establishes general aspects of FSC, such as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test report.

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This document establishes a method for determination of the thermal conductivity of solid unfilled and filled or fibre reinforced plastics and composites by means of differential scanning calorimetry (DSC). It is applicable for materials with thermal conductivities of up to 1 W/(m⋅K).

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This document specifies methods for determining the specific heat capacity of plastics by differential scanning calorimetry.

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This document specifies an analysis method for determining the activation energy using the Ozawa-Friedman plot. It also specifies the preparation of master plots for verification of the reaction kinetics determined by thermogravimetry.

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This document specifies a method for the determination of the activation energy, Ea, in the Arrhenius formula for the decomposition of polymers using a thermogravimetric technique. The method is applicable only if the reaction proceeds by a single mechanism. It is applicable to multistage reactions if they consist of clearly separated single-stage steps.

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This document establishes a method for measurement of specific heat capacity, cp, using temperature modulated differential scanning calorimetry.

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This document specifies methods for the determination of the glass transition temperature and the step height related to the glass transition of amorphous and partially crystalline plastics.

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This document specifies methods for determining a value of the glass transition temperature (Tg) from the dynamic mechanical properties measured during a linear temperature scan under heating conditions. The glass transition temperature is an indicator of the transition from a hard and relatively brittle glassy state to a rubbery or viscous liquid state in an amorphous polymer or in amorphous regions of a partially crystalline polymer. Usually referred to as dynamic mechanical analysis (DMA), the methods and their associated procedures can be applied to unreinforced and filled polymers, foams, rubbers, adhesives and fibre-reinforced plastics/composites. The methods are limited to materials that are inherently stable above Tg, i.e. amorphous materials that transform into a rubbery state or partially crystalline materials that keep their shape due to crystallinity. Different modes (e.g. flexure, torsion, shear, compression, tension) of dynamic mechanical analysis can be applied, as appropriate, to the form of the source material. Measured Tg values using instrumentation can vary as a result of material characteristics and/or the test set-up. The temperature sensor in a DMA instrument is not in contact with the test specimen and therefore measures temperature of the environment surrounding the specimen under test. The resulting data can vary with the heating rate applied. A procedure is included to take into account the thermal lag influencing the measured data.

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This document describes a forced, non-resonance method for determining the components of the tensile complex modulus E* of polymers at frequencies typically in the range 0,01 Hz to 100 Hz. NOTE Higher frequency measurements can be made, but significant errors in the dynamic properties measured are likely to result (see 10.2.2 and 10.2.3). The method is suitable for measuring dynamic storage moduli in the range 0,01 GPa to 5 GPa. Although materials with moduli outside this range can be studied, alternative modes of deformation are intended to be used for higher accuracy [i.e. a shear mode for G′ 5 GPa (see ISO 6721-3 or ISO 6721-5)]. This method is particularly suited to the measurement of loss factors and can therefore be conveniently used to study the variation of dynamic properties with temperature and frequency through most of the glass-rubber relaxation region (see ISO 6721-1). The availability of data determined over wide ranges of both frequency and temperature enables master plots to be derived, using frequency-temperature shift procedures, which display dynamic properties over an extended frequency range at different temperatures.

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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.

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This document specifies two methods (A and B) for determining the linear dynamic mechanical properties of plastics, i.e. the storage and loss components of the torsional modulus, as a function of temperature, for small deformations within the frequency range from 0,1 Hz to 10 Hz. NOTE The temperature dependence of these properties, measured over a sufficiently broad range of temperatures (for example from −50 °C to +150 °C for most commercially available plastics), gives information on the transition regions (for example the glass transition and the melting transition) of the polymer. It also provides information concerning the onset of plastic flow. The two methods described are not applicable to non-symmetrical laminates (see ISO 6721-3). The methods are not suitable for testing rubbers, for which the user is referred to ISO 4664-2.

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This document describes a forced, non-resonance method for determining the components of the shear complex modulus G* of polymers at frequencies typically in the range 0,01 Hz to 100 Hz. Higher-frequency measurements can be made, but significant errors in the dynamic properties measured are likely to result (see 10.2.2 and 10.2.3). The method is suitable for measuring dynamic storage moduli in the range 0,1 MPa to 50 MPa. NOTE Although materials with moduli greater than 50 MPa can be studied, more accurate measurements of their dynamic shear properties can be made using a torsional mode of deformation (see ISO 6721-2 and ISO 6721-7). This method is particularly suited to the measurement of loss factors greater than 0,02 and can therefore be conveniently used to study the variation of dynamic properties with temperature and frequency through most of the glass-rubber relaxation region (see ISO 6721-1). The availability of data determined over wide ranges of both frequency and temperature enables master plots to be derived, using frequency/temperature shift procedures, which display dynamic properties over an extended frequency range at different temperatures.

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This document describes a flexural, non-resonance method for determining the components of the flexural complex modulus Ef* of polymers at frequencies typically in the range 0,01 Hz to 100 Hz. Higher-frequency measurements can be made, but significant errors in the dynamic properties measured are likely to result (see 10.2.2 and 10.2.3). The method is suitable for measuring dynamic storage moduli in the range 10 MPa to 200 GPa. NOTE Although materials with moduli less than 10 MPa can be studied, more accurate measurements of their dynamic-mechanical properties can be made using shear modes of deformation (see ISO 6721-6). This method is particularly suited to the measurement of loss factors greater than 0,02 and can therefore be conveniently used to study the variation of dynamic properties with temperature and frequency through most of the glass-rubber relaxation region (see ISO 6721‑1). The availability of data determined over wide ranges of both frequency and temperature enables master plots to be derived, using frequency/temperature shift procedures, which present dynamic properties over an extended frequency range at different temperatures.

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This document describes a torsional, non-resonance method for determining the components of the shear complex modulus G* of solid polymers in the form of bars or rods at frequencies typically in the range 0,001 Hz to 100 Hz. Higher-frequency measurements can be made, but significant errors in the dynamic properties measured are likely to result (see 10.2.1 and 10.2.2). The method is suitable for measuring dynamic storage moduli ranging from about 10 MPa, which is typical of values obtained for stiff rubbers, to values of about 10 GPa which are representative of fibre-reinforced plastics. Although materials with moduli less than 10 MPa can be studied, more accurate measurements of their dynamic properties can be made using simple shear (see ISO 6721-6) or torsional deformations of thin layers between parallel plates. This method is particularly suited to the measurement of loss factors greater than 0,02 and may therefore be conveniently used to study the variation of dynamic properties with temperature and frequency through most of the glass-rubber relaxation region (see ISO 6721‑1). The availability of data determined over wide ranges of both frequency and temperature enable master plots to be derived, using frequency-temperature shift procedures, which display dynamic properties over an extended frequency range at different temperatures. NOTE Although loss factors below 0,1 can be more accurately determined using the torsion pendulum (see ISO 6721‑2), the method described in this document enables a much wider and continuous frequency range to be covered.

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This document describes a pulse propagation method for determining the storage component of the complex tensile modulus E' of polymers at discrete frequencies typically in the range 3 kHz to 10 kHz. The method is suitable for measuring materials with storage moduli in the range 0,01 GPa to 200 GPa and with loss factors below 0,1 at around 10 kHz. With materials having a higher loss, significant errors in velocity measurement are introduced through decay of amplitude. The method allows measurements to be made on thin films or fine fibres and long specimens, typically tapes of 300 mm × 5 mm × 0,1 mm or fibres of 300 mm × 0,1 mm (diameter). This method may not be suitable for cellular plastics, composite plastics and multilayer products.

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This document describes an ultrasonic wave propagation method for determining the storage components of the longitudinal complex modulus L* and the shear complex modulus G* of polymers at discrete frequencies typically in the range 0,5 MHz to 5 MHz. The method is suitable for measuring materials with storage moduli in the range 0,01 GPa to 200 GPa and with loss factors below 0,1 at around 1 MHz. With materials that have a higher loss, significant errors in velocity measurement are introduced through waveform distortion and can only be reduced using procedures that are outside the scope of this document. The method allows measurements to be made on small specimens, typically 50 mm × 20 mm × 5 mm, or small regions of larger specimens or sheets. It is therefore possible to obtain information on the homogeneity or anisotropy (see 10.5) of modulus in a specimen.

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This document specifies a method for the determination of the penetration temperature of thermoplastics using thermomechanical analysis (TMA). NOTE This method can also be used to measure the softening point.

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This document establishes general principles of temperature modulated differential scanning calorimetry (DSC) such as description of the principle and the apparatus, sampling, calibration and general aspects of the procedure and test report common to all parts of the ISO 19335 series. NOTE Details on performing specific methods are intended to be given in the future parts of the ISO 19335 series.

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ISO 11357-3:2018 specifies a method for the determination of the temperatures and enthalpies of melting and crystallization of crystalline or partially crystalline plastics.

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ISO 11357-6:2018 specifies methods for the determination of oxidation induction time (isothermal OIT) and oxidation induction temperature (dynamic OIT) of polymeric materials by means of differential scanning calorimetry (DSC). It is applicable to polyolefin resins that are in a fully stabilized or compounded form, either as raw materials or finished products. It can be applicable to other plastics.

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ISO 22007-1:2017 describes the background to methods for the determination of the thermal conductivity and thermal diffusivity of polymeric materials. Different techniques are available for these measurements and some may be better suited than others for a particular type, state and form of material. ISO 22007-1:2017 provides a broad overview of these techniques. Standards specific to these techniques, as referenced in this document, are used to carry out the actual test method.

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ISO 22007-4:2017 specifies a method for the determination of the thermal diffusivity of a thin solid disc of plastics in the thickness direction by the laser flash method. This method is based upon the measurement of the temperature rise at the rear face of the thin-disc specimen produced by a short energy pulse on the front face. The method can be used for homogeneous solid plastics as well as composites having an isotropic or orthotropic structure. In general, it covers materials having a thermal diffusivity, α, in the range 1 × 10−7 m2⋅s−1 α −4 m2⋅s−1. Measurements can be carried out in gaseous and vacuum environments over a temperature range from −100 °C to +400 °C. NOTE For inhomogeneous specimens, the measured values can be specimen thickness dependent.

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ISO 11357-1:2016 specifies several differential scanning calorimetry (DSC) methods for the thermal analysis of polymers and polymer blends, such as - thermoplastics (polymers, moulding compounds and other moulding materials, with or without fillers, fibres or reinforcements), - thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements), and - elastomers (with or without fillers, fibres or reinforcements). ISO 11357-1:2016 is intended for the observation and measurement of various properties of, and phenomena associated with, the above-mentioned materials, such as - physical transitions (glass transition, phase transitions such as melting and crystallization, polymorphic transitions, etc.), - chemical reactions (polymerization, crosslinking and curing of elastomers and thermosets, etc.), - the stability to oxidation, and - the heat capacity. ISO 11357-1:2016 specifies a number of general aspects of differential scanning calorimetry, such as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test report common to all following parts. Details on performing specific methods are given in subsequent parts of ISO 11357 (see Foreword).

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ISO 6721-10:2015 specifies the general principles of a method for determining the dynamic rheological properties of polymer melts at angular frequencies typically in the range of 0,01 rad·s-1 to 100 rad·s-1 by means of an oscillatory rheometer with a parallel-plate geometry. Angular frequencies outside this range can also be used (see Note 1). The method is used to determine values of the following dynamic rheological properties: complex shear viscosity η*, dynamic shear viscosity η', the out-of-phase component of the complex shear viscosity η", complex shear modulus G*, shear loss modulus G", and shear storage modulus G'. It is suitable for measuring complex shear viscosity values typically up to ~10 MPa·s (see Note 2). NOTE 1 The angular-frequency measurement range is limited by the specification of the measuring instrument and also by the response of the specimen. When testing using angular frequencies lower than 0,1 rad·s?1, the test time can increase significantly as the time taken to obtain a single measurement is proportional to the reciprocal of the angular frequency. Consequently, when testing at low angular frequencies, degradation or polymerization of the specimen is more likely to occur and have an effect on the results. At high angular frequencies, the specimen can distort or fracture at the edge, consequently invalidating the test results. NOTE 2 The range of complex shear viscosity values that can be measured is dependent on the specimen dimensions and also the specification of the measuring instrument. For a specimen of given dimensions, the upper limit of the range is limited by the machine's torque capacity, angular-displacement resolution, and compliance. However, correction can be made for compliance effects.

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ISO 11357-7:2015 specifies two methods (isothermal and non-isothermal) for studying the crystallization kinetics of partially crystalline polymers using differential scanning calorimetry (DSC). It is only applicable to molten polymers. NOTE These methods are not suitable if the molecular structure of the polymer is modified during the test.

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ISO 22007-2:2015 specifies a method for the determination of the thermal conductivity and thermal diffusivity, and hence the specific heat capacity per unit volume of plastics. The experimental arrangement can be designed to match different specimen sizes. Measurements can be made in gaseous and vacuum environments at a range of temperatures and pressures.

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ISO 11358-1:2014 specifies general conditions for the analysis of polymers using thermogravimetric techniques. It is applicable to liquids or solids. Solid materials may be in the form of pellets, granules or powders. Fabricated shapes reduced to appropriate specimen size may also be analysed by this method.

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ISO 11357-4:2014 specifies methods for determining the specific heat capacity of plastics by differential scanning calorimetry.

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ISO 22007-6:2014 specifies a modulated temperature method realizing the measurement of thermal conductivity. An input of temperature deviation is less than 1 K, and a double lock-in method is applied to amplify the small temperature modulation. ISO 22007-6:2014 specifies the method to determine the thermal conductivity in the range from 0,026 W/mK to 0,6 W/mK.

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ISO 11359-1:2014 specifies the general conditions for the thermomechanical analysis of thermoplastics and thermosetting materials, filled or unfilled, in the form of sheet or moulded parts. Thermomechanical analysis consists of the determination of deformations of a test specimen under constant load as a function of temperature and/or time.

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ISO 11358-3:2013 specifies an analysis method for determining the activation energy using the Ozawa-Friedman plot. It also specifies the preparation of master plots for verification of the reaction kinetics determined by thermogravimetry. The Ozawa-Friedman plot (logarithm of the rate of mass loss versus the reciprocal of absolute temperature at a given mass loss) is a derivative method that can be applied to data obtained by any mode of temperature change in thermal analysis; e.g. isothermal, constant heating rate, sample-controlled thermal analysis, temperature jump, and repeated temperature scanning.

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ISO 11357-5:2013 specifies a method for the determination of reaction temperatures and times, enthalpies of reaction, and degrees of conversion using differential scanning calorimetry (DSC). The method applies to monomers, prepolymers, and polymers in the solid or liquid state. The material can contain fillers and/or initiators in the solid or liquid state.

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ISO/TR 22007-5:2011 presents the results of interlaboratory testing for the determination of thermal conductivity and thermal diffusivity of two poly(methyl methacrylate) (PMMA) materials by means of the transient and the modulated methods presented in ISO 22007 parts 2 to 4 and additional transient and steady state methods.

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ISO 6721-12:2009 describes a compressive vibration, non-resonance method for determining the components of the compressive complex modulus E* of polymers at frequencies typically in the range 0,01 Hz to 100 Hz. The method is suitable for measuring dynamic storage moduli of semi-rigid polymers in the range 1 MPa to 1 GPa.

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ISO 22007-3:2008 specifies a temperature wave analysis method for the determination of the thermal diffusivity of thin films and plates of plastics in the through-thickness direction. The method can be used on plastics in either the solid or molten state, and having either an isotropic or an orthotropic structure. The method covers values of the thermal diffusivity, α, in the range 1,0 x 10-8 m2s-1 α -4 m2s-1. Measurements can be performed either in air or in another atmosphere, e.g. an inert gas, at atmospheric pressure or at other, reduced or elevated, pressures, or under a vacuum, at a variety of temperatures.

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This part of ISO 11359 specifies a test method, using thermodilatometry, for the determination of the coefficient of linear thermal expansion of plastics in a solid state by thermomechanical analysis (TMA). This part of ISO 11359 also specifies the determination of the glass transition temperature using TMA. NOTE The coefficient of linear thermal expansion can be measured using various types of thermodilatometry apparatus. This part of ISO 11359 concerns only TMA apparatus.

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Specifies a bending-vibration method based upon resonance curves for determining the flexural complex modulus of homogeneous plastics and the damping properties of laminated plastics intended for acoustic insulation.

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ISO 11358-2:2014 specifies a method for the determination of the activation energy, Ea, in the Arrhenius formula for the decomposition of polymers using a thermogravimetric technique. The method is applicable only if the reaction proceeds by a single mechanism. It is applicable to multistage reactions if they consist of clearly separated single-stage steps.

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ISO 11357-2:2013 specifies methods for the determination of the glass transition temperature and the step height related to the glass transition of amorphous and partially crystalline plastics.

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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. ISO 6721-1:2011 is an introductory section which includes the definitions and all aspects that are common to the individual test methods described in the subsequent parts. Different deformation modes may 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.

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ISO 11357-3:2011 specifies a method for the determination of the temperatures and enthalpies of melting and crystallization of crystalline or partially crystalline plastics.

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ISO 11357 specifies several differential scanning calorimetry (DSC) methods for the thermal analysis of polymers and polymer blends, such as thermoplastics (polymers, moulding compounds and other moulding materials, with or without fillers, fibres or reinforcements); thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements); elastomers (with or without fillers, fibres or reinforcements). ISO 11357 is intended for the observation and measurement of various properties of the above-mentioned materials, such as physical transitions (glass transition, phase transitions such as melting and crystallization, polymorphic transitions, etc.); chemical reactions (polymerization, crosslinking and curing of elastomers and thermosets, etc.); the stability to oxidation; the heat capacity. ISO 11357-1:2009 specifies a number of general aspects of differential scanning calorimetry, such as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test report common to all following parts. Details on performing specific methods are given in subsequent parts of ISO 11357.

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ISO 22007-1:2009 describes the background to methods for the determination of the thermal conductivity and thermal diffusivity of polymeric materials. Different techniques are available for these measurements and some may be better suited than others for a particular type, state and form of material. ISO 22007-1 provides a broad overview of these techniques. Standards specific to these techniques, as referenced in ISO 22007-1, are used for the actual test methods.

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ISO 22007-4:2008 specifies a method for the determination of the thermal diffusivity of a thin solid disc of plastics in the thickness direction by the laser flash method. This method is based upon the measurement of the temperature rise at the rear face of the thin-disc specimen produced by a short energy pulse on the front face. The method can be used for homogeneous solid plastics as well as composites having an isotropic or orthotropic structure. In general, it covers materials having a thermal diffusivity, α, in the range 1 x 10-7 m2s-1 α -4 m2s-1. Measurements can be carried out in gaseous and vacuum environments over a temperature range from -100 °C to +400 °C. For inhomogeneous specimens, the measured values may be specimen thickness dependent.

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ISO 22007-2:2008 specifies a method for the determination of the thermal conductivity and thermal diffusivity, and hence the specific heat capacity per unit volume, of plastics. The experimental arrangement can be designed to match different specimen sizes. Measurements can be made in gaseous and vacuum environments at a range of temperatures and pressures. This method is suitable for testing homogeneous and isotropic materials, as well as anisotropic materials with a uniaxial structure. In general, the method is suitable for materials having values of thermal conductivity, λ, in the approximate range 0,01 Wm-1K-1 λ -1K-1 and values of thermal diffusivity, α, in the range 5 x 10-8 m2s-1 ≤ α ≤ 10-4 m2s-1, and for temperatures, T, in the approximate range 50 K T The thermal-transport properties of liquids can also be determined, provided care is taken to minimize thermal convection.

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