ISO/TC 61/SC 5 - Physical-chemical properties

This document specifies general conditions for the analysis of polymers using thermogravimetric techniques. It is applicable to liquids or solids. Solid materials can be in the form of pellets, granules or powders. Fabricated shapes reduced to appropriate specimen size can also be analysed by this method. This document establishes methods for the investigation of physical effects and chemical reactions that are associated with changes of mass. This document can be used to determine the temperature(s) and rate(s) of decomposition of polymers, and to measure at the same time the amounts of volatile matter, additives and/or fillers they contain. This document is applicable to measurements in dynamic mode (mass change versus temperature or time under programmed temperature conditions) or isothermal mode (mass change versus time at constant temperature). This document is applicable to measurements at different testing atmospheres, such as separation of decomposition in an inert atmosphere from oxidative degradation.

This document 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.

This document specifies two methods for evaluating the melting behaviour of semi-crystalline polymers. a) Method A: Capillary tube This method is based on the changes in shape of the polymer. It is applicable to all semi-crystalline polymers and their compounds. NOTE 1 Method A can also be useful for the evaluation of the softening of non-crystalline solids. b) Method B: Polarizing microscope This method is based on changes in the optical properties of the polymer. It is applicable to polymers containing a birefringent crystalline phase. It might not be suitable for plastics compounds containing pigments and/or other additives which can interfere with the birefringence of the polymeric crystalline zone. NOTE 2 Another method applicable to semi-crystalline polymers is described in ISO 11357‑3.

This document specifies two test methods for determining the refractive index of plastics, namely: — Method A: a refractometric method for measuring the refractive index of moulded parts, cast or extruded sheet or film, by means of a refractometer. It is applicable not only to isotropic transparent, translucent, coloured or opaque materials but also to anisotropic materials. — Method B: an immersion method (making use of the Becke line phenomenon) for determining the refractive index of powdered or granulated transparent materials by means of a microscope. Monochromatic light, in general, is used to avoid dispersion effects. NOTE The refractive index is a fundamental property which can be used for checking purity and composition, for the identification of materials and for the design of optical parts. The change in refractive index with temperature can give an indication of transition points of materials.

This document 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 applicable for measuring dynamic storage moduli of semi-rigid polymers in the range 1 MPa to 1 GPa. This method is particularly suited to the measurements of dynamic moduli and loss factors of semi‑rigid plastics in the shape of a right-angled prism, cylinder or tube and can 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).

This document specifies the requirements for the laboratory testing of the resistivity of specially prepared specimens of plastics rendered conductive by the inclusion of conductive fillers or suitable modification of the structure. The test is applicable to materials of resistivity less than 106 Ω⋅cm (104 Ω⋅m). The result is not strictly a volume resistivity, because of surface conduction, but the effects of the latter are generally negligible.

This document specifies a test method, using thermodilatometry[1], for the determination of the coefficient of linear thermal expansion of plastics in a solid state by thermomechanical analysis (TMA). This document 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 document concerns only TMA apparatus.

This document specifies a method for the measurement of haze, an optical property resulting from wide-angle scattering of light, in transparent and substantially colourless plastics. This method is applicable to the measurement of haze values of less than 40 %. NOTE The haze of abraded or matted transparent plastics can be measured, but the value obtained can be erroneously lower than the true value due to light scattering within a narrow angle.

This document covers the determination of the total luminous transmittance, in the visible region of the spectrum, of planar transparent plastics and substantially colourless plastics, using a double-beam scanning spectrophotometer. This document cannot be used for plastics which contain fluorescent materials. This document is applicable to transparent moulding materials, films and sheets not exceeding 10 mm in thickness. NOTE 1 Total luminous transmittance can also be determined by a single-beam instrument as in ISO 13468-1. NOTE 2 Substantially colourless plastics include those which are faintly tinted. NOTE 3 Specimens more than 10 mm thick can be measured provided the instrument can accommodate them, but the results cannot be comparable with those obtained using specimens less than 10 mm thick.

This document specifies a procedure for the determination of an elasticity index based on measurements of the shear storage modulus using oscillatory rheometers, establishes general principles, and gives guidelines for performance of measurements. The elasticity index is applicable to all thermoplastics and viscoelastic materials for which the elastic behaviour is a crucial application property.

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.

This document specifies general terms and definitions that are used in the context of rotational and oscillatory rheometry. Further terms and definitions can be found in the other parts of the ISO 3219 series where they are used.

This document specifies the general principles of rotational and oscillatory rheometry. Detailed information is presented in Annex A. Further background information is covered in subsequent parts of the ISO 3219 series, which are currently in preparation.

This document specifies the general principles of a method for determining the transient extensional viscosity of polymer melts. The procedure details the measurement of polymer melt specimens stretched uniaxially under conditions of constant strain rate and constant temperature. The method is capable of measuring the transient extensional viscosity of polymer melts at Hencky strain rates typically in the range 0,01 s–1 to 1 s–1, at Hencky strains up to approximately 4 and at temperatures up to approximately 250 °C (see NOTEs 1 and 2). It is suitable for measuring transient extensional viscosity values typically in the range from approximately 104 Pa⋅s to 107 Pa⋅s (see NOTE 3). NOTE 1 Hencky strains and strain rates are used (see Clause 3). NOTE 2 Values of strain, strain rate and temperature outside these limiting values can be attained. NOTE 3 The operating limit of an instrument, in terms of the lowest transient extensional viscosity values that can be measured, is due to a combination of factors, including the ability of the specimen to maintain its shape during testing and the resolution of the instrument.

This document defines the general conditions for the determination of the reduced viscosity, intrinsic viscosity and K‑value of organic polymers in dilute solution. It defines the standard parameters that are applied to viscosity measurement. This document is used to develop standards for measuring the viscosities in solution of individual types of polymer. It is also used to measure and report the viscosities of polymers in solution for which no separate standards exist.

This document specifies methods for determining the fluidity of plastics melts subjected to shear stresses at rates and temperatures approximating to those arising in plastics processing. Testing plastics melts in accordance with these methods is of great importance since the fluidity of plastics melts is generally not dependent solely on temperature, but also on other parameters; in particular shear rate and shear stress. The methods described in this document are useful for determining melt viscosities from 10 Pa∙s to 107 Pa∙s, depending on the measurement range of the pressure and/or force transducer and the mechanical and physical characteristics of the rheometer. The shear rates occurring in extrusion rheometers range from 1 s−1 to 106 s−1. Elongational effects at the die entrance cause extrudate swelling at the die exit. Methods for assessing extrudate swelling have also been included. The rheological techniques described are not limited to the characterization of wall-adhering thermoplastics melts only; for example, thermoplastics exhibiting "slip" effects[1][2] and thermosetting plastics can be included. However, the methods used for determining the shear rate and shear viscosity are invalid for materials which are not wall-adhering. Nevertheless, this document can be used to characterize the rheological behaviour of such fluids for a given geometry.

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.

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.

This document specifies a method for determining the drawing and break characteristics of molten plastics. The method involves the measurement of the force generated in deforming a molten filament under defined extrusion temperature and drawing conditions. Data is generated under non-isothermal and non-homogeneous deformation conditions. However, it is useful for the interpretation of polymer behaviour in extensional flow. The method is suitable for thermoplastics moulding and extrusion materials that can be extruded using a capillary extrusion rheometer, or an extruder with capillary rod die or other extrusion devices and have sufficient melt strength to be handled without difficulty. The method is applicable to chemically stable materials that produce a uniform extrudate free from heterogeneities, bubbles, unmelted impurities, etc. This method can provide information on — processability for all extrusion techniques, — the effect of mechanical and thermal history, and — the effect of chemical structure, such as branching, entanglements and molecular mass. This technique is one of a number of techniques that can be used to measure the extensional flow behaviour of a material. This method of measurement does not necessarily reproduce the drawing conditions to which thermoplastics are subjected to during their processing.

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).

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

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.

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.

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

This document specifies the determination of total luminous transmittance and total luminous reflectance on clear, translucent or opaque plastics. Specimen shapes include moulded plaque or discs, films and sheets. Fluorescent plastics and chromatic colour plastics are not covered by this document. NOTE The scope of ISO 13468-1 shows that ISO 13468-1 covers planar transparent and substantially colourless plastics. The method in this document provide the way to trap diffused light and covers to measure translucent and opaque plastics.

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.

This document covers the determination of the total luminous transmittance, in the visible region of the spectrum, of planar transparent and substantially colourless plastics, using a single-beam photometer with a specified CIE Standard light source and photodetector. This document cannot be used for plastics which contain fluorescent materials. This document is applicable to transparent moulding materials, films and sheets not exceeding 10 mm in thickness. NOTE 1 Total luminous transmittance can also be determined by a double-beam spectrophotometer as in ISO 13468-2. This document, however, provides a simple but precise, practical and quick determination. This method is suitable for use not only for analytical purposes but also for quality control. NOTE 2 Substantially colourless plastics include those which are faintly tinted. NOTE 3 Specimens more than 10 mm thick can be measured provided the instrument can accommodate them, but the results might not be comparable with those obtained using specimens less than 10 mm thick.

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.

This document specifies a method for determining the average molecular weight and the molecular weight distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at a temperature lower than 60 °C (see Annex A). The average molecular weight and the molecular weight distribution are calculated from a calibration curve prepared using polymer standards. Therefore, this test method is classified as a relative method (see ISO 16014-1).

This document specifies a method for determining the average molecular weight and the molecular weight distribution of polymers using size-exclusion chromatography (SEC). The average molecular weight and the molecular weight distribution are calculated using a universal calibration curve instead of the conventional calibration curve. NOTE This test method is classified as a relative method as described in ISO 16014-1, but the average molecular weights and molecular weight distributions calculated by the method are equal to, or nearly equal to, the absolute values. For details, see the Annex A.

This document specifies a general method for determining the average molecular weight and the molecular weight distribution of polymers using SEC-LS, i.e. size-exclusion chromatography coupled with light-scattering detection. The average molecular weight and the molecular weight distribution are calculated from molecular weight data and weight concentrations determined continuously with elution time. The molecular weight at each elution time is determined absolutely by combining a light-scattering detector with a concentration-sensitive detector. Therefore, SEC-LS is classified as an absolute method. This method is applicable to linear homopolymers and to nonlinear homopolymers such as branched, star-shaped, comb-like, stereo-regular and stereo-irregular polymers. It can also be applied to heterophasic copolymers whose molecular composition cannot vary. However, SEC-LS is not applicable to block, graft or heterophasic copolymers whose molecular composition can vary. And the methods are applicable to molecular weights ranging from that of the monomer to 3 000 000, but are not intended for samples that contain > 30 % of components having a molecular weight

This document specifies a method for determining the average molecular weight and the molecular weight distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at temperatures between 60 °C and 220 °C (see Annex A). The average molecular weight and the molecular weight distribution are calculated from a calibration curve prepared using polymer standards. Therefore, this test method is classified as a relative method (see ISO 16014-1).

This document specifies a general method for determining the average molecular weight and the molecular weight distribution of polymers using size-exclusion chromatography (SEC). The average molecular weight and the molecular weight distribution are calculated from a calibration curve constructed using polymer standards if using one of the SEC techniques described in ISO 16014-2 to ISO 16014-4 or from a calibration curve constructed using absolute molecular weight data if using size-exclusion chromatography coupled with light-scattering detection (SEC-LS) as described in ISO 16014-5.

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.

This document specifies methods for the determination of the water content of plastics in the form of powder, granules, and finished articles. These methods do not test for water absorption (kinetics and equilibrium) of plastics as measured by ISO 62. Method A is suitable for the determination of water content as low as 0,1 % with an accuracy of 0,1 %. Method B and Method C are suitable for the determination of water content as low as 0,01 % with an accuracy of 0,01 %. Method D is suitable for the determination of water content as low as 0,01 % with an accuracy of 0,01 %. Method E is suitable for the determination of water content as low as 0,001 % with an accuracy of 0,001 %. The stated accuracies are detection limits which depend also on the maximal possible sample mass. The water content is expressed as a percentage mass fraction of water. Method D is suitable for polyamide (PA), polycarbonate (PC), polypropylene (PP), polyethylene (PE), epoxy resin, polyethylene terephthalate (PET), polyester, polytetrafluoroethylene (PTFE), polyvinyl chloride (PVC), polylactide (PLA), polyamidimid (PAI), it is especially not recommended for samples which can release NH3. Methods A, B, C and E are generally suitable for all types of plastic and moisture level. Water content is an important parameter for processing materials and is expected to remain below the level specified in the appropriate material standard. Six alternative methods are specified in this document. — Method A is an extraction method using anhydrous methanol followed by a Karl Fischer titration of the extracted water. It can be used for all plastics and is applicable to granules smaller than 4 mm × 4 mm × 3 mm. The method can also be used for, e.g. prepolymer materials in the form of a powder that are insoluble in methanol. — Method B1 is a vaporization method using a tube oven. The water contained in the test portion is vaporized and carried to the titration cell by a dry air or nitrogen carrier gas, followed by a Karl Fischer titration or a coulometric determination by means of a moisture sensor of the collected water. It can be used for all plastics and is applicable to granules smaller than 4 mm × 4 mm × 3 mm. — Method B2 is a vaporization method using a heated sample vial. The water contained in the test portion is vaporized and carried to the titration cell by a dry air or nitrogen carrier gas, followed by a Karl Fischer titration of the collected water. It can be used for all plastics and is applicable to granules smaller than 4 mm × 4 mm × 3 mm. — Method C is a manometric method. The water content is determined from the increase in pressure, which results when the water is evaporated under a vacuum. This method is not applicable to plastic samples containing volatile compounds, other than water, in amounts contributing significantly to the vapour pressure at room temperature. Checks for the presence of large amounts of volatile compounds are to be carried out periodically, for example by gas chromatography. Such checks are particularly required for new types or grades of material. — Method D is a thermocoulometric method using a diphosphorus pentoxide (P2O5) cell for the detection of the vaporized water. The water contained in the test portion is vaporized and carried to the sensor cell by a dry air or nitrogen carrier gas, followed by a coulometric determination of the collected water. This method is not applicable to plastic samples containing volatile compounds, other than water, in amounts contributing significantly to the vapour pressure at room temperature. This is specially related to volatile components which can react with the acidic coating of the diphosphorus pentoxide sensor, e.g. ammonia or any kind of amines. Checks for the presence of large amounts of volatile compounds are to be carried out periodically. Such checks are particularly required for new types or grades of material. — Method E is a calcium hydride based method. The water conte

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.

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.

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.

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.

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.

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.

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.

This document specifies a gradient column method for the determination of the density of non-cellular moulded or extruded plastics or pellets in void-free form. Density gradient columns are columns containing a mixture of two liquids, the density in the column increasing uniformly from top to bottom. NOTE Density is frequently used to follow variations in physical structure or composition of plastic materials. Density can also be useful in assessing the uniformity of samples or specimens. The density of plastic materials can depend upon the choice of specimen preparation method. When this is the case, precise details of the specimen preparation method are intended to be included in the appropriate material specification.

This document specifies three methods for the determination of the density of non-cellular plastics in the form of void-free moulded or extruded objects, as well as powders, flakes and granules. — Method A: Immersion method, for solid plastics (except for powders) in void-free form. — Method B: Liquid pycnometer method, for particles, powders, flakes, granules or small pieces of finished parts. — Method C: Titration method, for plastics in any void-free form. NOTE Density is frequently used to follow variations in physical structure or composition of plastic materials. Density can also be useful in assessing the uniformity of samples or specimens. Often, the density of plastic materials depend upon the choice of specimen preparation method. When this is the case, precise details of the specimen preparation method are intended to be included in the appropriate material specification. This note is applicable to all three methods.

This document specifies general methods, with suitable test conditions, for the determination of the ash of a range of plastics. The particular conditions chosen can be included in the specifications for the plastic material in question. Particular conditions applicable to poly(alkylene terephthalate) materials, unplasticized cellulose acetate, polyamides and poly(vinyl chloride) plastics, including some specific filled, glass-fibre-reinforced and flame-retarded materials, are specified in ISO 3451-2, ISO 3451-3, ISO 3451-4 and ISO 3451-5.

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.

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.

This document specifies the general principles of a method, using an inclined‑tube falling‑ball viscometer, for determining the viscosity of polymers and resins in the liquid emulsified or dispersed state. It is intended for application to liquids over a viscosity measurement range of 0,6 mPa·s to 250 000 mPa·s (temperature range −20 °C to +120 °C) for which the shear stress and shear rate are proportional, i.e. the viscosity is independent of the shear rate. This ideal behaviour is commonly known as Newtonian behaviour. If a liquid differs significantly from this behaviour, different results can be obtained with the different balls of a falling‑ball viscometer or from viscometers with different geometries, such as capillary and rotational viscometers.

This document describes a high-performance liquid chromatography (HPLC) method for determining the concentrations of cyclic oligomers of caprolactam, from 0,01 % by mass upwards, and linear oligomers of caprolactam, from 5 mg/kg upwards, both up to and including the hexamer of caprolactam (n = 6), in samples of polyamide 6, caprolactam and mixtures of rearrangement products in water. A second, significantly faster, HPLC method is included for determination of caprolactam and its cyclic dimer, based on the same principle and using the same equipment as the first method.

This document specifies a general method for determining the average molecular mass and molecular mass distribution of polymers (see Reference [1]) from 2 000 g ⋅ mol−1 to 20 000 g ⋅ mol−1 by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). The average molecular masses and molecular mass distributions are calculated from a calibration curve constructed using synthetic-polymer and/or biopolymer standards. This method is therefore classified as a relative method. The method is not applicable to polyolefins or to polymers with a polydispersity >1,2.