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

This document specifies methods for the determination of components in plastics that can be extracted by hot organic liquids near their boiling points. It also specifies a special extraction method called cold-extraction. The extractable components can be monomers, oligomers, polymers, plasticizers, stabilizers, etc. The kind and percentage of extractable matter influence the properties of plastics. This document does not apply to plastics that come into contact with food or drinking water, because special regulations for those plastics are established in many countries. The methods of this document are not intended to be used for migration tests. If this document is used to test plastics other than those mentioned in Table 1, the operating conditions are intended to be agreed upon by the interested parties.

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. Annex C provides further information for calculating the volume of the specimen used for the determination of the density in the case that method A (the immersion method) is applied.

This document 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.

This document specifies a method for the determination of the temperatures and enthalpies of melting and crystallization of crystalline or partially crystalline plastics using conventional DSC as specified in ISO 11357-1. This document is not applicable to fast DSC as specified in ISO 23976.

This document describes procedures for determining the specific volume of plastics as a function of temperature and pressure in both the molten and solid states. This document specifies the use of a piston-equipped apparatus in which the test sample, held in a measurement cell, is pressurized by means of the piston. Measurements under conditions of constant pressure or constant temperature can be made. NOTE For the acquisition of data needed for processing design, the isobaric cooling method is found to be more useful, see ISO 17282. The result of this measurement cannot be used directly for injection-moulding simulation. This document is used to obtain: — pvT diagrams that represent the relationship which exists between pressure, specific volume and temperature for a given material; — volumetric compressibility and volumetric thermal-expansion coefficients; — information on first-order and glass transitions as a function of temperature and pressure.

This document specifies a method for the determination of reaction temperatures and times, enthalpies of reaction, and degrees of conversion using conventional differential scanning calorimetry (DSC) as specified in ISO 11357-1. 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. This document is not applicable to fast DSC as specified in ISO 23976.[ REF Reference_ref_2 \r \h 1 08D0C9EA79F9BACE118C8200AA004BA90B0200000008000000100000005200650066006500720065006E00630065005F007200650066005F0032000000 ]

This document specifies three methods for the determination of the ash of poly(vinyl chloride). The general procedures given in ISO 3451-1 are followed. For ash, method A is used. For sulfated ash, methods B and C are used. All three methods are applicable to resins, compounds and finished products. Methods B and C are applicable when lead-containing compounds are present.

This document 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 or a cone-and-plate geometry. Angular frequencies outside this range can also be used. The method is applicable for determining 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”, shear storage modulus G', phase angle δ, and loss factor tanδ. It is suitable for measuring complex shear viscosity values typically up to ~10 MPa s. NOTE The shear loss modulus G´´ is sometimes also called viscous shear modulus and the shear storage modulus G´ is sometimes also called elastic shear modulus.

This document specifies the test method for determination of particle size of ion exchange resin by laser diffraction, ranging from 0,1 μm to 2,0 mm.

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

This document is applicable to the qualitative analysis of plastic materials in their original form by Raman spectroscopy. It describes procedures to determine the composition of unknown general plastics and multi-layer film plastics.

This document 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 can be better suited than others for a particular type, state and form of material. This document 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.

This document specifies methods for determination of the ash of polyamides, both filled and unfilled. It follows the general procedures given in ISO 3451-1.

This document specifies a method for the determination of the thermal diffusivity of a thin solid disc of plastics in the thickness direction by the light 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 is applicable to 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.

This part of IEC 62321 specifies two different techniques for the determination of tris(2‑chloroethyl) phosphate (TCEP) in plastics, the GC-MS or LC-MS method, both of which are applicable to quantitative analysis. These two techniques are applicable to use with polyurethane, polyvinylchloride, and polyethylene materials containing TCEP between 200 mg/kg to 2 000 mg/kg. These test methods do not apply to plastic materials having a processing temperature higher than 230 °C. GC-MS using a pyrolyser/thermal desorption accessory (Py/TD-GC-MS) technique is described in REF _Ref141858781 \w \h Annex A 08D0C9EA79F9BACE118C8200AA004BA90B02000000080000000E0000005F005200650066003100340031003800350038003700380031000000 and can be used for the screening of TCEP in plastics. NOTE TCEP starts thermal decomposition at approximately 230 °C. Polymer types that have a processing temperature into shapes of plastics (e.g. pellets, moulded parts or sheets) not exceeding the decomposition temperature can contain TCEP.

This document specifies a spectrometric method for the determination of the absorbance at a wavelength of 290 nm of caprolactam for industrial use.

This document specifies a spectrometric method of determining the colour, expressed in Hazen units, of a 50 % aqueous caprolactam solution as a measure of coloured impurities content of the sample.

This document specifies two methods, A and B, for determining the pourability of plastics in powdered and granular form, by measuring the flow time through a funnel under specified conditions. From method A, information concerning the processability can be derived, whilst method B is especially designed for process control during manufacture. The methods specified are not necessarily applicable to all plastics in powdered and granular form.

This document specifies test methods by centrifugation of water content of styrene anion exchange resins in hydroxide form.

This document specifies test methods of the strong-base group capacity, the weak-base group capacity and the weak-acid group capacity of acrylic anion exchange resins.

This document specifies test methods of the total exchange capacity, the strong-base group capacity and the weak-base group capacity of the styrene anion exchange resins in hydroxide form.

This document specifies a method for the determination of the thermal effusivity. This document is applicable to materials with thermal effusivity in the approximate range 40 W⋅s1/2⋅m−2⋅K−1 bn W⋅s1/2⋅m‑2⋅K‑1, and temperatures in the range of 50 K T

The ISO 11357 series 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). The ISO 11357 series is applicable 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. This document 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 parts. Details on performing specific methods are given in subsequent parts of the ISO 11357 series (see Foreword).

This document 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.

This document specifies a method for the determination of vinyl chloride monomer in homopolymer and copolymer resins of vinyl chloride and compounded materials. The method is based on sample dissolution and headspace gas chromatography. Concentrations of vinyl chloride in the range 0,1 mg/kg to 3,0 mg/kg can be determined.

This document specifies a method for the determination of the density of liquid resins using a pycnometer.

This document specifies a method of determining the bulk factor of a moulding material based on the ratio of the apparent volumetric density of a given quantity of particles and the corresponding material density.

This document specifies two procedures for the determination of the melt mass-flow rate (MFR) and the melt volume-flow rate (MVR) of thermoplastic materials under specified conditions of temperature and load. Procedure A is a mass-measurement method. Procedure B is a displacement-measurement method. Normally, the test conditions for measurement of melt flow rate are specified in the material standard with a reference to this document. The test conditions normally used for thermoplastics are listed in Annex A. The MVR is particularly useful when comparing materials of different filler content and when comparing filled with unfilled thermoplastics. The MFR can be determined from MVR measurements, or vice versa, provided the melt density at the test temperature is known. This document is also possibly applicable to thermoplastics for which the rheological behaviour is affected during the measurement by phenomena such as hydrolysis (chain scission), condensation and cross-linking, but only if the effect is limited in extent and only if the repeatability and reproducibility are within an acceptable range. For materials which show significantly affected rheological behaviour during testing, this document is not appropriate. In such cases, ISO 1133-2 applies. NOTE The rates of shear in these methods are much smaller than those used under normal conditions of processing, and therefore it is possible that data obtained by these methods for various thermoplastics will not always correlate with their behaviour during processing. Both methods are used primarily in quality control.

This document 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 gives guidelines for testing homogeneous and isotropic materials, as well as anisotropic materials with a uniaxial structure. The homogeneity of the material extends throughout the specimen and no thermal barriers (except those next to the probe) are present within a range defined by the probing depth(s) (see 3.1). The method is suitable for materials having values of thermal conductivity, λ, in the approximate range 0,010 W∙m−1∙K−1 −1∙K−1, values of thermal diffusivity, α, in the range 5 × 10−8 m2∙s−1 −4 m2∙s−1, and for temperatures, T, in the approximate range 50 K T NOTE 1 The specific heat capacity per unit volume, C, C = ρ ∙ cp, where ρ is the density and cp is the specific heat per unit mass and at constant pressure, can be obtained by dividing the thermal conductivity, λ, by the thermal diffusivity, α, i.e. C = λ/α, and is in the approximate range 0,005 MJ∙m−3∙K−1 −3∙K−1. It is also referred to as the volumetric heat capacity. NOTE 2 If the intention is to determine the thermal resistance or the apparent thermal conductivity in the through-thickness direction of an inhomogeneous product (for instance a fabricated panel) or an inhomogeneous slab of a material, reference is made to ISO 8301, ISO 8302 and ISO 472. The thermal-transport properties of liquids can also be determined, provided care is taken to minimize thermal convection.

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 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 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 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 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 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 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.