ISO/TC 61/SC 5/WG 11 - Analytical methods

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 by centrifugation of water content of styrene anion exchange resins in hydroxide form.

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 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 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 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 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 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 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 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 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 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 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 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 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 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 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 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.

ISO 19929:2017 specifies a general method for determining the average molecular mass and mixture ratio of poly(ethylene glycol) (PEG) and its derivatives with different end groups by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). It is applicable to PEG and its derivatives with molecular masses from 500 g mol−1 to 20 000 g mol−1. The composition is calculated by means of a calibration curve constructed using standard polymer mixtures, where the peak area ratio is plotted versus the mass ratio. This document can be applied to other polymers with monomeric unit similar to PEG.

ISO 6427:2013 specifies methods for the determination of components in plastics that can be extracted by hot organic liquids near their boiling points. For one special case, a so-called cold-extraction method is given. The extractable components can be monomers, oligomers, polymers, plasticizers, stabilizers, etc. The kind and percentage of extractable matter influence the properties of plastics. The recommended extraction liquid depends on the type of plastic and on the purpose of the determination. The extracted amounts of special constituents are often not quantitative in the sense of analytical chemistry.

ISO 24538:2008 specifies a method for the determination of residual vinyl chloride monomer in homopolymer and copolymer resins of vinyl chloride. The method is based on a static headspace gas-chromatographic technique (i.e. the analysis of the vapour phase in equilibrium with the solid phase at constant temperature) and is suitable for all kinds of homopolymer and copolymer resin. It is done directly on the resin in powder form.

This part of ISO 3451 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 International Standard specifies a spectrometric method for the determination of the permanganate absorption number of caprolactam for industrial use. The permanganate absorption number is a measure of the oxidizable impurities in caprolactam, determined in a buffered neutral aqueous medium under fixed conditions. The method is applicable to purified caprolactam (and intermediates in the caprolactam purification process) with an alkalinity or acidity lower than 0,50 mmol/kg and a PAN value of up to 35.

This part of ISO 1183 specifies a method for the determination of the density or the specific volume of solid noncellular plastics of any shape which do not contain closed pores.

This part of ISO 3451 specifies methods for determination of the ash of poly(ethylene terephthalate), poly(butylene terephthalate) and copolymers of the two, both filled and unfilled. The general procedures given in ISO 3451-1 are followed. For unfilled materials method A or method C of ISO 3451-1:1997 is used. For filled and glass-fibre reinforced materials method A of ISO 3451-1:1997 is used. For glass-fibre filled materials, containing flame retardant, antimony trioxide, and/or other, volatilize additives, for instance pigment zinc sulfide, a modification is incorporated to remove these as volatile bromine component(s).

Specifies a method for the determination of the ash unplasticized cellulose acetate, free of additives, fillers, dyes or other materials, which may affect the result. -Ignition of a test portion and calcination in a muffle furnace maintained at 575 C or 850 C (as agreed). Higher temperatures such as 850 C will convert carbonates to the oxides and thus give lower values. The general instructions in ISO 3451/1 shall be followed.

1.1 ISO 15512:2016 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 %. Water content is an important parameter for processing materials and has to remain below the level specified in the appropriate material standard. 1.2 Four alternative methods are specified in this International Standard. ? 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 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.

ISO 15512:2014 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 %.

ISO 16014-1:2012 specifies a general method for determining the average molecular mass and the molecular mass distribution of polymers using size-exclusion chromatography (SEC). The average molecular mass and the molecular mass distribution are calculated from a calibration curve constructed using polymer standards if using one of the SEC techniques described in ISO 16014-2 to -4 or from a calibration curve constructed using absolute molecular mass data if using size-exclusion chromatography coupled with light-scattering detection (SEC‑LS) as described in ISO 16014-5.

ISO 16014-3:2012 specifies a method for determining the average molecular mass and the molecular mass distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at a temperature lower than 60 °C. The average molecular mass and the molecular mass distribution are calculated from a calibration curve prepared using polymer standards. Therefore, this test method is classified as a relative method.

ISO 16014-4:2012 specifies a method for determining the average molecular mass and the molecular mass distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at temperatures between 60 °C and 180 °C. The average molecular mass and the molecular mass distribution are calculated from a calibration curve prepared using polymer standards. Therefore, this test method is classified as a relative method.

ISO 16014-2:2012 specifies a method for determining the average molecular mass and the molecular mass distribution of polymers using size-exclusion chromatography (SEC). The average molecular mass and the molecular mass distribution are calculated using a universal calibration curve instead of the conventional calibration curve.

ISO 10927:2011 specifies a general method for determining the average molecular mass and molecular mass distribution of polymers 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.

ISO 6401:2008 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. A "dry method", suitable for PVC resins but not compounded materials, is widely used within the industry for in-house determinations. A separate International Standard based on this methodology is under development.

ISO 3451-1:2008 specifies general methods, with suitable test conditions, for the determination of the ash of a range of plastics (resins and compounds). The particular conditions chosen may 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.

ISO 15512:2008 specifies methods for the determination of the water content of plastics in the form of granules and finished articles. These methods do not test for water absorption (kinetics and equilibrium) of plastics as measured by ISO 62. The methods are suitable for the determination of water content as low as the following levels: Method A 0,1 % or better; Method B 0,01 % or better; Method C 0,01 % or better. Three alternative methods are specified: 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 having a maximum size of 4 mm x 4 mm x 3 mm. Method B is a vaporization method using heated, dry air or nitrogen gas to evaporate the water, 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 x 4 mm x 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 should be carried out periodically, for example by gas chromatography. Such checks are particularly required for new types or grades of material.

ISO 15033:2007 describes an HPLC (high-performance liquid chromatography) 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.

ISO 1183-2:2004 specifies a gradient column method for the determination of the density of non-cellular moulded or extruded plastics 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.

ISO 11337:2004 specifies a method for determining epsilon-caprolactam and omega-laurolactam in polyamides by gas chromatography. It is suitable particularly for the determination of epsilon-caprolactam in polyamide 6 and omega-laurolactam in polyamide 12. Bearing in mind that gas chromatography offers a wide range of possible conditions, the method specified is that shown to have been suitable in practice. Two variants of the basic method are specified: Method A is an extraction method with boiling methanol, and the extract is injected into a gas chromatograph. Method B is a method using a solvent, and the solution is injected into a gas chromatograph. Method A is suitable for the determination of epsilon-caprolactam and method B for epsilon-caprolactam and omega-laurolactam.

ISO 1183-1:2004 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 pyknometer method, for particles, powders, flakes, granules or small pieces of finished parts. Method C: Titration method, for plastics in any void-free form. This part of ISO 1183 is applicable to pellets as long as they are void-free.

ISO 16014-2:2003 specifies a method for determining the average molecular mass and the molecular mass distribution of polymers using size-exclusion chromatography (SEC). The average molecular mass and the molecular mass distribution are calculated using a universal calibration curve instead of the conventional calibration curve. This test method is classified as a relative method as described in ISO 16014-1, but the average molecular masses and molecular mass distributions calculated by the method are equal to, or nearly equal to, the absolute values.

ISO 16014-4:2003 specifies a method for determining the average molecular mass and the molecular mass distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at temperatures between 60 °C and 180 °C. The average molecular mass and the molecular mass distribution are calculated from a calibration curve constructed using polymer standards. Therefore this method is classified as a relative method.

ISO 16014-1:2003 specifies a general method for determining the average molecular mass and the molecular mass distribution of polymers using size-exclusion chromatography (SEC). The average molecular mass and the molecular mass distribution are calculated from a calibration curve constructed using polymer standards. Therefore this method is classified as a relative method.

ISO 16014-3:2003 specifies a method for determining the average molecular mass and the molecular mass distribution of polymers using size-exclusion chromatography (SEC) with organic eluent at a temperature lower than 60 °C. The average molecular mass and the molecular mass distribution are calculated from a calibration curve constructed using polymer standards.