CEN/TC 248/WG 26 - Methods of test for phthalates

This document specifies a test method for the determination of the content of the preservative agents (biocidal products) 2-phenylphenol (OPP) and triclosan in textile materials and articles composed of textile products, by liquid chromatography.

This document specifies a method for determining the amount of free formaldehyde and formaldehyde extracted partly through hydrolysis by means of an extraction method. The method can be applied for the testing of textile fibres, fabrics or yarns.
NOTE            This method, based on liquid chromatography (LC), is selective and not sensitive to coloured extracts and is intended to be used for precise quantification of formaldehyde.

This document specifies a test method using gas chromatography with a mass selective detector (GC-MS) for detection and quantification of chlorophenols (CPs), which are either freely present or released from salts and esters: pentachlorophenol (PCP), tetrachlorophenol- (TeCP), trichlorophenol- (TriCP), dichlorophenol- (DiCP) and monochlorophenol- (MoCP) isomers. The method is applicable to textile fibres, yarns, fabrics, coated fabrics, printed fabrics, plastic, and wooden parts of textile products (for example buttons).

This document specifies a method of determining phthalates in textiles with gas chromatography–mass spectrometry (GC-MS).
This document is applicable to textile products where there is a risk of the presence of some phthalates.

This document specifies a test method (using gas chromatography, GC) for detection and quantification of selected extractable perfluorinated and polyfluorinated substances in textile materials (fibres, yarns, fabrics) and coated fabrics.
NOTE 1 CEN/TR 16741 defines which materials are applicable to this determination.
A test method (using liquid chromatography, LC) for detection and quantification of selected extractable perfluorinated and polyfluorinated substances is specified in EN 17681-1.
NOTE 2 Both this document and EN 17681-1 are needed for PFOA related substances.
Classes of regulated compounds are listed in Table 2. Classes of other non-regulated compounds that can be determined by this document are defined in Annex C, Table C.1. This document is also applicable for further PFAS substances provided that the method is validated with the additional compounds.
NOTE 3 Commission Delegated Regulation (EU) 2020/784 amending Annex I to the POP Regulation (EU) 2019/1021 as regards the listing of perfluorooctanoic acid (PFOA), its salts and PFOA-related compounds defines among other that “’…PFOA-related compounds’ means the following: … any substances that degrade to PFOA, including any substances (including salts and polymers) having a linear or branched perfluoroheptyl group with the moiety (C7F15)C as one of the structural elements.” To determine whether these are intentionally present it could be necessary to introduce an alkaline hydrolysis method to remove the side-chain from the polymer. According to Commission Regulation (EU) 2021/1297 [7], this applies similarly to C9-C14 PFCAs-related compounds. A future revision of this document will address this aspect.

This document specifies a test method (using liquid chromatography, LC) for detection and quantification of selected extractable perfluorinated and polyfluorinated substances in textile materials (fibres, yarns, fabrics) and coated fabrics.
NOTE 1 CEN/TR 16741 defines which materials are applicable to this determination.
A test method (using gas chromatography, GC) for detection and quantification of selected extractable perfluorinated and polyfluorinated substances is specified in EN 17681-2.
NOTE 2 Both this document and EN 17681-2 are needed for the determination and totalization of the PFOA related substances.
Classes of regulated compounds are listed in Table 2. Classes of other non-regulated compounds that can be determined by this document are defined in Annex C, Table C.1. This document is also applicable for further PFAS substances provided that the method is validated with the additional compounds.
NOTE 3 Commission Delegated Regulation (EU) 2020/784 amending Annex I to the POP Regulation (EU) 2019/1021 as regards the listing of perfluorooctanoic acid (PFOA), its salts and PFOA-related compounds defines among other that “’…PFOA-related compounds’ means the following: … any substances that degrade to PFOA, including any substances (including salts and polymers) having a linear or branched perfluoroheptyl group with the moiety (C7F15)C as one of the structural elements.” To determine whether these are intentionally present it could be necessary to introduce an alkaline hydrolysis method to remove the side-chain from the polymer. According to Commission Regulation (EU) 2021/1297 [7], this applies similarly to C9-C14 PFCAs-related compounds. A future revision of this document will address this aspect.

This document specifies a chromatographic method to determine the amount of short-chain chlorinated paraffins (SCCPs: C10-C13) and middle-chain chlorinated paraffins (MCCPs: C14-C17) in textile articles, especially in polymer of the coated fabrics, prints made of polymer and buttons made of polymer (e.g. polyvinylchloride) by means of solvent extraction and gas chromatography negative ion chemical ionization mass spectrometry (GC-NCI-MS).

This document specifies a test method for the qualification and quantification of organotin compounds. This test method is applicable to all types of materials of textile products.
NOTE    CEN/TR 16741 defines which materials are applicable to this determination.

This document specifies a test method for the qualification and quantification of organotin compounds. This test method is applicable to all types of materials of textile products.
NOTE    CEN/TR 16741 defines which materials are applicable to this determination.

This document specifies a method for determining the pH of the aqueous extract of textiles. The method is applicable to textiles in any form (e.g. fibres, yarns, fabrics).

This document specifies a method to determine the amounts of polycyclic aromatic hydrocarbons (PAH) in components of textile products. This method has been elaborated to achieve a limit of quantification of 0,1 mg/kg.
NOTE A list of relevant materials can be found in CEN/TR 16741 [2].

This document gives a test method for determining the amounts of dimethyl fumarate (DMFu) in textile materials and textile articles. It also includes desiccant sachets that can be present.
The test method is not applicable to metal parts. The materials to which it is applicable are given in CEN/TR 16741:2015, Tables 1 and 3.

This document specifies a method to determine the amounts of extractable dimethylformamide (DMF) in components of textile products containing polyurethane or acrylic.
NOTE   Further information can be found in CEN/TR 16741:2015, Tables 1 and 3 that define which materials are applicable to this determination.

This document describes a testing procedure to determine the rate of lead release from all materials of textile articles.
NOTE   With this test procedure it can be demonstrated that the rate of lead release from such an article or any accessible part of an article, whether coated or uncoated, does or does not exceed 0,05 μg/cm2 per hour, and, for coated articles, that the coating is sufficient to ensure that this release rate is not exceeded for a period of at least two years of normal or reasonably foreseeable conditions of use of the article (Annex XVII of Regulation (EC) No 1907/2006, column 2 of entry 63 paragraph 7, second clause) [5].

This document specifies the method for the determination of extractable alkylphenols (AP) without derivatization step in textile and textile products.

This document specifies the normal phase liquid chromatography (NPLC) separation method for the qualitative and quantitative analysis of extractable alkylphenol ethoxylates (APEO) in textiles and textile products.
This method provides several instrument options for the determination of alkylphenol ethoxylates (APEO) such as normal phase liquid chromatograph with mass spectrometer (NPLC/MS), normal phase liquid chromatograph with fluorescence detector (NPLC/FLD), normal phase liquid chromatograph with charged aerosol detector (NPLC/CAD) and normal phase liquid chromatograph with evaporative light scattering detector (NPLC/ELSD).

This document specifies a method of analysis for determining the content of chlorobenzenes and chlorotoluenes in textile products made of components such as outer fabric, interlining, lining, plastic slide fasteners, plastic buttons, labels, threads and appliques.
The method applies to a mass fraction of 0,1 mg/kg to 10 mg/kg per single isomer. Both higher and lower concentrations can be determined if the mass of the sample is selected accordingly or if appropriate dilutions are made during the analysis.

The effects of synthetic nanoparticles on human health and the environment are still poorly understood and therefore uncertain. In particular, it is unclear in which areas nanoparticles-dose caused negative effects in the organism or in the environment (unknown dose-response relationship). The underlying toxicological mechanisms and possible effects of nanoparticle exposure over long periods of time are poorly understood.
In product advertisements on the Internet and in reports in international journals, especially the functional properties of "nanotextiles" are described. The type of integration of the nanoparticles in textiles is often described only sparsely. Therefore, the present document is based primarily on research studies that include information on the integration of the nanoparticles in the textile material.
The purpose of the present document is to give some guidance on tests to nanoparticle release. The determination of the release of nanoparticles could be performed either through quantification by chemical analysis (5.1), or by determining the linting (5.2), for example.

ISO 14362-1:2017 describes a method to detect the use of certain azo colorants that may not be used in the manufacture or treatment of certain commodities made of textile fibres and that are accessible to reducing agent with and without extraction.
Azo colorants accessible to reducing agent without extraction are those used to colour with pigments or to dye
-      cellulosic fibres (e.g. cotton, viscose),
-      protein fibres (e.g. wool, silk), and
-      synthetic fibres (e.g. polyamide, acrylic).
Azo colorants accessible with extraction are those used to dye man-made fibres with disperse dyes. The following man-made fibres can be dyed with disperse dyes: polyester, polyamide, acetate, triacetate, acrylic and chlorofibre.
The method is relevant for all coloured textiles, e.g. dyed, printed and coated textiles.

Azo colorants that are able to form 4-aminoazobenzene, generate under the conditions of ISO 14362-1, the amines aniline and 1,4-phenylenediamine. The presence of these 4-aminoazobenzene colorants cannot be reliably ascertained without additional information (e.g. the chemical structure of the colorant used) or without a special procedure.
ISO 14362-3:2017 is supplementary to ISO 14362-1 and describes a special procedure to detect the use, in commodities, of certain azo colorants, which may release 4-aminoazobenzene, and that are
-      accessible to reducing agent without extraction, particularly concerning textiles made of cellulose and protein fibres (e.g. cotton, viscose, wool, silk), and
-      accessible by extracting the fibres (e.g. polyester or imitation leather).
For certain fibre blends, in 9.3 and 9.4 (with and without extraction) may need to be applied.
The procedure also detects 4-aminoazobenzene (Solvent Yellow 1), which is already available as free amine in commodities without reducing pre-treatment.
The use of certain azo colorants, which may release, by reductive cleavage of their azo group(s), one or more of the other aromatic amines listed in the Regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorization and Restriction of Chemicals (REACH) as regards Annex XVII, except 4-aminoazobenzene, cannot be determined quantitatively with this method.

ISO 18254-1:2016 describes analyses that are used to detect extractable alkylphenol ethoxylates (nonylphenol ethoxylates and octylphenol ethoxylates) in textile products. This document provides a method that uses Liquid Chromatograph (LC) with Mass Spectrometry (MS) system to detect and quantify alkylphenol ethoxylates of defined ethoxylate chain length.

ISO 17881-1:2016 specifies a test method for determining some brominated flame retardants in textiles by gas chromatography ? mass spectrometry (GC-MS).
The method is applicable to all kinds of textile products.

ISO 17881-2:2016 specifies a test method for determining some phosphorous flame retardants in textiles by high performance liquid chromatography ? tandem mass spectrometry (HPLC-MS/MS).
The method is applicable to all kinds of textile products.
NOTE          For tris (1-aziridinyl) phosphineoxide (TEPA), only unbonded TEPA is extractable.

ISO 16373-1:2015 gives the definition of the colourant classes and the relationship to textile fibres.
It describes some procedures to identify qualitatively the colourant class used in textile material.

This European Standard specifies a procedure for determination of antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), lead (Pb), mercury (Hg), nickel (Ni) in natural and man-made textiles, including coated fabrics and garment components (e.g. buttons, zips, etc.) after extraction with acidic artificial perspiration solution.

This European Standard specifies a procedure for determination of metals, in particular antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), lead (Pb), mercury (Hg), nickel (Ni) in natural and man-made textiles, including coated fabrics and garment components (e.g. buttons, zips, etc.) after microwave digestion.

This Technical Report specifies environmental and health recommendations for textile products (including accessories) with direct skin contact and in the surroundings of the human body.
This Technical Report facilitates the understanding of chemicals with intended uses in the manufacturing of goods in the fields of textile products intended to clothing, interior textiles and upholstery, to comply with the European chemical regulations and recommendations in force in EU.
WARNING: This Technical Report is not intended to substitute the existing regulations. The reader is requested to check the current existing regulation.
By suggesting that the textile market follows the ethos of this Technical Report, and thereby avoiding products containing unwanted substances, human health and the environment are protected in producing, supplying and importing countries to EU.
The distinguishing properties of the chemicals and the processes in which they are used (intended use substances) or they occur (unintended release substances) are described in this technical report.
This Technical Report mentions, when relevant, the existing standardised test methods commonly in use, as well as, the related limit values which are generally accepted.
NOTE 1.   When limit values are given, possible contamination by the external environment and inaccuracy in the measurement of very low concentration may be taken into consideration.
The listed substances of this Technical Report can be categorised in two: one related to intended use, another one related to unintended release.
NOTE 2.   For filling material such as "feather & down", refer to CEN TC 222 and, for other material used in clothing such as leather, refer to CEN TC 309, for toys, refer to CEN TC 252.

ISO 16373-2:2014 specifies the analyses used to detect extractable dyestuffs in textile products, with the extraction performed for all kind of fibres and types of dyestuffs using pyridine/water (1:1). It lists the allergenic and carcinogenic dyestuffs which can be analysed using this method; the lists of dyestuffs are expandable.

ISO 16373-3:2014 specifies a method for the detection and quantitative determination of the presence of carcinogenic dyestuffs in dyed, printed or coated textile products by chromatographic analysis of their extracts.

This document specifies a method using gas chromatography with mass selective detector (GC-MS) for detection and quantification of extractable N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMAC), N-methyl-2-pyrrolidone (NMP) and N-ethyl-2-pyrrolidone (NEP) in filaments and coatings of textile products.

This document specifies a test method, including the degradation of certain side-chain fluorinated polymers during the extraction with simultaneous alkaline hydrolysis, and using liquid chromatography (LC) and tandem mass spectrometry (MS/MS) for identification and quantification of certain per- and polyfluoroalkyl substances (PFAS). The document is applicable to all materials of textile products.
Table 2 indicates a list of target PFAS which can be analysed with this document. PFAS of Table 2 marked with the footnote e) and footnote f) undergo alkaline hydrolysis and only their per- or polyfluorinated degradation products such as PFOA or n:2 fluorotelomer alcohols (n:2 FTOHs, n = 4, 6, 8, 10) can be determined.
By applying the methods outlined in the informative Annex E and Annex F, free n:2 FTOHs, PFOA and non-polymeric PFAS of Table 2 marked with the footnote e) and footnote f), that are not stable to alkaline hydrolysis, can be identified and quantified.
Certain side-chain fluorinated polymers release n:2 FTOHs (n = 4, 6, 8, 10) under the described extraction conditions. Since these side-chain fluorinated polymers can be PFOA or C9-C14 PFCA-related substances restricted by the EU-POPs [1] or EU-REACH [2] regulations, the amounts of released n:2 FTOHs can be used to indirectly assess whether the concentration of the aforementioned side-chain fluorinated polymers exceed limits for PFOA or C9-C14 PFCA-related substances.
This document is also applicable for the determination of further PFAS, provided that the method is validated with the additional substances and that these PFAS are stable to alkaline hydrolysis and dehydrofluorination.

This document specifies a method using headspace gas chromatography and mass selective spectroscopy (HS-GC-MS) for detection and quantification of benzene in components of textile products.

This document specifies a test method using gas chromatography with mass selective detector (GC-MS) for detection and quantification of chlorobenzenes, chlorotoluenes, and α-chlorinated toluenes in fibres, yarns, fabrics, coated fabrics and plastics.

ISO 17751-2:2016 specifies a method for the identification, qualitative, and quantitative analysis of cashmere, wool, other speciality animal fibres, and their blends using scanning electron microscopy (SEM).
ISO 17751-2:2016 is applicable to loose fibres, intermediate products, and final products of cashmere, wool, other speciality animal fibres, and their blends.

This document specifies a test method for the determination of the content of the preservative agents (biocidal products) 2-phenylphenol (OPP) and triclosan in textile materials and articles composed of textile products, by liquid chromatography.

ISO 17751-1:2016 specifies a method for the identification, qualitative, and quantitative analysis of cashmere, wool, other speciality animal fibres, and their blends using light microscopy (LM).
ISO 17751-1:2016 is applicable to loose fibres, intermediate-products, and final products of cashmere, wool, other speciality animal fibres, and their blends.

ISO 14389:2014 specifies a method of determining phthalates in textiles with gas chromatography-mass spectrometry (GC-MS) with mass selective detector. It is applicable to textile products where there is a risk of the presence of some phthalates.

Azo colorants that are able to form 4-aminoazobenzene, generate under the conditions of EN 14362-1 the
amines aniline and 1,4-phenylenediamine. The presence of these 4-aminoazobenzene colorants cannot be
reliably ascertained without additional information (e.g. the chemical structure of the colorant used) or without
a special procedure.
This part of EN 14362 is supplementary to Part 1 and describes a special procedure to detect the use of
certain azo colorants in commodities, which may release 4-aminoazobenzene,
- accessible to reducing agent without extraction, particularly concerning textiles made of cellulose and
protein fibres (e.g. cotton, viscose, wool, silk);
- accessible by extracting the fibres (e.g. polyester or imitation leather).
For certain fibre blends both parts of this standard (without or with extraction) may need to be applied.
The procedure detects as well 4-aminoazobenzene (Solvent Yellow 1) which is already available as free
amine in commodities without reducing pre-treatment.
The use of certain azo colorants, which may release by reductive cleavage of their azo group(s) one or more
of the other aromatic amines listed in the Regulation (EC) No 1907/2006 of the European Parliament and of
the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) as regards
Annex XVII, except 4-aminoazobenzene, cannot be determined quantitatively with this method.

This European Standard describes a procedure to detect the use of certain azo colorants that may not be used in the manufacture or treatment of certain commodities made of textile fibres and that are accessible to reducing agent with and without extraction.
Azo colorants accessible to reducing agent without extraction are those used to dye:
   cellulosic fibres (e.g. cotton, viscose);
   protein fibres (e.g. wool, silk);
   synthetic fibres (e.g. polyamide, acrylic).
Azo colorants accessible with extraction are those used to dye man-made fibres with disperse dyes. The following man-made fibres can be dyed with disperse dyes: polyester, polyamide, acetate, triacetate, acrylic and chlorofibre.
For certain commodities made of cellulose and/or protein fibres blended with man-made fibres it is necessary to extract the dye first.
The method is relevant for all coloured textiles, e.g. dyed, printed and coated textiles.

This standard specifies a test method for taking representative specimens, extraction of phthalates from the
material and determination of phthalates by gas chromatography mass spectrometry.
This standard applies to textiles articles, where there is a possibility of the presence of some phthalates.