BS/EN 17137-2018 pdf download.Textiles – Determination of the content of compounds based on chlorobenzenes and chlorotoluenes.
This BS/EN 17137 specifies a method of analysis for determining the content of chlorobenzenes and chiorotoluenes 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.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at httpj/www.electroyedia,orgJ
— ISO Online browsing platform: available at http://www.iso.org/obp
component
Individual part (one material) of the textile product sample
3.2
composite test specimen
test specimen composed from various sub-test specimens of components
4 Principle
The cut test specimen is extracted via ultrasonication in a closed vessel using dichloromethane.
Interfering particles and fibres are removed by filtering through membrane filters. Without additional
purification, the extract is analysed to determine the content of chlorobenzenes and chiorotoluenes by
GC-MS with selected ion mode, using an internal standard for quantification.
5 Apparatus
5.1 Standard laboratory equipment.
5.2 Glass vials with tight closure.
NOTE Vial volumes 0140 ml to 100 ml have been found suitable.
5.3 UltrasonIc bath for extraction.
5.4 Analytical balance, resolution of at least 0,000 1 g.
5.5 Syringes with Luer Lock, 2 ml, with disposable syringe filters, made of polytetrafluoroethylene (PTFE) membrane.
NOTE Pore size of 0,45 pm has been found suitable.
5.6 Gas chromatograph with mass selective detector (MSD).
6 Reagents
6.1 Dichloromethane for residue analysis (analytical grade).
6.2 Reference substances Reference substances are listed in Table 1.
7 Procedure
7.1 Sampling and test specimen preparation
The test specimen is usually a composite test specimen of sub-test specimens of different components. Attention has to be paid to take equivalent masses of the different selected coniponents. For multicoloured and differently coloured products all available colours shall be selected and be tested.
Up to four colours may be tested together.
In order to gather four colours, the following rules shall be applied. The rules have been listed in order of preference:
— select the four colours from the same part of the textile article;
— if the four colours do not come from the same part of the textile article, select these four colours from textile parts made of the same type of textile fibre.
Each colour shall have approximately the same mass in order to obtain the total mass of 2 g.
lithe rules cannot be applied (e.g. due to a complex printed pattern, plastic buttons), the sampling description of the selected test specimens shall be reported.
The test specimens are cut into pieces (approx. 5 mm wide) and stored in sealed glass vials until further processing.
7.2 Extraction
(2,0 ± 0,1) g of the cut test specimen are weighed in a vial, and overlaid with 20 ml dichloromethane. After adding 200 jil internal standard solution (e.g. at concentration of 10 ig/ml), the test specimen is extracted for (30 ± 1) mm in an ultrasonic bath (starting at laboratory ambient temperature).
7.3 Filtration
1 ml of the extract is taken with a disposable syringe and cleaned of interfering particles and fibres with the help of membrane filters. After filtration, the extract is transferred into a vial.
7.4 Gas chromatographic determination
The substances of the extract arc separated on a capillary column, and analysed using a mass-selective detector in selected ion mode (SIM).
Examples of instrumental parameters are shown in Annex A.
7.5 Calibration
Individual stock solutions are prepared for calibration of the reference substances (e.g. 10 mg to 10 ml of dichloromethane, mass concentration 3 = 1 mg/mI). Then a mixed standard is prepared (e.g. 1 ml of each stock solution to 100 ml of dichioromethane, mass concentration = 10 ig/ml). This mixed calibration standard is used to prepare calibration solutions of various concentrations (e.g. 10, 50. 100, 200. 400, 600,800, 1 000 ng/mI). Finally 1 ml of each individual calibration solution is mixed with 10 p1 of the internal standard solution (e.g. at concentration of 10ig/ml) and analysed.
7.6 Calculation and expression of the results
The concentrations of chlorobenzenes or chlorotoluenes arise as a mass fraction in pg/mI of the following formula:BS/EN 17137-2018 pdf download.