EN 15777:2009 – Textiles – Test method for phthalates
1 Scope
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.
2 Terms and definitions
For the purposes of this European Standard, the following terms and definitions apply.
2.1
blank
application of the method without test specimen
2.2
plasticized or softened materials
plastic material (coating, pigment print binder, etc) that is treated with chemicals (for this specific standard they are phthalates) to make it more flexible
2.3
overall treated textiles
textiles with a continuous finish, coating or print
2.4
locally treated textiles
textile with a discontinuous finish, coating or print
2.5
representative specimen
specimen obtained by mixing pieces of all the different treated parts and colours
3 Preparation of the test specimens
Remove the untreated mass of the specimen if possible (see Annex A). If the untreated mass cannot be removed, see 5.4.
Use a scalpel or other appropriate cutting tool to cut two representative specimens into small pieces.
4 Apparatus and reagents
4.1 Apparatus
4.1.1 Balance (resolution of 1 mg).
4.1.2 150 ml flask.
4.1.3 Soxhlet extractor with siphon cup of approximately 20 ml.
4.1.4 Soxhlet cellulose thimble, approximately 15 mm in diameter and 50 mm height.
4.1.5 Water-cooled condenser.
4.1.6 Spark proof heating mantle/water bath.
4.1.7 Steam bath or rotary evaporator.
4.1.8 Calibrated volumetric flasks of suitable volume.
NOTE Avoid direct contact between the samples and glassware and/or equipment to be used to minimize crosscontamination. Glassware, after washing, should have an extra rinse with 0,1 N nitric acid and finally with acetone, acetone/methanol and/or cyclohexane. Dry at 110 °C (1 h). Beware, the vapour of the organic solvents are highly flammable, especially at high temperature! Allow glassware to cool down before use.
4.1.9 Gas chromatography with mass selective detector (GC-MS).
4.2 Reagents (analytical grade)
4.2.1 n-Hexane, CAS No. 110-54-3.
4.2.2 Di-isononyl phthalate (DINP), CAS No. 28553-12-0 or 68515-48-0.
4.2.3 Di-(2-ethylhexyl) phthalate (DEHP), CAS No. 117-81-7.
4.2.4 Di-n-octyl phthalate (DNOP), CAS No. 117-84-0.
4.2.5 Di-iso-decyl phthalate (DIDP), CAS No. 26761-40-0 or 68515-49-1.
4.2.6 Butyl benzyl phthalate (BBP), CAS No. 85-68-7.
4.2.7 Di-butyl phthalate (DBP), CAS No.84-74-2.
4.2.8 Dicyclohexyl phthalate (DCHP), CAS no.84-61-7 – Internal Standard.
EN 15777:2009 – Textiles – Test method for phthalates