ISO 16186:2021 pdf download – Footwear — Critical substances potentially present in footwear and footwear components — Determination of dimethyl fumarate (DMFU).
6.6? Volumetric? flasks 6.7 Gas chromatograph with mass selective detector (GC-MS or GC-MS/MS). 6.8 Amber glass vial, with screw cap that can be tightly sealed (e.g. volume of 10 ml). 6.9 Activated magnesium silicate cartridge. NOTE The two following cartridges have been found suitable. a) Pre-packed cartridge of FL-PR Florisil® 2) (170 µm, 80 Å) 2 g/12 ml. b) Bulk material of Florisil® 100-200 mesh, fine powder. 6.10 Nitrogen evaporator, with conical tubes and with adjustable temperature, suitable for operation up to 40 °C. 7 Sampling The test specimen shall consist of a single material type (made of textile, leather, polymer or other organic material), which is tested separately. Cut the homogenous material samples into pieces of about 3 mm to 5 mm edge length. NOTE 1 Up to three test specimens (of equal mass) of the same material type can be tested together, taking into consideration the limits of detection and quantification. NOTE 2 Desiccant can be a source of DMFU contamination of the footwear. Desiccant samples can be used without any processing. 8 Procedure 8.1 Standard procedure Weigh (1,0 ± 0,1) g of the sample in a glass vial (6.2), record the mass to the nearest 1 mg, add 0,1 ml of the solution of internal standard working solution (5.6.2) and 9,9 ml of acetone (5.1), and seal the vial. Extract the sample at (60 ± 5) °C for (60 ± 5) min in an ultrasonic bath (6.3). WARNING — Do not open the vial before cooling as the content can be under pressure. After cooling to below at least 27 °C, decant the solution and, if necessary, reduce to 1,0 ml under a gentle stream of nitrogen (6.10). Filter this solution through a PTFE membrane filter (6.4). Transfer an aliquot of the extract to a GC vial (6.5) and seal with a cap. 8.2 Procedure for complex matrix 8.2.1 Extraction Weigh (1,0 ± 0,1) g of the sample in a glass vial (6.2), record the mass to the nearest 1 mg, add 0,1 ml of the solution of internal standard (5.6.2) and 9,9 ml of acetone (5.1), and seal the vial. Extract the sample at (60 ± 5) °C for (60 ± 5) min in an ultrasonic bath (6.3).