BS EN 17131:2019 pdf free.Textiles and textile products – Determination of dimethylformamide (DMF), method using gas chromatography.
4 Principle of method The sample is cut into small pieces and extracted with methanol, in a sealed vial at 70°C, in an ultrasonic bath. An aliquot of the extract is analysed using a gas chromatograph with mass selective detector (GC-MS). 5 Reagents Unless otherwise specified, analytical grade chemicals shall be used. 5.1 Dimethylformamide (DMF), CAS Number: 68-12-2, highest available defined purity standard 5.2 Dimethylformamide – d7 (DMF-d7), CAS Number 4472-41-7, highest available defined purity standard 5.3 Methanol, CAS Number 67-56-1 5.4 Stock solutions 5.4.1 Internal standard – Stock solution (1 000 mg/1) Weigh 10 mg of DMF-d7 (5.2), with an accuracy of 0,1 mg, into a 10 ml volumetric flask, fill to the mark with methanol (5.3) and mix. Transfer the content into an amber 10 ml vial with cap (6.6) and keep in a refrigerator at about6 °C.8 Procedure 8.1 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 1 ml of the solution of internal standard (5.4.2) and 9 ml of methanol (5.3), and seal the vial. Extract the sample at(70+5)°Cfor 1 h士5 min in an ultrasonic bath. WARNING – Do not open the vial before cooling as the contents may be under pressure. After cooling to 27 °C, or below, filter this solution through a PTFE membrane filter (6.4). Transfer an aliquot of the extract to a GC-MS vial (6.5) and seal with a cap. 8.2 Determination with GC-MS 8.2.1 Preparation of the calibration solutions Prepare at least 3 calibration solutions of DMF, including internal standard, from the working solutions (5.4.2 and 5.4.4), in methanol (5.3), at suitable concentrations for the analysis. 8.2.2 Determination with GC-MS Determine the DMF extracted in 8.1 by GC-MS (6.8). An example of chromatographic conditions is given in Annex A.10 Test report The test report shall include at least the following: a) reference to this test method, i.e. EN 17131:2019; b) date of the test; c) all details necessary for complete identification of the sample tested;
d) condition of sample receipt and storage before the test; e) result of the extracted dimethylformamide, in mg/kg; f) any deviation from the given procedure.BS EN 17131 pdf download.