BS EN 17131 pdf free download
BS EN 17131-2019 pdf free download.Textiles and textile products – Determination of dimethylformamide (DMF), method using gas chromatography.
5.4.2 Internal standard – Working solution (200 mg/I)
The solution is prepared by 1:5 dilution of the stock solution (5.4.1) with methanol (5.3).
5.4.3 Target compound – Stock solution (1 000 mg/1)
Weigh 10 mg of DMF (5.1), with an accuracy of 0,1 mg into a 10 ml volumetric flask, fill up 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.
5.4.4 Target compound – Working solution (200 mg/I)
The solution is prepared by 1:5 dilution of the stock solution (5.4.3) with methanol (5.3).
6 Equipment
The usual laboratory equipment and laboratory glassware, according to EN IS0 4787, shall be used, in addition to the following:
6.1 Analytical balance with a precision of at least 0,1 mg
6.2 Glass vial, with a screw cap that can be tightly sealed (eg volume of 20 ml),
6.3 Ultrasonic bath with adjustable temperature suitable for operation at about70 °c,
6.4 PTFE-membrane filter, pore width 0,45 um,
6.5 GC vial, capped (eg volume of2 ml),
6.6 Amber glass vial, with a screw cap that can be tightly sealed (eg volume of 10 ml),
6.7 Micropipettes,
6.8 Gas chromatograph with mass selective detector (GC-MS),
7 Sampling
7.1 Samples
DMF is volatile and care should be taken to minimize loss. It is recommended that samples are individually wrapped in aluminium foil before shipping.
7.2 Preparation of test specimens
If possible, sampling is carried out according to EN IS0 5089. Samples of materials are cut into pieces of about 0,3 cm to 0,5 cm edge length.
NOTE
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 quantiication.
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土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.
9 Expression of results
Plot a calibration graph of the response against the known standard concentration (corrected for the response for the internal standard). From the calibration graph, interpolate the concentration of DMF in ug/ml (Ps).
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.