ISO 14389:2014 pdf free
ISO 14389:2014 pdf free.Textiles一Determination of the phthalate content一Tetrahydrofuran method
Most of the stock standards may be made in a mixed stock. This saves time and effort when preparing calibration solutions. DINP, DIDP and DIHP have overlapping peaks. It is recommended to make up these stock standard solutions separately, as their calibration solutions have to be made in higher (5x) concentrations than for the other phthalates because of their multi-peak nature. Hence, the higher limit of detection in Annex B.
From the stock standard solutions, prepare at least five appropriate phthalate calibration solutions (example of concentrations at 1 mg/l, 3 mg/l, 15 mg/l, 30 mg/l and 90 mg/l as described in the Table 2), each containing an equal amount of the target phthalates (4.4 through 4.13) and an amount of internal standard (4.3) in a mixture of tetrahydrofuran and the solvent used for the precipitation, mixed by volume at a ratio of 1:2 (33 parts tetrahydrofuran to 66 parts of the other solvent), as shown in Table 2.
Each calibration solution should have a final internal standard concentration of 5 mg/l. Prepare one calibration blank. Analyse the calibration solutions and calibration blank with the GC-MS. Qualitatively analyse the result to ensure proper retention times and the absence of contamination and built up the calibration curve.
A representative test specimen shall be prepared by mixing and cutting pieces from every coated area/part of the textile sample. Cut the representative specimen into small pieces (less than 5 mm in the greatest dimension), homogenize it, and weigh (0,30±0,01) g of these pieces in each of two 40 ml airtight vials (5.2) sealed with a PTFE septum. Ensure that the vials remain airtight in the ultrasonic bath (5.3) throughout the entire extraction process.
Using a volumetric graduated pipette (5.6), add to each vial 10 ml of tetrahydrofuran (4.1) containing 5 mg/l of internal standard (4.3).
If necessary, prepare further diluted solutions using an appropriate volume of a mixture of tetrahydrofuran (4.1) and the solvent used for the precipitation (4.2) mixed by volume at a ratio of 1:2 (33 parts tetrahydrofuran to 66 parts of the other solvent) containing 5mg/l of the internal standard (4.3) and then repeat the analysis.ISO 14389 pdf download.