T/ZFB 0005-2020 The determination of tri(2-chloroethyl) phosphate in textiles

Scope

Scope: This standard specifies the method for detecting phosphoric acid tri(2-ethylhexyl) ester in textile products using gas chromatography-mass spectrometry (GC-MS). This standard applies to the determination of organic phosphorus flame retardant phosphoric acid tri(2-ethylhexyl) ester in textile materials and products. Main technical content: 5.1 Preparation of standard solutions 5.1.1 Standard stock solution: Prepare a standard stock solution of phosphoric acid tri(2-ethylhexyl) ester with acetone (4.2) as the solvent, with a concentration of 1000 μg/mL. 5.1.2 Standard working solution: Prepare a series of standard working solutions with acetone as the solvent and dilute them to appropriate concentrations as needed. Select at least 5 standard working solution concentrations to plot a working curve and analyze by GC-MS. Note: The validity period of the standard stock solution does not exceed 12 months, and that of the standard working solution does not exceed 3 months. Store at 0–4 °C. 5.2 Sample preparation Take representative samples, cut them into approximately 5 mm × 5 mm pieces, mix them well, and weigh 1.0 g (accurate to 0.01 g) of the sample with a balance (3.3). Place it in a 40 mL glass extraction bottle (4.3) with a screw cap, add 10 mL of acetone, and ensure the bottle is sealed during ultrasonic extraction. Place the bottle in an ultrasonic generator (3.2) at (40 ± 2) °C for 40 minutes. Remove the bottle, transfer the extract to a 25 mL volumetric flask. Add 10 mL of acetone to the residue and ultrasonicate for another 10 minutes under the same conditions. Combine the extracts. Wash the residue with a suitable amount of acetone and transfer it to a volumetric flask for final dilution. Filter the extract through an organic filter membrane (4.4) and analyze by GC-MS (3.1). 5.3 Determination 5.3.1 Gas chromatography-mass spectrometry conditions Since the test results depend on the instrument used, it is not possible to provide univers

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