T/ZFB 0006-2020 Determination of Chlorphenolphthalein in Textiles by Gas Chromatography-Mass Spectrometry Method

Scope

Scope: This method specifies the determination of 19 chlorophenols in textiles using a gas chromatograph (GC-MSD) equipped with a mass selective detector. This method is applicable to all types of textile materials and products; Main technical content: 6.1 Extraction: Take representative samples, cut them into pieces smaller than 5 mm × 5 mm, and mix them well. Weigh out 1.0 g (accurate to 0.01 g) of the sample and place it in a 100 mL conical flask. Add 80 mL of potassium carbonate solution (5.5), extract for 20 minutes in an ultrasonic generator, filter, and combine the extract with the residue after ultrasonic extraction for 10 minutes with 30 mL of potassium carbonate solution. 6.2 Acetylation: Place the filtrate in a 150 mL separatory funnel, add 2 mL of acetic anhydride (5.2), shake for 2 minutes, accurately add 5 mL of n-hexane (5.1), shake for 2 minutes, and let it stand for 5 minutes. Discard the lower layer. Add 50 mL of sodium sulfate solution to the n-hexane phase, discard the lower layer, and transfer the n-hexane phase to a 10 mL centrifuge tube. Add 5 mL of sodium sulfate solution (5.6), shake for 1 minute, let it separate into layers, and centrifuge if necessary. Take the upper organic phase for instrument analysis. 6.3 Preparation of standard working solutions: Accurately transfer a certain volume of a suitable concentration of mixed standard working solutions to a 150 mL separatory funnel, dilute it to about 110 mL with potassium carbonate solution (5.5), add 2 mL of acetic anhydride (5.2), and follow the steps in 6.2. 6.4 Determination 6.4.1 Gas chromatography-mass spectrometry conditions: Since the test results depend on the instrument used, no general parameters for chromatographic analysis can be provided. The following data have been proven to be suitable for the test: a) Chromatographic column: HP-5MS (30 m × 0.25 mm × 0.25 μm) or equivalent; b) Column temperature: Maintain at 50 °C for 2 minutes, then increase to 220 °C at 30 °

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