GB/T 29786-2013Determination of phthalates in electrical and electronic equipment - Gas chromatography-mass spectrometry (English PDF)

7.1.2 Ultrasonic extraction

WEIGH 0.2 g of sample (to the nearest 0.1 mg); PLACE it in a 50 mL

Erlenmeyer flask; ADD 30 mL of ethyl acetate (4.1); PERFORM ultrasonic extraction for 20 min. TRANSFER the extract to a 100 mL round-bottomed flask;

KEEP the sample in the Erlenmeyer flask; and then ADD 30 mL of ethyl acetate and PERFORM ultrasonic extraction for 20 min. REPEAT the above steps for a total of 3 extractions. COMBINE the extracts; CONCENTRATE the extracts with a rotary evaporator (5.4) to about 4 mL; TRANSFER to a 10 mL volumetric flask. WASH with 5 mL of ethyl acetate; COMBINE the washing solution into the volumetric flask; DILUTE with ethyl acetate to constant volume. After filtering with organic phase filter membrane (5.5), the filtrate is to be tested. For

GC-MS (5.1) determination.

7.2 Determination

7.2.1 Reference conditions for gas chromatography-mass spectrometry

a) Chromatographic column. DB-5MS capillary column 30 m × 0.25 mm ×

0.25 µm, or equivalent;

b) Sample inlet temperature. 280 °C;

c) Interface temperature. 290 °C;

d) Heating program. the initial temperature is 60 °C, maintain for 1 min;

increase to 280 °C at 30 °C/min, maintain for 10 min;

e) Ion source temperature. 230 °C;

f) Carrier gas. helium (4.5), flow rate of 1.2 mL/min;

g) Sample injection mode. splitless injection, open the valve after 1 min;

h) Ionization method. electron ionization source (EI);

i) Electron energy. 70 eV;

j) Measurement method. scan (scan range of 50 amu ~ 500 amu) for qualitative analysis; selective ion monitoring (SIM) for quantitation.

7.2.2 Qualitative and quantitative analysis

Analyze according to the above conditions. According to the retention time of the chromatographic peak and refer to the qualitative ions of phthalates in

Annex B for qualitative analysis; refer to the quantitative ions in Annex B, using

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