GB/T 33345-2016Determination of short chain chlorinated paraffins in electrical and electronic products—Gas chromatography-mass spectrometry (English PDF)

3.1 6.3 Soxhlet extraction device, equipped with condenser and heating device, or

use an automatic Soxhlet extraction device.

8.1 Sample extraction

Use Soxhlet extraction method to process the sample, using the steps as follows.

a) Weigh 0.5 g of the crushed sample (accurate to 0.0001 g); place it in the cellulose filter paper cartridge after extraction and washing; then place it in the installed Soxhlet extraction device;

b) Add about 50 mL of toluene (5.2) to the Soxhlet extraction device; the total number of extraction cycles is not less than 60;

c) Concentrate the extract in [8.1.b)] by rotary evaporation in a water bath at 80 °C to about 1 mL. If the extract is more viscous, it can be processed directly according to [8.2.a)]; otherwise it can be transferred to a 10.0 mL volumetric flask; the distillation flask shall be rinsed at least 3 times by the use of n-hexane (5.1). The rinse solution can be combined into a 10.0 mL volumetric flask. After making the volume of n-hexane (5.1) to the mark, follow [8.2.b)] to process it.

It is recommended that no sample is added during the extraction and cleaning process of the cellulose filter paper cartridge; the operation shall be performed according to the extraction procedure [8.1.b)].

Depending on the instrument used, the optimal analysis conditions may also be different, so it is impossible to give general parameters for gas chromatography-electron capture negative chemical ion source analysis. The set parameters shall ensure the effective separation and determination of the tested components. The parameters given below have proven to be feasible.

a) Chromatographic column. 15 m × 0.25 mm (inner diameter) × 0.1 µm (film thickness), the stationary phase is 5% phenyl, 95% dimethyl polysiloxane quartz capillary column or equivalent;

b) Inlet temperature. 280 °C;

c) Chromatographic column temperature program. Hold at 100 °C for 1 min; then increase the temperature in a programmed manner to 300 °C at 20 °C/min; hold for 9 minutes;

d) Transmission line temperature. 300 °C;

e) Carrier gas. Helium, which has a purity greater than or equal to 99.999%;

f) Carrier gas flow rate. 1 mL/min;

g) Injection volume. 1.0 µL;

h) Sample injection mode. Adopt splitless sample injection; switch to split mode after 1 min (split ratio 20.1);

i) Ion source temperature. 160 °C;

j) Reagent gas. Methane;

k) Reagent gas flow rate. 2.0 mL/min;

l) Ionization method. Electron capture negative chemical source ionization;

m) Determination method. Select ion scan mode, see Table 1 for qualitative and quantitative ions;

n) Solvent delay. 5 min.

A.1 Gas chromatography electron impact mass spectrometry conditions

Depending on the instrument used, the optimal analysis conditions may also be different, so it is impossible to give general parameters of gas chromatography electron bombardment mass spectrometry. The set parameters shall ensure the effective separation and determination of the tested components. The parameters given below have proven to be feasible.

a) Chromatographic column. 15 m × 0.25 mm (inner diameter) × 0.1 µm (film thickness), the stationary phase is 5% phenyl, 95% dimethyl polysiloxane quartz capillary column or equivalent;

b) Chromatographic column temperature program. keep at 100 °C for 1 min, then program to raise temperature to 300 °C at 20 °C/min, keep it for 5 min;

c) Sample inlet temperature. 280 °C;

d) Chromatography-mass spectrometry interface temperature. 300 °C;

e) Ion source and its temperature. Electron bombardment ion source, temperature. 250 °C;

f) Carrier gas. Helium, with a purity greater than or equal to 99.999%, 1 mL/min;

g) Ionization method. EI;

h) Ionization energy. 70 eV;

B.1 Gas chromatography conditions

Depending on the instrument used, the optimal analysis conditions may also be different, so it is impossible to give general parameters of gas chromatography.

The set parameters shall ensure the effective separation and determination of the tested components. The parameters given below have proven to be feasible.

a) Chromatographic column. 30 m × 0.25 mm (inner diameter) × 0.25 µm (film thickness), the stationary phase is 5% phenyl, 95% dimethyl polysiloxane quartz capillary column or equivalent;

b) Chromatographic column temperature program. keep at 100 °C for 3 min; then program to raise temperature to 300 °C at 25 °C/min; keep for 10 min;

c) Sample inlet temperature. 280 °C;

d) Carrier gas. nitrogen, purity greater than or equal to 99.99%, 1 mL/min;

e) Sampling mode. Pulsed splitless sample injection;

f) Sample injection volume. 1.0 µL;

g) Detector and its temperature. Electron capture detector (ECD), temperature at 180 °C.

B.2 Qualitative and quantitative analysis by gas chromatography

Standard solution preparation. Use n-hexane (5.1) as the solvent, to prepare […]