GB/T 32883-2016Determination of hexabromocyclododecanes in electrical and electronic products - High performance liquid chromatography-mass spectrometry (English PDF)

3.1 Hexabromocyclododecanes; HBCDDs

Hexabromocyclododecanes is a type of bromine-containing flame retardant. In this

Standard, hexabromocyclododecanes includes three isomers: alpha, beta, gamma.

such as: 10 mL and 100 mL, etc.

5.13 Syringe filter

0.22 µm, two-phase membrane.

5.14 Syringe

5 mL.

5.15 Scale centrifuge tube: 10 mL, with a screw cap, containing poly-fluoroethylene

gasket.

5.16 Sample tube

30 mL, with a screw cap, containing poly-fluoroethylene gasket.

5.17

Cellulose sleeve.

5.18 Filter paper

use toluene to pre-extract for above 3 times; dry it for later use.

5.19 Zeolite

use toluene to pre-extract for above 3 times; dry it for later use.

5.20 Solid phase extraction column: C18, 500 mg/6 mL; or others with equivalent

performance.

6.1 High performance liquid chromatograph-mass spectrometer, equipped with

electrospray ion source (ESI source).

6.2 Crushing device: including cutting machine or scissors, grinding machine and

freezing-crushing facility, etc. It is mainly used for crushing samples.

6.3 18-mesh standard sieve (sieve diameter

1 mm).

6.4 Electronic analytical balance

division value is 0.1 mg or above.

6.5

Soxhlet extraction device, with a condenser.

6.6

Heating device used to heat up the flask used in Soxhlet extraction device.

6.7

Nitrogen blowing instrument.

6.8

Vortex miser.

6.9 Ultrasonic instrument: ultrasonic frequency 40 kHz, ultrasonic function 400 W; or

others with equivalent performance.

6.10 Centrifuge

5,000 r/min and 12,000 r/min.

6.11

Fast solvent extraction instrument.

6.12 Heating furnace

heat up to above 400 °C.

gentle nitrogen to blow-dry it. Use methanol-water solution (5.8) to reach a constant volume of 1 mL. Conduct vortex oscillation for 1 min. Use syringe filter to filter it, or, centrifuge it at 12,000 r/min for 5 min. Take the filtrate or supernatant for later testing. If the concentration of the analyte in the sample exceeds the range of the standard curve, conduct appropriate dilution, then, determine it.

b) Ultrasonic-assisted extraction: weigh-take 0.1 g of the above-mentioned mixed sample, accurate to 0.001 g. Use filter paper (5.18) to wrap it, then, place it in a centrifuge tube (5.15); add 4 mL of toluene (5.5). In an ultrasonic instrument (6.9), conduct ultrasonic extraction for 15 min, then, centrifuge it at

5,000 r/min (6.10) for 5 min. Transfer the supernatant to the sample tube (5.16). Repeat the above steps twice, then, combine the three extracts in the same sample tube (5.16); reach a constant volume in a 100 mL volumetric flask. Before the detection, take an appropriate amount (for example, 1 mL) of the extract in a nitrogen blowing instrument; use gentle nitrogen to blow- dry it. Use methanol-water solution (5.8) to reach a constant volume of 1 mL.

Conduct vortex oscillation for 1 min. Use syringe filter to filter it, or, centrifuge it at 12,000 r/min for 5 min. Take the filtrate or supernatant for later testing. If the concentration of the analyte in the sample exceeds the range of the standard curve, conduct appropriate dilution, then, determine it.

c) Fast solvent extraction: weigh-take 0.1 g of the crushed sample, accurate to

0.001 g. Use filter paper (5.18) to wrap it, then, place it in the extraction tank to conduct fast solvent extraction (6.11). The extractant is acetone-n-hexane solution (5.7). The sample cell temperature is 120 °C; the pressure is 10.3

MPa; the heating time is 5 min; the static extraction time is 10 min; the nitrogen-blowing time is 100 s. The number of cycles is 3 times; the volume of the sample cell rinsing is 20%. After the extraction is completed, reach a constant volume in a 100 mL volumetric flask. Before the detection, take an appropriate amount (for example, 1 mL) of the extract in a nitrogen blowing instrument; use gentle nitrogen to blow-dry it. Use methanol-water solution (5.8) to reach a constant volume of 1 mL. Conduct vortex oscillation for 1 min.

Use syringe filter to filter it, or, centrifuge it at 12,000 r/min for 5 min. Take the filtrate or supernatant for later testing. If the concentration of the analyte in the sample exceeds the range of the standard curve, conduct appropriate dilution, then, determine it.

During the sample analysis, simultaneously conduct blank test and parallel test.

8.2 Determination by High Performance Liquid Chromatography-mass

Spectrometry

Different instruments being used might lead to different optimal analysis conditions.

Hence, it is impossible to provide general parameters suitable for all determinations by