GB/T 32883-2016 PDF English
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Determination of Hexabromocyclododecanes in Electrical and Electronic Products - High Performance Liquid Chromatography-mass Spectrometry
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GB/T 32883-2016: PDF in English (GBT 32883-2016) GB/T 32883-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 31.020
L 10
Determination of Hexabromocyclododecanes in
Electrical and Electronic Products - High Performance
Liquid Chromatography-mass Spectrometry
ISSUED ON. AUGUST 29, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Terms and Definitions... 4
4 Principle... 5
5 Reagents or Materials... 5
6 Instruments and Equipment... 6
7 Samples... 7
8 Test Procedures... 7
9 Test Data Processing... 9
10 Recovery Rate... 10
11 Precision... 10
Appendix A (informative) High Performance Liquid Chromatogram-mass
Spectrum of Standard Substance of Hexabromocyclododecane... 11
Determination of Hexabromocyclododecanes in
Electrical and Electronic Products - High Performance
Liquid Chromatography-mass Spectrometry
WARNING. personnel applying this Standard shall have practical experience in
formal laboratory work. This Standard does not point out all possible safety
issues. The user is responsible for taking appropriate safety and health
measures and ensuring the compliance with the conditions stipulated by
relevant national laws and regulations.
1 Scope
This Standard specifies the high performance liquid chromatography-mass
spectrometry of determining hexabromocyclododecanes (HBCDDs) in electrical and
electronic products.
This Standard is applicable to the determination of hexabromocyclododecanes
(HBCDDs) in electrical and electronic products. In accordance with this Standard, the
detection limits of three HBCDDs isomers (, , ) are respectively. 30 mg/kg, 20 mg/kg
and 25 mg/kg.
2 Normative References
The following documents are indispensable to the application of this document. In
terms of references with a specified date, only versions with a specified date are
applicable to this document. In terms of references without a specified date, the latest
version (including all the modifications) is applicable to this document.
GB/T 6682-2008 Water for Analytical Laboratory Use - Specification and Test Methods
3 Terms and Definitions
The following terms and definitions are applicable to this document.
3.1 Hexabromocyclododecanes; HBCDDs
Hexabromocyclododecanes is a type of bromine-containing flame retardant. In this
Standard, hexabromocyclododecanes includes three isomers. , , .
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 Instruments and Equipment
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
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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