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SN/T 3512-2013 English PDF (SNT3512-2013)

SN/T 3512-2013 English PDF (SNT3512-2013)

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SN/T 3512-2013: Determination of tetrabromobisphenol A bis(2, 3-dibromopropyl ether) in electrical and electronic equipment. High performance liquid chromatography

This Standard specifies the determination method of high performance liquid chromatography of tetrabromobisphenol A bis (2,3-dibromopropyl ether) in electrical and electronic equipment. This Standard is applicable to the determination of tetrabromobisphenol A bis (2,3-dibromopropyl ether) in plastic parts of electrical and electronic equipment.
SN/T 3512-2013
ENTRY-EXIT INSPECTION AND QUARANTINE INDUSTRY
STANDARD OF THE PEOPLE REPUBLIC OF CHINA
Determination of tetrabromobisphenol A bis (2,3-
dibromopropyl ether) in electrical and electronic
equipment - High performance liquid chromatography
ISSUED ON: MARCH 01, 2013
IMPLEMENTED ON: SEPTEMBER 16, 2013
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Method summary ... 4
4 Reagents and materials ... 4
5 Instruments and equipment ... 5
6 Sample preparation ... 5
7 Analysis steps ... 5
8 Result calculation ... 7
9 Report ... 7
10 Method's linear range, low detection limit, and precision ... 7
Annex A (informative) Liquid chromatogram of tetrabromobisphenol A bis (2,3- dibromopropyl ether) standard solution ... 8
Annex B (informative) Method precision ... 9
Determination of tetrabromobisphenol A bis (2,3-
dibromopropyl ether) in electrical and electronic
equipment - High performance liquid chromatography
1 Scope
This Standard specifies the determination method of high performance liquid chromatography of tetrabromobisphenol A bis (2,3-dibromopropyl ether) in electrical and electronic equipment.
This Standard is applicable to the determination of tetrabromobisphenol A bis (2,3-dibromopropyl ether) in plastic parts of electrical and electronic equipment. 2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682, Water for analytical laboratory use - Specification and test methods
3 Method summary
Use toluene-methanol as extraction solvent to conduct microwave extraction of Tetrabromobisphenol A bis (2, 3-dibromopropyl ether), referred to as BDDP. The extraction solution is purified. Use high performance liquid chromatography to analyze.
4 Reagents and materials
Unless otherwise stated, all reagents used are analytical reagents. Water used is grade one water that complies with GB/T 6682. All solvents for liquid chromatography mobile phases are chromatographically pure and filtered by a 0.45??m filter membrane.
4.1 Toluene: chromatographically pure.
in an extraction can. Accurately pipette 20mL of toluene + methanol (4.5). Seal and place in the microwave extraction instrument (5.2). Rise the temperature to 115??C within 5min. Maintain for more than 15min. Cool to room temperature. If the extraction solution is cloudy and cannot be filtered through a filter, then accurately pipette 2mL of sample extraction solution. Conduct precipitation purification treatment according to 7.2. If the extraction solution is clear, then directly use a 0.46??m nylon filter membrane. Then take part of the filtrate for chromatographic analysis.
7.2 Precipitation purification
In 2mL of extraction solution that is obtained after processing as 7.1, accurately add 6mL of n-hexane or methanol. If precipitation occurs in the solution, it shall conduct centrifuge separation. After removing the serum, set volume to 10mL. Use a 0.46??m nylon filter membrane to filter, then conduct spectrum analysis. 7.3 Chromatographic conditions
Since the test results depend on the instrument used, it is not possible to give general parameters for liquid chromatography. The set parameters shall ensure that the measured component can be effectively separated from other
components during chromatographic determination. The parameters given
below prove to be feasible.
a) Chromatographic column: C18 reverse-phase column [150 ?? 4.6mm
(inner diameter) ?? 5??m] or equivalent;
b) Column temperature: 30??C;
c) Isocratic elution: acetonitrile (4.3) + water (95 + 5, V/V);
d) Detection wavelength: 230nm;
e) Injection volume: 10??L;
f) Flow rate: 0.8mL/min.
7.4 Determination
Inject the samples of standard solution (4.8) and sample solution with equal volume alternately. Determine the nature according to chromatographic
retention time of standard solution. Use external standard method to quantify based on chromatographic peak area.
Analyze the standard solution according to the above analysis conditions (7.3). See Annex A for its typical chromatogram.
7.5 Blank test

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