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This standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of the National Technical Committee 480 on Furniture of Standardization Administration of China (SAC/TC 480).
Methods for the determination of prohibited substances in furniture products and related materials - Flame retardants
WARNING — Persons using this document should be familiar with normal laboratory practice. This document does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This document describes a gas chromatography-mass spectrometry (GC-MS) method for the determination of polybromobiphenyls (PBBs), polybromobiphenyl ethers (PBDEs) and six organophosphate flame retardants (OPFRs) in furniture products and related materials.
This document is applicable to the determination of polybromobiphenyls, polybromobiphenyl ethers and six organophosphate flame retardants in furniture products and related materials.
2 Normative references
No normative reference is listed in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
polybromobiphenyls (PBBs)
compounds formed by the substitution of one or more bromine atoms for the hydrogen atom on biphenyl, respectively
Note 1 to entry: See Figure 1 for the specific structural formula.
Figure 1 Structure of polybromobiphenyls
Note 2 to entry: According to the number and position of bromine atoms in benzene ring, there are 209 isomers of polybromobiphenyls.
3.2
polybromobiphenyl ethers (PBDEs)
compounds formed by the substitution of one or more bromine atoms for hydrogen atoms in diphenyl ether
Note 1 to entry: See Figure 2 for the specific structural formula.
Figure 2 Structure of polybromobiphenyl ethers
Note 2 to entry: According to the number and position of bromine atoms in benzene ring, there are 209 isomers of polybromobiphenyl ethers.
3.3
organophosphate flame retardants (OPFRs)
organophosphate flame retardants with flame retardant properties such as phosphate, phosphonate, phosphine oxide, phosphorus heterocyclic compounds, polycondensed phosphate and organophosphate
Note: See Table 1 for six organophosphate flame retardants.
4 Principle
4.1 Determination of polybromobiphenyls and polybromobiphenyl ethers
The specimen is ultrasonically extracted with the mixed solvent of n-hexane and dichloromethane, and the extract is purified by solid phase silica gel and concentrated to constant volume, and then subjected to quantitative analysis by gas chromatograph-mass spectrometer (GC-MS).
4.2 Determination of organophosphate flame retardants
The specimen is ultrasonically extracted with the acetone solvent, and after the extract is concentrated to constant volume, it is subjected to quantitative analysis by gas chromatograph-mass spectrometer (GC-MS).
5 Reagents or materials
Unless otherwise specified, only reagents confirmed to be analytical grade shall be used in the analysis.
5.1 n-Hexane.
5.2 Dichloromethane.
5.3 Toluene.
5.4 Acetone: chromatographically pure.
5.5 Methanol: chromatographically pure.
5.6 Organic-phase filtration membrane: with an aperture of 0.45 μm.
5.7 Glass sample bottle: about 50 mL in volume, provided with a cover for seal.
5.8 Silicone solid phase extraction column: with a specification of 500 mg/6 mL, or equivalent; preconditioned with 5 mL of mixed solvent of n-hexane and dichloromethane (5.9) before use to keep the column moist.
Foreword i
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Reagents or materials
6 Apparatus
7 Sample
8 Test procedures
9 Test data processing
10 Precision
Annex A (Informative) Compound names, molecular formulae, qualitative ions and quantitative ions of typical PBBs and PBDEs
Annex B (Informative) GC-MS ion chromatogram of PBB and PBDE standard samples
Annex C (Informative) GC-MS selective ion chromatogram of six organophosphate flame retardant (OPFR) standard samples