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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 - Azo dyes
WARNING — Persons using this document should be familiar with normal laboratory practice. Aromatic amines have been classified as substances known or suspected to be human carcinogens. 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 the methods for the determination of 24 prohibited azo dyes in furniture products and related materials.
This document is applicable to the determination of 24 prohibited azo dyes in furniture products and related materials.
2 Normative references
The following documents contain provisions which, through reference in this text, constitute provisions 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 Terms and definitions
No terms and definitions are listed in this document.
4 Principle
In the citrate buffer solution, the azo dyes in the specimen are reduced to the corresponding aromatic amine intermediate by sodium hydrosulfite. Aromatic amines produced by reductive cleavage is extracted by a Kieselguhr column for liquid-liquid extraction into tert-butyl methyl ether, then concentrated and dissolved with appropriate solvent to the scale for gas chromatography-mass spectrometry (GC-MS) analysis. If necessary, choose another method or more methods to confirm the isomers.
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5 Reagents or materials
Water used shall meet the requirements for Grade 3 water as specified in GB/T 6682.
5.1 Methanol, chromatographically pure.
5.2 N-hexane: chromatographically pure.
5.3 Ethyl acetate: Chromatographic grade.
5.4 Tert-butyl methyl ether: chromatographically pure.
5.5 Citrate buffer solution, 0.06 mol/L, pH＝6, preheated to (70±5)℃. Dissolve 12.526g of citric acid and 6.320g of sodium hydroxide in water and dilute to 1,000mL.
5.6 Sodium hydrosulfite, with purity ≥ 87%.
5.7 Aqueous solution of sodium hydrosulfite, 200mg/mL. Dissolve 10g of sodium hydrosulfite (5.6) in water and dilute to 50mL. The solution shall be used immediately after being stored in a closed vessel for 1 h.
5.8 20% sodium hydroxide-methanol solution, prepared by dissolving 20g of sodium hydroxide in 100mL of methanol.
5.9 Aromatic amine standards, with the highest purity available; see Annex A.
5.10 Aromatic amine (5.9) stock solution, 1,000mg/L, using methanol or other suitable solvents.
5.11 Aromatic amine standard working solution, with aromatic amine mass content of 20μg/mL, prepared using aromatic amine stock solution (5.10) or aromatic amine standards (5.9) depending on the analytical method.
5.12 Kieselguhr, porous granulated Kieselgur, burned at 600℃ for 4h, cooled and stored in a dryer for later use.
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) Chemical names, CAS No. and characteristic ions of 24 prohibited aromatic amines
Annex B (Informative) Pretreatment method of polyester specimens
Bibliography
