Leather and fur - Chemical test -Determination of fire retardants
1 Scope
This document describes the test methods for the determination of fire retardants in leather and fur by GC-MS and LC-MS/MS.
This document is applicable to the determination of 29 fire retardants (see Annex A) in leather and fur and their products.
2 Normative references
The following documents contain requirements 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 (including any amendments) applies.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 39364 Leather - Chemical, physical, mechanical and fastness tests - Sampling location
QB/T 1267 Fur - Chemical, physical and mechanical and fastness tests - Sampling location
QB/T 1272 Fur - Preparation of chemical test samples
QB/T 2716 Leather - Preparation of chemical test samples
3 Terms and definitions
No terms and definitions are listed in this document.
4 GC-MS - Method A
4.1 Principles
Ultrasonic extraction is carried out with the mixture of dichloromethane and n-hexane, after the extraction solution is purified by C18 solid phase extraction column, it is separated and determined by GC-MS method and quantified by internal standard method.
This method is applicable to the determination of 10 polybrominated biphenyls and 10 Poly Brominated Diphenyl Ethers fire retardants (see Table A.1) in leather and fur.
4.2 Reagents and materials
4.2.1 Unless otherwise specified, analytical grade reagents shall be used.
4.2.2 Dichloromethane, chromatographically pure.
4.2.3 N-hexane: chromatographically pure.
4.2.4 Mixed solution of dichloromethane and n-hexane: dichloromethane (4.2.2) and n-hexane (4.2.3) are mixed with equal volume;
4.2.5 Fire retardant standards are detailed in Table A.1.
4.2.6 Decachlorobiphenyl (internal standard), prepared with n-hexane (4.2.3) in appropriate concentrations as required.
4.2.7 Mixed standard solution: accurately weigh an appropriate amount of each fire retardant standard product (4.2.5, accurate to 0.01mg), dissolve it with n-hexane (4.2.3) and prepare a mixed standard solution of a certain concentration (including internal standards).
Contents
Foreword I
1 Scope
2 Normative references
3 Terms and definitions
4 GC-MS - Method A
5 LC-MS/MS - Method B
6 Test report
Annex A (Informative) Chinese and English names, abbreviations, relative molecular mass and CAS No. of fire retardant standards
Annex B (Informative) GC-MS reference conditions and quantitative limits of fire retardant standards and internal standards
Annex C (Informative) SIM figure of target compound
Annex D (Informative) MRM figure of target compound