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GB/T 24279 consists of the following parts, under the general title Textiles - Determination of certain flame retardants:
——Part 1: Brominated flame retardants;
——Part 2: Phosphorus flame retardants.
This is Part 1 of GB/T 24279.
This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This part replaces GB/T 24279-2009 Textiles - Determination of banned retardant and the following main technical changes have been made with respect to GB/T 24279-2006:
——The standard name is modified;
——The types of tested retardant targets are adjusted;
——“Normative references” is deleted;
——Pre-treatment extraction method is modified;
——Quantitative method is changed from external standard method to internal standard method;
——Three annexes are deleted and informative Annex A Test parameters by GC-MS is added.
This part, by means of translation, is identical to ISO 17881-1:2016 Textiles - Determination of certain flame retardants - Part 1: Brominated flame retardants.
The following editorial changes are made in this part:
——Note is added in 5.1.3 to provide information on the preservation conditions of standard solution for ease of use;
——In informative Annex A, chromatograms are added for convenience of operation and the determination limit of individual tested substances is adjusted.
This part was proposed by the China National Textile and Apparel Council.
This standard is under the jurisdiction of National Technical Committee on Textiles of Standardization Administration of China (SAC/TC 209).
The previous edition of this part is as follows:
——GB/T 24279-2009.
Textiles - Determination of certain flame retardants - Part 1: Brominated flame retardants
Warning: It has been assumed in the drafting of this part that the execution of its provisions is entrusted to appropriately qualified and experienced people. This part does not address all of the safety problems, The user is responsible for taking proper safety and health measures and ensuring conformance to the requirements specified in relevant national laws and regulations.
1 Scope
This part of GB/T 24279 specifies a test method for determining some brominated flame retardants in textiles by gas chromatography – mass spectrometry (GC-MS).
The method is applicable to all kinds of textile products.
2 Principle
The flame retardants are extracted from textile specimen by ultrasonic generator with toluene. The flame retardants in the specimen are identified by GC-MS and quantified by using internal standard method.
3 Reagents
Unless otherwise specified, use only reagents of recognized analytical grade.
3.1 Monobromobiphenyl (MonoBB), CAS no. 2052-07-5.
3.2 Dibromobiphenyl (DiBB), CAS no. 57422-77-2.
3.3 Tribromobiphenyl (TriBB), CAS no. 59080-34-1.
3.4 Tetrabromobiphenyl (TetraBB), CAS no. 60044-24-8.
3.5 Pentabromo-1,1’-biphenyl (PentaBB), CAS no. 59080-39-6.
3.6 Hexabromobiphenyl (HexaBB), CAS no. 60044-26-0.
3.7 Heptabromo-1,1’-biphenyl (HeptaBB), CAS no. 88700-06-5.
3.8 Octabromobiphenyl (OctaBB), CAS no. 67889-00-3.
3.9 Nonabromobiphenyl (NonaBB), CAS no. 69278-62-2.
3.10 Decabromobiphenyl (DecaBB), CAS no. 13654-09-6.
3.11 Tetrabromodiphenylether (TetraBDE) CAS no. 5436-43-1.
3.12 Pentabromodiphenylether (PentaBDE), CAS no.32534-81-9.
3.13 Hexabromodiphenylether (HexaBDE), CAS no. 207122-15-4.
3.14 Heptabromodiphenylether (HeptaBDE), CAS no. 207122-16-5.
3.15 Octabromodiphenylether (OctaBDE), CAS no. 337513-72-1.
3.16 Decabromodiphenylether (DecaBDE), CAS no. 1163-19-5.
3.17 Hexabromocyclododecane (HBCDD), CAS no. 25637-99-4.
3.18 Decachlorobiphenyl, CAS no.2051-24-3, internal standard (IS).
3.19 Toluene.
Note: Since brominated flame retardants have many isomers, this method might not cover all of them. Determination of the isomers of flame retardants in Clause 3 can refer to this method according to the principle.
4 Apparatus
4.1 Gas chromatograph-mass spectrometer (GC-MS).
4.2 Ultrasonic generator, with a frequency from 35kHz to 45kHz.
4.3 Evaporator device, with water bath at 50℃.
4.4 Brown glass vial, 40ml with tight closure.
4.5 Flask, 100ml.
4.6 Filtration membrane, 0.45μm.
4.7 Balance, an accuracy of 0.1mg.
5 Procedure
5.1 Preparation of standard solutions
5.1.1 Stock standard solution
Prepare 1 000μg/ml of stock standard solutions with individual flame retardant (3.1 to 3.17) and internal standard (3.18) in toluene (3.19).
Some commercial reference material solutions may be available in a different solvent
5.1.2 Internal standard solution
Prepare 10μg/ml standard solution of decachlorobiphenyl in toluene.
5.1.3 Working solution
Prepare an admixture working solution with 10μg/mL for 17 flame retardants in internal standard solution (5.1.2) by taking toluene as the solvent and dilute it to a series of suitable concentrations depending on test needs. Select at least five dilutions of the calibration sets to create calibration curve and perform GC-MS analysis
Note: Warranty for standard stock solutions is 12 months and 6 months for mixture standard stock solutions. Decabromobiphenyl solution is stored at room temperature while others are stored in refrigerator at 0-4℃.
5.2 Preparation of test specimen
Prepare a representative test specimen of the sample. Cut it into small pieces and weigh (1.00±0.01)g of the pieces with a balance (4.7).
5.3 Ultrasonic wave extraction
Put the pieces in a vial with tight closure (4.4) and add 20ml of toluene. Place the vial in an ultrasonic generator (4.2) and extract the pieces for 30min at room temperature. Filter and transfer the extract into 100ml flask (4.5). Add 10ml of toluene to the residue in the vial and place the vial in the ultrasonic generator to extract the residue for 15min at room temperature. Filter and merge the extract into the flask (4.5).
Evaporate the extract to near dryness by evaporator device (4.3). Add 2 ml of internal standard solution (5.1.2) to dissolve the residue and then filter by filtration membrane (4.6). The filtrate is ready for determination of flame retardants.
Foreword i
1 Scope
2 Principle
3 Reagents
4 Apparatus
5 Procedure
6 Calculation
7 Test report
Annex A (Informative) Test parameters by GC-MS
Annex B (Informative) Round Robin test
