GB/T 24279.1-2018 English PDF (GBT24279.1-2018)

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GB/T 24279.1-2018: Textiles -- Determination of certain flame retardants -- Part 1: Brominated flame retardants
GB/T 24279.1-2018
Textiles--Determination of certain flame retardants--Part 1. Brominated flame retardants
ICS 59.080.01
W04
National Standards of People's Republic of China
Replaces GB/T 24279-2009
Determination of certain flame retardants in textiles
Part 1. Brominated flame retardants
Textiles-Determinationofcertainflame retards-
Part 1. Brominated flame retardants
(ISO 17881-1..2016, IDT)
2018-12-28 release
2019-07-01 Implementation
State Administration of Market Supervision
Published by China National Standardization Administration
Foreword
GB/T 24279 "Determination of certain flame retardants in textiles" is divided into 2 parts.
--- Part 1. Brominated flame retardants;
--- Part 2. Phosphorous flame retardant.
This part is the first part of GB/T 24279.
This section is drafted in accordance with the rules given in GB/T 1.1-2009.
This section replaces GB/T 24279-2009 "Determination of flame retardants restricted in textiles", compared with GB/T 24279-2009
The technical changes are as follows.
--- Modified the standard name;
--- Adjusted the type of flame retardant target;
--- Removed the chapter on normative references;
--- Modified the pre-treatment extraction method;
--- The quantitative method was modified from the external standard method to the internal standard method;
--- Deleted 3 appendices in the original standard, and added informative appendix A about examples of GC-MS detection parameters.
This section uses the translation method equivalent to ISO 17881-1..2016 "Determination of certain flame retardants in textiles. Part 1. Bromine resistance
Fuel ".
The following editorial changes have been made in this section.
--- In order to provide information on storage conditions of standard solutions and easy to use, a note was added in 5.1.3;
--- Informative Appendix A, the chromatogram was added for easy operation, and the lower limit of determination of individual measured substances was adjusted.
This section is proposed by China Textile Industry Federation.
This section is under the jurisdiction of the National Technical Committee for Textile Standardization (SAC/TC209).
This section was drafted. China Textile Standards Inspection and Certification Co., Ltd., Jilin Entry-Exit Inspection and Quarantine Bureau, Yantai Zhenghai Hetai Technology Co., Ltd.
Co., Ltd., Fujian Fiber Inspection Bureau, Lilang (China) Co., Ltd., Fujian Fengzhu Textile Technology Co., Ltd., Shanghai Quality Supervision
Inspection Technology Research Institute, Shanghai Tianxiang Quality Technology Service Co., Ltd.
The main drafters of this section. Corning, Si Ying, Zheng Yuying, Li Aijun, Wang Lin, Pei Dejun, Guo Huanxiang, Zheng Juan, Wang Anying, Gao Bing, and Fan Rong.
The previous versions of the standards replaced by this section are.
--- GB/T 24279-2009.
Determination of certain flame retardants in textiles
Part 1. Brominated flame retardants
Caution --- Personnel using this section should have practical experience in formal laboratory work. This section does not indicate all possible security issues.
question. It is the user's responsibility to take appropriate safety and health measures and ensure compliance with relevant national laws and regulations.
1 Scope
This part of GB/T 24279 specifies the use of gas chromatography-mass spectrometry (GC-MS) to determine certain brominated flame retardants in textiles
Test method.
This section applies to all types of textiles.
2 Principle
The flame retardant in the sample was extracted with toluene through an ultrasonic generator, measured and confirmed by gas chromatography-mass spectrometry, and quantified by internal standard method.
3 reagents
Unless otherwise specified, the reagents used are analytical grade.
3.1 Monobromobiphenyl, CAS No. 2052-07-5.
3.2 Dibromobiphenyl, CAS No. 57422-77-2.
3.3 Tribromobiphenyl, CAS No. 59080-34-1.
3.4 Tetrabromobiphenyl, CAS No. 60044-24-8.
3.5 Pentabromobiphenyl, CAS No. 59080-39-6.
3.6 Hexabromobiphenyl, CAS No. 60044-26-0.
3.7 Heptabromobiphenyl, CAS No. 88700-06-5.
3.8 Octabromobiphenyl, CAS No. 67889-00-3.
3.9 Nonabromobiphenyl, CAS No. 69278-62-2.
3.10 Decabromodiphenyl, CAS No. 13654-09-6.
3.11 Tetrabromodiphenyl ether, CAS No. 5436-43-1.
3.12 Pentabromodiphenyl ether, CAS No. 32534-81-9.
3.13 Hexabromobiphenyl ether, CAS No. 207122-15-4.
3.14 Heptabromodiphenyl ether, CAS No. 207122-16-5.
3.15 Octabromodiphenyl ether, CAS No. 337513-72-1.
3.16 Decabromodiphenyl ether, CAS No. 1163-19-5.
3.17 Hexabromocyclododecane, CAS No. 25637-99-4.
3.18 Decachlorobiphenyl, CASNo. 2051-24-3, internal standard.
3.19 toluene.
Note. Due to the many isomers of brominated flame retardants, this method cannot include all isomers. Flame retardant isomers listed in Chapter 3
The determination can be referred to this method.
4 Instruments and equipment
4.1 Gas chromatography-mass spectrometry (GC-MS).
4.2 Ultrasonic generator. Working frequency 35kHz ~ 45kHz.
4.3 Rotary evaporator, can provide 50 ℃ water bath.
4.4 Brown glass extraction bottle with stopper, 40mL.
4.5 Concentration bottle, 100mL.
4.6 Organic filter, 0.45μm.
4.7 balance, the division value is 0.1mg.
5 Test steps
5.1 Standard solution preparation
5.1.1 Standard and internal standard stock solutions
Toluene (3.19) was used as a solvent to prepare each standard stock solution of each flame retardant (3.1 ~ 3.17) and internal standard (3.18) at a concentration of
1000 μg/mL.
Standard solutions dissolved in other solvents can also be used.
5.1.2 Internal standard working solution
Using toluene as a solvent, a 10 μg/mL decachlorobiphenyl internal standard working solution was prepared.
5.1.3 Standard working solution
Toluene was used as a solvent, and standard and internal standard stock solutions were used to prepare a mixed standard working solution of 17 flame retardants.
The standard concentration is 10 μg/mL, and the internal standard working solution (5.1.2) is used to serially dilute the serial standard to the appropriate concentration as required.
Solution. Select at least 5 standard solution concentration gradients to draw a working curve and analyze by GC-MS.
Note. The validity period of the standard stock solution is 12 months, and the validity period of the mixed standard solution is 6 months. Decabromobiphenyl solution is stored at room temperature.
Store in refrigerator at 0 ℃ ~ 4 ℃.
5.2 Sample preparation
Take a representative sample from the sample, cut and mix it, and weigh (1.00 ± 0.01) g of the sample with a balance (4.7).
5.3 Ultrasonic extraction
Place the sample in a stoppered brown extraction bottle (4.4), add 20 mL of toluene, place in an ultrasonic generator (4.2) and extract at room temperature
30min. The extract was filtered and transferred to a 100 mL concentrating flask (4.5), and 10 mL of toluene was used for ultrasonic extraction at room temperature to extract the
The residue was 15 min. The filtrates were combined and collected in a concentration bottle (4.5).
Concentrate on a rotary evaporator (4.3), make the residue nearly dry, make up to 2.0 mL with the internal standard working solution (5.1.2), and pass through the filter membrane (4.6)
The obtained filtrate was used for the determination of a flame retardant.
5.4 Determination
The flame retardants in the filtrate obtained in 5.3 were determined by GC-MS (4.1) and quantified by internal standard method. Standard working solution and sample solution
Insert the sample and give an example of the detection parameters of fla...