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

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 flame retardant by GC-MS in Appendix A. At the same time, a blank test is performed, and the blank value is subtracted. When the content of flame retardant is too low, it is necessary to appropriately increase the mass of the sample to reach a detection limit of at least 3 times. When the flame retardant concentration exceeds the linear range of the instrument response value, it is necessary to properly dilute the solution. 6 Results calculation
The working curve was used to quantitatively determine the concentration of each flame retardant, expressed as the mass fraction of the sample, and the unit was μg/g. Calculated according to formula (1). Xi =
(ci-c0) × V
(1)
Where.
Xi --- the content of flame retardant i in the textile sample, the unit is micrograms per gram (μg/g); ci --- the concentration of flame retardant i in the test solution, the unit is micrograms per milliliter (μg/mL); c0 --- the concentration of flame retardant i in the blank test solution, the unit is micrograms per milliliter (μg/mL); V --- the final constant volume of the test solution, in milliliters (mL); m --- the mass of the sample, in grams (g).
7 Test report
The test report should include the following.
a) GB/T 24279 number of this part;
b) sample description;
c) the content of each flame retardant;
d) any deviation from the prescribed procedures.
Appendix A
(Informative appendix)
GC-MS detection parameter example
A.1 Instrument parameters
Because the test results depend on the instrument used, it is not possible to give general parameters for GC-MS analysis. The set parameters should be To ensure that the measured component can be effectively separated from other components during chromatographic determination, the parameters given below prove that it is feasible. a) Chromatographic column. VF-5ht quartz capillary column, length 15m, inner diameter 0.25mm, film thickness 0.1μm, or equivalent; b) Column temperature. 100 ℃ (2min), 100 ℃ ~ 310 ℃ (20 ℃/min), 310 ℃ (5min); c) inlet temperature. 280 ℃;
d) Mass spectrometry interface temperature. 300 ℃;
e) Carrier gas. Helium, purity ≥99.999%, flow rate 1.5mL/min;
f) Ionization mode. EI;
g) Ionization energy. 70eV;
h) Measurement method. Select ion monitoring method;
i) Sampling method. splitless injection, open valve after 1.0min;
j) Injection volume. 1.0 μL.
A.2 Characteristic ions and low limits of determination
The characteristic ions and the lower limit of determination of the flame retardant are shown in Table A.1. Table A.1 Table of Quantitative and Qualitative Selective Ion and Determination of Flame Retardants No. flame retardant
Characteristic ion/u
Qualitative ion
Low limit of determination /
(μg/g)
1 Monobromobiphenyl (MonoBB) 152 234,232,152 1
2 Dibromobiphenyl (DiBB) 152 312,310,152 1
3 Tribromobiphenyl (TriBB) 230 392,390,230 1
4 Tetrabromobiphenyl (TetraBB) 310 470,310,308 1
5 Pentabromobiphenyl (PentaBB) 388 550,390,388 1
6HexaBB 468 628,468,466 5
7HeptaBB 546 705,546,544 5
8 Octabromobiphenyl (OctaBB) 544 785,546,544 5
9 NonaBB 705 864,705,703 5
10 Decabromodiphenyl (DecaBB) 783 944,783,781 10
11 TetraBDE (TetraBDE) 326 488,486,326 1
12 PentaBDE (PentaBDE) 404 564,406,404 1
Table A.1 (continued)
No. flame retardant
Characteristic ion/u
Qualitative ion
Low limit of determination /
(μg/g)
13 Hexabromodiphenyl ether (HexaBDE) 484 6,484,482 5
14 HeptaBDE 562 722,562,456 5
15 OctaBDE (OctaBDE) 642 801,642,639 5
16 Decabromodiphenyl ether (DecaBDE) 799 959,799,797 10
17 Hexabromocyclododecane (HBCDD) 157 319,239,157 10
18 Decachlorobiphenyl (IS) 498 498,428,214-
The chromatograms of 17 flame retardant standards and internal standards are shown in Figure A.1. Explanation.
1 --- bromobiphenyl;
2 --- dibromobiphenyl;
3--tribromobiphenyl;
4 --- tetrabromobiphenyl;
5 --- tetrabromodiphenyl ether;
6 --- pentabromobiphenyl;
7 --- Pentabromobiphenyl ether;
8 --- decachlorobiphenyl (IS);
9 --- hexabromobiphenyl;
10 --- hexabromodiphenyl ether;
11 --- hexabromocyclododecane;
12 --- Heptabromobiphenyl;
13 --- Heptabromodiphenyl ether;
14 --- octabromodiphenyl ether;
15 --- octabromobiphenyl;
16 --- nonabromobiphenyl;
17 --- Decabromodiphenyl;
18 --- Decabromodiphenyl ether.
Figure A.1 Chromatograms of 17 flame retardant standards and 1 internal standard Appendix B
(Informative appendix)
Joint test
The joint trial was conducted in 5 laboratories.
Nine samples were prepared, three of which were taken from cotton fabrics (numbered 1 to 3), three were taken from polyester fabrics (numbered 4 to 6), and three were taken from 50% Cotton/50% polyester fabric (numbers 7-9), each sample contains 6 flame retardants, namely DiBB, PentaBB, DecaBB, PentaBDE, DecaBDE and HBCDD. Three samples of each fabric contained 50mg/kg,.200mg/kg and 500mg/kg. Three samples were prepared for each sample.
The combined test results are shown in Table B.1.
Table B.1 Joint test results
sample
Numbering
Flame retardant
name
Actual value /
(mg/kg)
average value/
(mg/kg)
Recovery rate/
Repeatability
Sr/(mg/kg) CVr /% SR/(mg/kg) CVR /%
Dibromobiphenyl (DiBB) 50 49.62 99.24 2.08 4.20 5.72 11.52
Pentabromobiphenyl (PentaBB) 50 45.00 90.00 1.97 4.37 6.16 13.69
Decabromodiphenyl (DecaBB) 50 44.76 89.52 1.63 3.64 6.401 14.30
PentaBDE (PentaBDE) 50 42.52 85.03 1.46 3.42 7.57 17.82
Decabromodiphenyl ether (DecaBDE) 50 46.23 92.46 1.82 3.94 7.97 17.24
Hexabromocyclododecane (HBCDD) 50 46.56 93.12 2.78 5.96 1.79 3.85
Dibromobiphenyl (DiBB).200.199.37 99.68 6.71 3.36 14.04 7.04
Pentabromobiphenyl (PentaBB).200 198.84 99.42 6.77 3.41 12.49 6.28
Decabromodiphenyl (DecaBB).200 191.39 95.70 6.28 3.28 10.35 5.41
PentaBDE (PentaBDE).200 189.96 94.98 8.26 4.35 15.69 8.26
Decabromodiphenyl ether (DecaBDE).200 183.85 91.93 9.51 5.17 20.68 11.25 Hexabromocyclododecane (HBCDD).200 192.05 96.03 6.16 3.21 7.70 4.01
Dibromobiphenyl (DiBB) 500 491.48 98.30 13.99 2.85 46.44 9.45
Pentabromobiphenyl (PentaBB) 500 482.46 96.49 21.19 4.39 12.12 2.51
Decabromodiphenyl (DecaBB) 500 478.75 95.75 20.72 4.33 27.11 5.66
PentaBDE (PentaBDE) 500 479.23 95.85 9.47 1.98 19.74 4.12
Decabromodiphenyl ether (DecaBDE) 500 480.40 96.08 18.65 3.88 23.59 4.91 Hexabromocyclododecane (HBCDD) 500 475.28 95.06 35.11 7.39 28.18 5.93
Dibromobiphenyl (DiBB) 50 46.14 92.28 2.38 5.17 3.50 7.59
Pentabromobiphenyl (PentaBB) 50 44.90 89.79 1.30 2.90 6.30 14.03
Decabromodiphenyl (DecaBB) 50 47.07 94.14 2.14 4.55 7.42 15.77
PentaBDE (PentaBDE) 50 41.70 83.40 1.43 3.43 7.82 18.76
Decabromodiphenyl ether (DecaBDE) 50 46.35 92.70 2.00 4.31 8.85 19.11
Hexabromocyclododecane (HBCDD) 50 43.84 87.68 2.23 5.08 6.59 15.04
Table B.1 (continued)
sample
Numbering
Flame retardant
name
Actual value /
(mg/kg)
average value/
(mg/kg)
Recovery rate/
Repeatability
Sr/(mg/kg) CVr /% SR/(mg/kg) CVR /%
Dibromobiphenyl (DiBB).200 192.47 96.24 7.96 4.14 10.64 5.53
Pentabromobiphenyl (PentaBB).200 191.08 95.54 10.80 5.65 11.75 6.15
Decabromodiphenyl (DecaBB).200 185.75 92.87 6.57 3.54 16.27 8.76
PentaBDE (PentaBDE).200 189.28 94.64 7.65 4.04 15.06 7.96
Decabromodiphenyl ether (DecaBDE).200 187.99 94.00 9.46 5.03 15.05 8.00 Hexabromocyclododecane (HBCDD).200 180.58 90.29 6.55 3.63 12.76 7.07
Dibromobiphenyl (DiBB) 500 480.93 96.19 17.75 3.69 30.69 6.38
Pentabromobiphenyl (PentaBB) 500 483.82 96.76 13.65 2.82 13.84 2.86
Decabromodiphenyl (DecaBB) 500 479.54 95.91 12.94 2.70 25.24 5.26
PentaBDE (PentaBDE) 500 473.41 94.68 7.21 1.52 28.69 6.06
Decabromodiphenyl ether (DecaBDE) 500 468.39 93.68 16.59 3.54 18.11 3.87 Hexabromocyclododecane (HBCDD) 500 485.21 97.04 21.12 4.35 17.67 3.64
Dibromobiphenyl (DiBB) 50 47.14 94.29 1.52 3.23 4.31 9.15
Pentabromobiphenyl (PentaBB) 50 44.67 89.34 1.79 4.01 6.99 15.65
Decabromodiphenyl (DecaBB) 50 45.03 90.06 2.73 6.05 3.06 6.79
PentaBDE (PentaBDE) 50 40.33 80.66 2.06 5.11 8.93 22.15
Decabromodiphenyl ether (DecaBDE) 50 45.43 90.86 2.70 5.94 5.61 12.34
Hexabromocyclododecane (HBCDD) 50 42.52 85.04 2.21 5.19 4.54 10.69
Dibromobiphenyl (DiBB).200 189.40 94.70 7.37 3.89 10.50 5.55
Pentabromobiphenyl (PentaBB).200 202.38 101.19 5.89 2.91 12.36 6.11
Decabromodiphenyl (DecaBB).200 189.63 94.82 8.12 4.28 5.80 3.06
PentaBDE (PentaBDE).200 189.05 94.53 3.99 2.11 15.31 8.10
Decabromodiphenyl ether (DecaBDE).200 191.94 95.97 7.07 3.68 7.78 4.05
Hexabromocyclododecane (HBCDD).200 179.18 89.59 7.65 4.27 15.56 8.69
Dibromobiphenyl (DiBB) 500 475.97 95.19 31.27 6.57 41.19 8.65
Pentabromobiphenyl (PentaBB) 500 494.46 98.89 11.23 2.27 23.03 4.66
Decabromodiphenyl (DecaBB) 500 503.78 100.76 16.22 3.22 24.95 4.95
PentaBDE (PentaBDE) 500 477.93 95.59 12.26 2.57 8.95 1.87
Decabromodiphenyl ether (DecaBDE) 500 479.87 95.97 19.73 4.11 35.29 7.35 Hexabromocyclododecane (HBCDD) 500 489.33 97.87 20.70 4.23 13.04 2.67

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