GB/T 29493.1-2021 English PDF (GBT29493.1-2021)

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GB/T 29493.1-2021: Determination of harmful substances in textile dyeing and finishing auxiliaries -- Part 1: Determination of the prohibited or restricted flame retardants
GB/T 29493.1-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
CCS G 70
Replacing GB/T 29493.1-2013
Determination of Harmful Substances in Textile Dyeing and
Finishing Auxiliaries – Part 1: Determination of the Prohibited
or Restricted Flame Retardants
ISSUED ON: OCTOBER 11, 2021
IMPLEMENTED ON: MAY 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 5
1 Scope ... 6
2 Normative References ... 6
3 Terms and Definitions ... 6
4 Gas Chromatography-Mass Spectrometry (GC-MS) ... 7
5 Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) ... 11
6 Test Report ... 18
Appendix A (Informative) Basic Information of Flame Retardants Tested in This
Document ... 19
Appendix B (Informative) Quantitative and Qualitative Ions of GC-MS ... 22
Appendix C (Informative) GC-MS Total Ion Flow Chromatograms of Polybrominated
Biphenyls (PBBs) and Polybrominated Diphenyl Ethers (PBDEs) ... 23
Appendix D (Informative) Mass Spectrometry Parameters of LC-MS/MS ... 26
Appendix E (Informative) LC-MS/MS Total Ion Flow Chromatograms of Phosphorus-
Containing Flame Retardants and Bromine-Containing Flame Retardants ... 28
Determination of Harmful Substances in Textile Dyeing and
Finishing Auxiliaries – Part 1: Determination of the Prohibited
or Restricted Flame Retardants
Warning: People who use this Document shall have practical experience working in
formal laboratory. This Document does not point out all possible safety issues. Users are
responsible for taking appropriate safety and health measures and ensuring that the
conditions specified in relevant national laws and regulations are met.
1 Scope
This Document specifies the method for determining the content of polybrominated biphenyls
(PBBs) and polybrominated diphenyl ethers (PBDEs) in textile dyeing and finishing auxiliaries
by gas chromatography-mass spectrometry (GC-MS); and the method for determining the
content of other prohibited and restricted phosphorus-containing flame retardants and bromine-
containing flame retardants in textile dyeing and finishing auxiliaries by liquid
chromatography-tandem mass spectrometry (LC-MS/MS).
This Document is applicable to the determination of 32 prohibited and restricted flame
retardants (see Appendix A) in textile dyeing and finishing auxiliaries.
2 Normative References
The provisions in following documents become the essential provisions of this Document
through reference in this Document. For the dated documents, only the versions with the dates
indicated are applicable to this Document; for the undated documents, only the latest version
(including all the amendments) is applicable to this Document.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 8170-2008 Rules of rounding off for numerical values and expression and judgement
of limiting values
3 Terms and Definitions
For the purposes of this Document, there are no terms and definitions apply.
4 Gas Chromatography-Mass Spectrometry (GC-MS)
4.1 Principle
After the sample is extracted with toluene by ultrasonic wave, the polybrominated biphenyls
(PBBs) and polybrominated diphenyl ethers (PBDEs) in the extract are determined by gas
chromatography-mass spectrometry and quantified by external standard method.
4.2 Reagents or materials
Unless otherwise specified, only reagents confirmed as analytically pure shall be used.
4.2.1 Anhydrous sodium sulfate.
4.2.2 Toluene: chromatographically pure.
4.2.3 Methanol: chromatographically pure.
4.2.4 Polybrominated biphenyls (PBBs) standard substances, purity ≥ 99% (mass fraction), see
SN 1 to 10 in Table A.1 of Appendix A.
4.2.5 Polybrominated diphenyl ethers (PBDEs) standard substances, purity ≥ 99% (mass
fraction), see SN 11 to 20 in Table A.1.
4.2.6 Polybrominated biphenyls (PBBs) standard stock solution, 1000 mg/L: Accurately weigh
50.0 mg (accurate to 0.1 mg) of polybrominated biphenyls (PBBs) standard substance (4.2.4);
place them in 50 mL volumetric flasks, respectively; dissolve them with toluene (4.2.2) and
dilute to the scale; and mix well.
4.2.7 Polybrominated diphenyl ether (PBDEs) standard stock solution, 1000 mg/L: Accurately
weigh 50.0 mg (accurate to 0.1 mg) of polybrominated diphenyl ether (PBDEs) standard
substance (4.2.5); place them in 50 mL volumetric flasks, respectively; dissolve them with
toluene (4.2.2) and dilute to scale; and mix well.
4.2.8 Mixed intermediate concentration solution of polybrominated biphenyls (PBBs) and
polybrominated diphenyl ethers (PBDEs), 10 mg/L: Respectively take 1 mL of polybrominated
biphenyl (PBBs) standard stock solution (4.2.6) and polybrominated diphenyl ether (PBDEs)
standard stock solution (4.2.7); place them in 100 mL volumetric flasks; dilute to scale with
toluene (4.2.2); and mix well.
4.2.9 Mixed standard working solution of polybrominated biphenyls (PBBs) and
polybrominated diphenyl ethers (PBDEs): Take an appropriate amount of the mixed
intermediate concentration solution of polybrominated biphenyls (PBBs) and polybrominated
diphenyl ethers (PBDEs) (4.2.8); dilute with toluene (4.2.2); and prepare 0.1 mg/L, 0.5 mg/L,
1 mg/L, 2 mg/L and 5 mg/L mixed standard working solutions. The preparation process is
shown in Table 1.
c) Mass spectrometer interface temperature: 340℃;
d) Injection volume: 1.0μL;
e) Injection mode: pulse non-divided flow;
f) Carrier gas: helium, purity ≥99.999% (volume fraction);
g) Carrier gas flow rate: 1.8mL/min;
h) Chromatographic column temperature: ;
i) Data acquisition method: Selected ion monitoring (SIM)/full scan (SCAN),
Octabromobiphenyl (OctaBB), Nonabromobiphenyl (NonaBB), Decabromobiphenyl
(DecaBB), Octabromodiphenyl ether (OctaBDE), Nonabromodiphenyl ether (NonaBDE)
and Decabromodiphenyl ether (DecaBDE) use SIM; and other components use SCAN;
j) Mass scanning range: 100u~1000u;
k) Ionization source: Electron bombardment ionization source (EI);
l) Ionization energy: 70eV;
m) Quadrupole temperature: 150℃;
n) Ion source temperature: 230℃.
NOTE: Before use, adjust the parameters to completely separate the peaks of each polybrominated
biphenyl (PBBs) and polybrominated diphenyl ether (PBDEs) component and the impurity peaks.
4.4.2.2 Qualitative analysis
Under the analytical conditions of 4.4.2.1, qualitative analysis is performed by comparing the
retention time of the measured components in the specimen solution and the standard working
solution and the relative abundance ratio of the characteristic ions in the mass spectrum (see
Appendix B). If the allowable deviation of the relative ion abundance of the measured
components in the specimen solution and the relative ion abundance of the measured
components in the standard working solution with equivalent concentration does not exceed the
provisions of Table 2, it can be judged that the corresponding analyte exists in the sample.
f - dilution factor.
4.6.2 Expression of results
The calculation result is expressed by the arithmetic mean of the results of two parallel
determinations, rounded-off to the unit according to the rounding value comparison method in
4.3.3 of GB/T 8170-2008.
4.7 Determination lower limit, recovery rate, precision
4.7.1 Determination lower limit
The determination lower limit of polybrominated biphenyl (PBBs) and polybrominated
diphenyl ether (PBD...