GB/T 29493.2-2021 English PDF (GBT29493.2-2021)

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GB/T 29493.2-2021: Determination of harmful substances in textile dyeing and finishing auxiliaries -- Part 2: Determination of perfluorinated compounds (PFCs)
GB/T 29493.2-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
CCS G 70
Replacing GB/T 29493.2-2013
Determination of Harmful Substances in Textile Dyeing and
Finishing Auxiliaries – Part 2: Determination of the
Perfluorinated Compounds (PFCs)
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 Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) ... 7
5 Gas Chromatography-Mass Spectrometry (GC-MS) ... 11
6 Test Report ... 16
Appendix A (Informative) Basic Information of Perfluorinated Compounds and Internal
Standards Substance Tested in This Document ... 17
Appendix B (Informative) Mass Spectrometry Parameters of LC/MS/MS (ESI) for 27
Perfluorinated Compounds ... 20
Appendix C (Informative) Perfluorinated Compound Chromatograms ... 23
Appendix D (Informative) Quantitative and Qualitative Ions of GC-MS ... 33
Determination of Harmful Substances in
Textile Dyeing and Finishing Auxiliaries – Part 2:
Determination of the Perfluorinated Compounds (PFCs)
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 27 ionic perfluorinated
compounds in textile dyeing and finishing auxiliaries by liquid chromatography-tandem mass
spectrometry (LC-MS/MS); and the method for determining the content of 4 fluorinated
telomer alcohols (FTOH) and 3 fluorinated acrylates (FTA) in textile dyeing and finishing
auxiliaries by gas chromatography-mass spectrometry (GC-MS).
This Document is applicable to the determination of 34 perfluorinated compounds (see
Appendix A) in various 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 Liquid Chromatography-Tandem Mass Spectrometry (LC-
MS/MS)
4.1 Principle
Using methanol as solvent, ultrasonic extraction of 27 ionic perfluorinated compounds in the
specimen is performed; and the extract is determined and confirmed by liquid chromatography-
tandem mass spectrometry; and quantified by external standard method.
4.2 Reagents or materials
Unless otherwise specified, only reagents confirmed as analytically pure and Class-1 water
specified in GB/T 6682 are used.
4.2.1 Methanol, chromatographically pure.
4.2.2 Acetonitrile, chromatographically pure.
4.2.3 27 ionic perfluorinated compound standard substances, purity ≥ 95% (mass fraction); see
SN 1 to 27 in Table A.1.
4.2.4 Ammonium acetate aqueous solution, 5mmol/L: Accurately weigh 0.385g of ammonium
acetate and dissolve it in water; transfer it to a 1L volumetric flask and dilute to the scale; and
shake well.
4.2.5 Ionic perfluorinated compound standard stock solution, 200 mg/L: Accurately weigh
0.020 g (accurate to 0.1 mg) of each of the 27 ionic perfluorinated compound standard
substances (4.2.3); place in a 100 mL volumetric flask; dissolve with methanol; dilute to scale;
and mix well.
NOTE: The ionic perfluorinated compound standard stock solution is stored at 0℃~4℃ away from light
and has a shelf life of 12 months.
4.2.6 Ionic perfluorinated compound primary mixed standard intermediate solution, 2 mg/L:
Accurately transfer 0.5 mL of each ionic perfluorinated compound standard stock solution
(4.2.5) to a 50 mL volumetric flask; dilute with methanol (4.2.1) and make the constant volume
to the scale.
NOTE: The ionic perfluorinated compound primary mixed standard intermediate solution is stored at
0℃~4℃ away from light and has a shelf life of 6 months.
4.2.7 Ionic perfluorinated compound secondary mixed standard intermediate solution, 0.1 mg/L:
Accurately transfer 5 mL of ionic perfluorinated compound primary mixed standard
intermediate solution (4.2.6) to a 100 mL volumetric flask; dilute with methanol (4.2.1) and
make constant volume to the scale.
NOTE: The ionic perfluorinated compound secondary mixed standard intermediate solution shall be
stored at 0℃~4℃ away from light, and the shelf life is 3 months.
4.2.8 Ionic perfluorinated compound mixed standard working solution: Accurately transfer
40μL, 100μL, 200μL, 500μL, 1000μL of ionic perfluorinated compound secondary mixed
standard intermediate solution (4.2.7) to a 10 mL volumetric flask; dilute with methanol (4.2.1)
and make constant volume to the scale; and prepare 0.4μg/L, 1.0μg/L, 2.0μg/L, 5.0μg/L, 10μg/L
standard working solutions, respectively.
NOTE: The ionic perfluorinated compounds mixed standard working solution shall be stored at 0℃~4℃
away from light and has a shelf life of 1 month.
4.3 Instruments
4.3.1 Liquid chromatography-tandem mass spectrometry: Equipped with electrospray
ionization source (ESI).
4.3.2 Ultrasonic generator: Working frequency 40kHz.
4.3.3 Analytical balance: Sensitivity 0.0001g.
4.3.4 Extractor: With airtight stopper, 50mL~70mL, made of hard glass.
4.3.5 Volumetric flask: 10mL, 50mL, 100mL.
4.3.6 Disposable syringe: 1mL~5mL.
4.3.7 Regenerated cellulose (RCE) filter head: 0.45μm.
NOTE: Other proven suitable filter heads can be used.
4.4 Test procedures
4.4.1 Preparation of specimen solution
Accurately weigh 0.2g (accurate to 0.001g) of sample, place in the extractor; accurately add
10.0mL of methanol (4.2.1); and seal with a stopper. Place the extractor in an ultrasonic
generator and extract for 30 min at room temperature; then cool to room temperature. Use a
disposable syringe to filter the specimen solution through a regenerated cellulose filter head
into a sample bottle; dilute it 10 times with methanol (4.2.1) and perform LC-MS/MS analysis.
4.4.2 Analysis method
4.4.2.1 Analysis conditions
Since the test results depend on the used instrument, it is impossible to give general parameters
for chromatographic analysis. The set parameters shall ensure that the measured component can
be effectively separated from other components when measured under chromatographic
4.7 Determination lower limit, recovery rate and precision
4.7.1 Determination lower limit
The determination lower limit of this Document is 0.5mg/kg.
4.7.2 Recovery rate
The recovery rate of the spiked sample shall be 70%~120%.
4.7.3 Precision
The absolute difference between two independent test results obtained by the same operator
using the same equipment and the same test method in the same laboratory and on the same test
object within a short period of time shall not exceed 10% of the...