GB/T 29493.2-2021 PDF in English
GB/T 29493.2-2021 (GB/T29493.2-2021, GBT 29493.2-2021, GBT29493.2-2021)
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GB/T 29493.2-2021 | English | 350 |
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Determination of harmful substances in textile dyeing and finishing auxiliaries -- Part 2: Determination of perfluorinated compounds (PFCs)
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GB/T 29493.2-2013 | English | 125 |
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Determination of harmful substances in textile dyeing and finishing auxiliaries -- Part 2: Determination of perfluorooctane sulfonates and perfluorooctanoic acid -- HPLC-MS/MS method
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Standards related to (historical): GB/T 29493.2-2021
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GB/T 29493.2-2021: PDF in English (GBT 29493.2-2021) 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 & 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 arithmetic mean of the two
measured values.
5 Gas Chromatography-Mass Spectrometry (GC-MS)
5.1 Principle
Tert-butyl methyl ether is used as solvent; and ultrasonic extraction is used to extract the 4
fluorinated telomer alcohols (FTOH) and 3 fluorinated acrylates (FTA) in the specimen; and
the determination is carried out by gas chromatography-mass spectrometry; and the internal
standard method is used for quantification.
5.2 Reagents or materials
Unless otherwise specified, only reagents confirmed as analytically pure and Class-1 water
specified in GB/T 6682 are used.
5.2.1 Tert-butyl methyl ether.
5.2.2 4 fluorinated telomer alcohol (FTOH) standard substances, purity ≥ 95% (mass fraction),
see SN 28 to 31 in Table A.1.
5.2.3 3 fluorinated acrylate (FTA) standard substances, purity ≥ 95% (mass fraction), see SN
32 to 34 in Table A.1.
5.2.4 Internal standard substance: Perfluorodecane-1,10-dicarboxylic acid dimethyl ester (CAS
No.: 84750-88-9).
5.2.5 Preparation of standard stock solution, 1000 mg/L: Accurately weigh 0.100 g (accurate to
0.0001 g) of 4 fluorinated telomer alcohol (FTOH) standard substances (5.2.2) and 0.100 g
(accurate to 0.0001 g) of 3 fluorinated acrylate (FTA) standard substances (5.2.3), respectively;
dissolve them in tert-butyl methyl ether (5.2.1) and make constant volume to 100 mL.
NOTE: The standard stock solution shall be stored at -18℃ away from light and has a shelf life of 12
months.
5.2.6 Preparation of 4 fluorotelomer alcohol (FTOH) mixed intermediate solutions, 100 mg/L:
Accurately pipette 1 mL of each of the 4 fluorotelomer alcohol (FTOH) standard stock solutions
(5.2.5) into a 10 mL volumetric flask; dilute with tert-butyl methyl ether (5.2.1) and make
constant to the scale.
NOTE: The fluorotelomer alcohol (FTOH) mixed standard intermediate solution shall be stored at -18℃
away from light and has a shelf life of 1 month.
5.2.7 Preparation of 3 fluorinated acrylate (FTA) mixed intermediate solutions, 10mg/L:
Accurately transfer 0.1mL of each of the 3 fluorinated acrylate (FTA) standard stock solutions
(5.2.5) into a 10mL volumetric flask; dilute with tert-butyl methyl ether (5.2.1) and make
constant volume to the scale.
NOTE: The fluorinated acrylate (FTA) mixed standard intermediate solution shall be stored at -18℃
away from light, and has a shelf life of 1 month.
5.2.8 Internal standard substance standard stock solution, 1000mg/L: Accurately weigh 0.010g
(accurate to 0.0001g) of the internal standard substance (5.2.4); dissolve it with tert-butyl
methyl ether (5.2.1) and make constant volume to 10mL.
NOTE: The internal standard stock solution shall be stored at -18℃ away from light, and has the shelf
life of 3 months.
5.2.9 Internal standard substance standard intermediate solution, 15 mg/L: Accurately pipette
0.15 mL of the internal standard substance standard stock solution (5.2.8) into a 10 mL
volumetric flask; dilute with tert-butyl methyl ether (5.2.1) and make constant volume to the
scale.
NOTE: The internal standard substance standard intermediate solution shall be stored at -18°C away
from light and has a shelf life of 1 month.
5.2.10 The 4 fluorinated telomer alcohols (FTOH) and 3 fluorinated acrylates (FTA) mixed
standard working solutions: The preparation method is shown in Table 3. The mass
concentrations of fluorinated telomer alcohols in the mixed standard working solutions are 0.02
mg/L, 0.05 mg/L, 0.1 mg/L, 0.5 mg/L, and 1 mg/L, respectively; and the mass concentrations
of fluorinated acrylates are 0.2 mg/L, 0.5 mg/L, 1 mg/L, 5 mg/L, and 10 mg/L, respectively.
peak area as the ordinate, and use the ratio of the target compound and internal standard
concentration as the abscissa to make a standard working curve; and perform quantification by
internal standard method. The response values of fluorinated telomer alcohol (FTOH) and
fluorinated acrylate (FTA) in the specimen solution shall be within the linear range of
instrument detection. If the content exceeds the range of the standard working curve, dilute to
an appropriate concentration with tert-butyl methyl ether solution containing an internal
standard concentration of 0.15 mg/L and analyze. The selected ion flow spectra of each target
compound are shown in Figure C.28 of Appendix C.
5.5 Blank test
Except for the addition of no sample, all the operation procedures in 5.4 are followed.
5.6 Test data processing
5.6.1 Calculation of results
The test results are expressed by the test results of each fluorinated telomer alcohol (FTOH) or
fluorinated acrylate (FTA).
The content of each fluorinated telomer alcohol (FTOH) or fluorinated acrylate (FTA) in the
sample is expressed by mass fraction, wi, and the value is expressed in mg/kg, calculated
according to Formula (2):
Where:
Aci - the value of the peak area of the internal standard compound in the standard working
solution;
Ai - the value of the peak area of the target compound in the specimen solution;
ρi - the value of the mass concentration of the target compound in the standard working solution,
in mg/L;
V - the value of the total volume of tert-butyl methyl ether used for specimen extraction, in mL;
f - dilution factor;
Asi - the value of the peak area of the target compound in the standard working solution;
Ac - the value of the peak area of the internal standard compound in the sample solution;
m - the value of the specimen mass, in g.
5.6.2 Expression of results
The calculation result is expressed by the arithmetic mean of the results of two parallel
determinations, rounded off to two digits after the decimal point according to the rounding
value comparison method in 4.3.3 of GB/T 8170-2008.
5.7 Determination lower limit, recovery rate and precision
5.7.1 Determination lower limit
The determination lower limit of this Document for fluorinated telomer alcohol (FTOH) is 10
mg/kg, and the determination lower limit for fluorinated acrylate (FTA) is 1 mg/kg.
5.7.2 Recovery rate
The recovery rate of spiked samples shall be 70%~120%.
5.7.3 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 independently
testing the same object within a short period of time shall not exceed 10% of the arithmetic
mean of the two determination values.
6 Test Report
The test report shall at least give the following:
a) Sample source and description;
b) This Document number;
c) The used method;
d) Differences from this Document;
e) Abnormal conditions encountered during the test;
f) Experimental results;
g) Test date.
...... Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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