GB/T 40917-2021 PDF English
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Textiles - Determination of perfluorohexane-1-sulphonic acid and its salts
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GB/T 40917-2021: Textiles - Determination of perfluorohexane-1-sulphonic acid and its salts---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT40917-2021
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
Textiles - Determination of perfluorohexane-1-
sulphonic acid and its salts
ISSUED ON: OCTOBER 11, 2021
IMPLEMENTED ON: MAY 01, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principle ... 4
5 Reagents or materials ... 5
6 Instruments and equipment ... 5
7 Analysis steps ... 6
8 Result calculation and presentation ... 7
9 Limit of quantitation and precision ... 8
10 Test report ... 8
Annex A (informative) Reference conditions for high performance liquid-tandem
mass spectrometry ... 10
Annex B (informative) Typical LC-MS/MS total ion chromatogram of standard
material PFHxS ... 12
Annex C (informative) Mass spectrometry multiple reaction monitoring (MRM)
selected ion chromatogram of reference material PFHxS ... 13
Textiles - Determination of perfluorohexane-1-
sulphonic acid and its salts
WARNING - Persons using this document should have practical
experience in formal laboratory work. This document does not address all
possible security issues. It is the user's responsibility to take appropriate
safety and health measures, and to ensure compliance with the
conditions stipulated by relevant national regulations.
1 Scope
This Standard specifies the method of high-performance liquid
chromatography-tandem mass spectrometer (HPLC-MS/MS) to determine the
content of perfluorohexane-1-sulphonic acid and its salts (PFHxS) in textiles.
This document applies to all types of textiles.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 6682, Water for analytical laboratory use - Specification and test
methods
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Principle
Use organic solvent ultrasonic to extract perfluorohexane-1-sulphonic acid and
its salts in the specimen. After the extract is filtered through a membrane, use
high-performance liquid chromatography-tandem mass spectrometer (HPLC-
MS/MS) to determine. Quantify with the external standard method.
5 Reagents or materials
Unless otherwise stated, the reagents used are analytically-pure and water is
grade one specified in GB/T 6682.
5.1 Methanol: Chromatographically pure.
5.2 Formic acid: Chromatographically pure.
5.3 PFHxS standard product: Potassium perfluorohexanesulfonate (CAS No.
3871-99-6) or perfluorohexanesulfonic acid (CAS No. 355-46-4) standard
product; Content≥99.0%.
NOTE: Perfluorohexanesulfonate exists in solution as perfluorohexanesulfonic acid ion.
The sample solution and standard solution are quantified with perfluorohexanesulfonate.
5.4 PFHxS standard stock solution: Accurately weigh an appropriate amount of
PFHxS standard product (5.3). Use methanol (5.1) to dissolve and dilute.
Prepare a standard stock solution of the desired concentration. The
concentration is 1000mg/L.
NOTE: The standard stock solution is valid for 12 months when stored in the dark at
0°C~4°C.
5.5 PFHxS standard solution: Pipette an appropriate amount of PFHxS
standard stock solution (5.4). Use methanol (5.1) to prepare a standard solution
with a concentration of 10 mg/L.
NOTE: The validity period of the standard solution is 6 months when stored in the dark at
0°C~4°C.
5.6 PFHxS standard working solution: Pipette an appropriate amount of PFHxS
standard solution (5.5). Use methanol (5.1) to prepare standard working
solutions with concentrations of 1μg/L, 3μg/L, 5μg/L, 7μg/L and 10μg/L.
NOTE: Prepare the standard working solution when it is required.
5.7 0.05% formic acid solution: Take a certain volume of formic acid (5.2) to
prepare an aqueous solution with a volume fraction of 0.05%.
6 Instruments and equipment
6.1 High performance liquid chromatography-tandem mass spectrometer
(HPLC-MS/MS): Equipped with an electrospray ionization source (ESI).
6.2 Extractor: 50mL, polypropylene or polyethylene tube with screw cap.
6.3 Ultrasonic generator: The working frequency is 40kHz~60kHz.
6.4 Balance: The division values are 0.0001g and 0.01g respectively.
6.5 Nylon organic phase syringe filter: The pore size is 0.22μm.
7 Analysis steps
7.1 Specimen preparation and extraction
Take a representative sample. Cut into small pieces about 5mm×5mm. Mix.
Weigh 1g (accurate to 0.01g) from the mixed sample with the balance (6.4). Put
in the extractor (6.2). Add 30mL of methanol (5.1). Place the extractor (6.2) in
the ultrasonic generator (6.3) to extract for 50min. Use the syringe filter (6.5) to
filter the sample solution into the sample vial, used for HPLC-MS/MS
determination.
7.2 Determination
7.2.1 Liquid chromatography-tandem mass spectrometry conditions
Since the test results depend on the instrument used, it is not possible to give
general parameters for chromatographic analysis. The liquid chromatography
and mass spectrometry given in Annex A have been found to be suitable.
7.2.2 Qualitative and quantitative determination
Standard working solution and sample solution are determined according to the
conditions of Annex A. If a peak appears at the same retention time as the
standard working solution, confirm it. The retention time of the chromatographic
peak of the tested substance is consistent with that of the reference substance.
The selected ions appear in the sample spectrum after subtracting the
background. At the same time, the abundance ratio of the selected ions is
consistent with the relative ion abundance of the standard material. The
similarity is within the allowable range of relative deviation specified in Table 1.
Confirmed samples can be judged as positive detections.
The quantification is performed by external standard method according to the
standard working curve.
Under the liquid chromatography-tandem mass spectrometry conditions given
in Annex A, the liquid chromatography-tandem mass spectrometry total ion
chromatogram of the standard substance PFHxS is shown in Annex B. The
mass spectrometry multiple reaction monitoring (MRM) selected ion
chromatogram of the standard material PFHxS is shown in Annex C.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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