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GB/T 29493.2-2013 English PDF (GBT29493.2-2013)

GB/T 29493.2-2013 English PDF (GBT29493.2-2013)

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GB/T 29493.2-2013: Determination of harmful substances in textile dyeing and finishing auxiliaries -- Part 2: Determination of perfluorooctane sulfonates and perfluorooctanoic acid -- HPLC-MS/MS method

This Part of GB/T 29493 specifies the HPLC-MS/MS method for the determination of perfluorooctane sulfonates and perfluorooctanoicacid in textile dyeing and finishing auxiliaries. This Part applies to the determination of perfluorooctane sulfonates and perfluorooctanoicacid in various textile dyeing and finishing auxiliaries.
GB/T 29493.2-2013
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.100.40
G 70
Determination of harmful substances in textile dyeing
and finishing auxiliaries - Part 2: Determination of
perfluorooctane sulfonates and perfluorooctanoicacid
- HPLC-MS/MS method
ISSUED ON: FEBRUARY 07, 2013
IMPLEMENTED ON: SEPTEMBER 01, 2013
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle ... 4
4 Reagents and materials ... 5
5 Instruments and equipment ... 6
6 Analysis steps ... 6
7 Blank test ... 8
8 Result calculation ... 8
9 Low limit of determination, recovery and precision ... 9
10 Test report... 9
Annex A (informative) HPLC-MS/MS analysis diagrams ... 10
Determination of harmful substances in textile dyeing
and finishing auxiliaries - Part 2: Determination of
perfluorooctane sulfonates and perfluorooctanoicacid
- HPLC-MS/MS method
1 Scope
This Part of GB/T 29493 specifies the HPLC-MS/MS method for the
determination of perfluorooctane sulfonates and perfluorooctanoicacid in textile dyeing and finishing auxiliaries.
This Part applies to the determination of perfluorooctane sulfonates and perfluorooctanoicacid in various textile dyeing and finishing auxiliaries. 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 6682-2008 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 Principle
USE methanol as the solvent for the sample. EXTRACT perfluorooctane
sulfonates (PFOS) and perfluorooctanoicacid (PFOA) in the sample by
ultrasonic. DETERMINE and CONFIRM by high performance liquid
chromatography/mass spectrometry (HPLC-MS/MS). QUANTIFY by external
standard method.
before use.
Accurately PIPETTE 12.5 ??L, 25 ??L, 50 ??L, 100 ??L, 200 ??L of perfluorooctane sulfonates and perfluorooctanoicacid mixed standard solution (4.8), DILUTE to 1 mL with methanol.
5 Instruments and equipment
5.1 High performance liquid chromatography-tandem quadrupole mass
spectrometer (LC-MS/MS), equipped with an electrospray ion source (ESI). 5.2 Temperature-controllable ultrasonic bath, of which the working frequency is 40 kHz, and the temperature control accuracy is ??5 ??C at 70 ??C.
5.3 Electronic balance, with a sensitivity of 0.0001 g.
5.4 Extractor, made of hard glass, tubular, with a plug, 50 mL.
5.5 Disposable syringe, 1 mL ~ 5 mL.
5.6 0.45 ??m nylon filter.
6 Analysis steps
6.1 Sample treatment
WEIGH 1.00 g of sample (accurate to 0.01 g); PLACE it in an extractor (5.4); accurately ADD 10.0 mL of methanol (4.1); PUT the plug in. PLACE the
extractor in a temperature-controllable ultrasonic bath (5.2) at (70 ?? 5) ??C for extraction for (30 ?? 2) min, then COOL to room temperature. USE a disposable syringe (5.5) to make the sample solution passed through a 0.45 ??m nylon filter (5.6) into a sample bottle. DILUTE 10 times with methanol (4.1) for HPLC- MS/MS analysis.
6.2 Analysis method
6.2.1 HPLC-MS/MS analysis conditions
Because the test results depend on the instrument used, it is not possible to give general parameters for chromatographic analysis. The following
parameters have been proven suitable for test.
a) Chromatographic column: C18 column, 2.1 mm ?? 150 mm, particle size
3.5 ??m, or equivalent;
b) Flow rate: 0.3 mL/min;
Take the arithmetic mean of two parallel determinations and round off to the whole number according to GB/T 8170-2008, which is the determination result. 9 Low limit of determination, recovery and precision
9.1 Low limit of determination
The Low limit of determination of this method is 10 mg/kg.
9.2 Recovery
The recovery of PFOS and PFOS by this method is 80 % ~ 120 %.
9.3 Precision
The absolute difference between the two independent test results obtained by the test on the same test object, in the same laboratory, by the same operator, using the same equipment, according to the same determination method, and within a short period of time, is not greater than the two 20 % of the arithmetic mean of the determined values.
10 Test report
The test report shall have at least the following contents:
a) description of the specimen;
b) serial number of this Part;
c) test results;
d) differences from this Part;
e) test date.

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