GB/T 36940-2018 English PDF (GBT36940-2018)

This Standard specifies the test method for determination of certain benzotriazole compounds (see Appendix A) in textile products using high performance liquid chromatography-tandem mass spectrometer (HPLCMS/MS) or high performance liquid chromatograph-diode array detector (HPLC-DAD).

GB/T 36940-2018
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
W 04
Textiles - Determination of certain benzotriazole
compounds
ISSUED ON: DECEMBER 28, 2018
IMPLEMENTED ON: JULY 01, 2019
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle ... 4
4 Reagents and materials ... 5
5 Apparatus and equipment ... 6
6 Test procedures ... 6
7 Calculation and expression of results ... 9
8 Lower limit of determination and precision of the methods ... 10
9 Test report ... 10
Appendix A (Normative) Information on reference materials ... 12
Appendix B (Informative) Mass spectrometry reference conditions ... 13 Appendix C (Informative) Multi-reaction monitoring diagrams (MRM) of
benzotriazole compound reference materials ... 14
Appendix D (Informative) HPLC-DAD chromatograms and UV spectrograms of
benzotriazole compound reference materials ... 16
Textiles - Determination of certain benzotriazole
compounds
WARNING — The personnel using this Standard shall have practical
experience in regular laboratory work. This Standard does not point out all possible safety problems. It is the responsibility of the user 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 test method for determination of certain
benzotriazole compounds (see Appendix A) in textile products using high performance liquid chromatography-tandem mass spectrometer (HPLC-
MS/MS) or high performance liquid chromatograph-diode array detector
(HPLC-DAD).
This Standard applies to all types of textile products.
2 Normative references
The following documents are indispensable for the application of this document. For the dated references, only the editions with the dates indicated are applicable to this document. For the undated references, the latest edition (including all the amendments) are applicable to this document.
GB/T 6682 Water for analytical laboratory use - Specification and test
methods
3 Principle
USE n-hexane-saturated acetonitrile-ultrasound to extract certain benzotriazole compounds in textiles. After the extract is filtered through a filter membrane, use high performance liquid chromatography-tandem mass spectrometer
(HPLC-MS/MS) or high performance liquid chromatograph-diode array detector (HPLC-DAD) to determine and confirm; use external standard method to
quantify.
5 Apparatus and equipment
5.1 Analytical balance: The division value is 0.01 g.
5.2 Reactor: sealed with a plug. It is about 25 mL and made of hard glass. 5.3 Ultrasonic generator: The working frequency is 40 kHz. Temperature is controllable.
5.4 Volumetric flask: 25 mL.
5.5 Disposable syringe: 1 mL.
5.6 Organic filter membrane: 0.22 μm; nylon or other organic phase.
5.7 High performance liquid chromatography-tandem mass spectrometer
(HPLC-MS/MS).
5.8 High performance liquid chromatograph-diode array detector (HPLC-DAD). 6 Test procedures
6.1 Extraction and purification
TAKE a representative sample; CUT it to less than 5 mm×5 mm and mix well. WEIGH 1.0 g (accurate to 0.01 g); PUT it in the reactor (5.2); ADD 15 mL of n- hexane saturated acetonitrile (4.9); EXTRACT in a 60 °C ultrasonic generator (5.3) for 15 min. FILTER the extract; USE 10 mL of n-hexane-saturated
acetonitrile (4.9) to ultrasonically extract the residue for 15 min. Combine the filtrates and collect in a 25 mL volumetric flask (5.4); COOL to room temperature and dilute to the mark. The sample solution is filtered through a 0.22 μm organic filter membrane (5.6). TAKE the filtrate as a test solution for machine analysis. 6.2 HPLC-MS/MS method
6.2.1 HPLC-MS/MS analysis conditions
Because the test results depend on the apparatus used, it is not possible to give general parameters for chromatography/mass spectrometry. The following parameters have proven suitable for testing:
a) Chromatographic column: Eclipse Plus C18 column, 3.5 μm, 2.1 mm×50
mm or an equivalent column;
b) Mobile phase A: methanol (4.1);
standard working curve, in milligrams per liter (mg/L);
c0 - The concentration of the blank test solution obtained from the standard working curve, in milligrams per liter (mg/L);
V - The constant volume of sample solution, in milliliters (mL);
m - The mass of sample, in grams (g).
7.2 Expression of results
The test results are expressed by the detection results of benzotriazole compounds respectively. The results are retained to one decimal place. When below the lower limit of determination, the test result is “not-detected”. 8 Lower limit of determination and precision of the
methods
8.1 Lower limit of determination
The lower limit of determination of benzotriazole compounds by HPLC-MS/MS method is 1 mg/kg. The lower limit of determination of benzotriazole compounds by HPLC-DAD method is 20 mg/kg.
8.2 Precision
In the same laboratory, using the same equipment by the same operator,
according to the same test method, and within a short period of time, the relative standard deviation of the two test results obtained from tests performed independently on the same measured object is not more than 10%, on the
premise of no more than 5% in cases greater than 10%.
9 Test report
The test report shall give at least the following:
a) The number of this Standard;
b) A detailed description of the test sample;
c) Description of apparatus method;
d) Test results;
e) Any differences from the prescribed procedures;