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SN/T 5260-2020: (Determination of Tetrabromobisphenol A and Tris(1,3-Dichloropropyl) Phosphate in Coatings Liquid Chromatography-Mass Spectrometry/Mass Spectrometry)
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(Determination of Tetrabromobisphenol A and Tris(1,3-Dichloropropyl) Phosphate in Coatings Liquid Chromatography-Mass Spectrometry/Mass Spectrometry)
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SN/T 5260-2020
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Basic data | Standard ID | SN/T 5260-2020 (SN/T5260-2020) | | Description (Translated English) | (Determination of Tetrabromobisphenol A and Tris(1,3-Dichloropropyl) Phosphate in Coatings Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | G50 | | Classification of International Standard | 87.040 | | Word Count Estimation | 8,838 | | Date of Issue | 2020-08-27 | | Date of Implementation | 2021-03-01 | | Regulation (derived from) | General Administration of Customs Announcement No. 98 [2020] | | Issuing agency(ies) | General Administration of Customs | SN/T 5260-2020: (Determination of Tetrabromobisphenol A and Tris(1,3-Dichloropropyl) Phosphate in Coatings Liquid Chromatography-Mass Spectrometry/Mass Spectrometry)
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The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
Determination of Tetrabromobisphenol A and Tris(1,3-Dichloroisopropyl) Phosphate in Coatings Liquid Chromatography-Mass Spectrometry/Mass Spectrometry
2020-08-27 release
2021-03-01 implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organizations of this standard. Xiamen Customs Technology Center of the People's Republic of China, Shenzhen Vocational and Technical College.
The main drafters of this standard. Lai Ying, Lin Rui, Hu Zhiyuan, Li Bin, Tu Xingpeng, Ding Huajun, Sun Weijia.
Tetrabromobisphenol A and phosphoric acid tribromide in paint
(1,3-Dichloroisopropyl) ester determination
Liquid chromatography-mass spectrometry/mass spectrometry
1 Scope
This standard specifies the liquid chromatography quality of tetrabromobisphenol A and tris(1,3-dichloroisopropyl) phosphate in water-based paints and solvent-based paints.
Spectrum determination method.
This standard applies to the determination of tetrabromobisphenol A and tris(1,3-dichloroisopropyl) phosphate in water-based paints and solvent-based paints.
The lower limits of this standard for the determination of tetrabromobisphenol A and tris(1,3-dichloroisopropyl) phosphate in water-based paints and solvent-based paints are respectively
1 mg/kg and 5 mg/kg.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle
The water-based paint was ultrasonically extracted with ethyl acetate, the solvent was replaced with acetonitrile by nitrogen blowing, and the solvent-based paint was directly ultrasonically extracted with acetonitrile.
After filtering the acetonitrile extract, it was determined and confirmed by liquid chromatography-mass spectrometry/mass spectrometry, and quantified by external standard method.
4 Reagents and materials
Unless otherwise specified, the reagents used are all analytically pure, and the water is first-grade water that meets the requirements of GB/T 6682.
4.1 Ethyl acetate. chromatographically pure.
4.2 Acetonitrile. chromatographically pure.
4.3 Tetrabromobisphenol A (Tetrabromobisphenol A, CAS number. 79-94-7). purity ≥ 97%.
4.4 Tris (1,3-dichloroisopropyl) phosphate [Tris (1,3-dichloroisopropyl) phosphate, CAS number. 13674-87-8]. purity
≥ 97%.
4.5 Standard stock solution (1 000 mg/L). accurately weigh out each of tetrabromobisphenol A (4.3) and tris(1,3-dichloroisopropyl) phosphate (4.4)
0.10 g (accurate to 0.0001 g), placed in a 100 mL volumetric flask, dissolved in acetonitrile (4.2) and dilute to volume.
4.6 Standard working solution. Pipette appropriate amount of standard stock solution (4.5) respectively, and dilute it step by step with acetonitrile (4.2) to 10 μg/L, 20 μg/L,
Standard working solutions of 50 μg/L, 100 μg/L,.200 μg/L, 500 μg/L, and 1,000 μg/L.
4.7 Organic phase filter membrane. 0.22 μm.
5 Apparatus and equipment
5.1 Liquid chromatography-mass spectrometer/mass spectrometer. equipped with electrospray ion source.
5.2 Electronic balance. Sensitivity 0.1 mg.
5.3 Vortex mixer.
5.4 Ultrasonic cleaner (power ≥ 220 W).
5.5 Centrifuge. the speed is not less than 4 000 r/min.
6 Analysis steps
6.1 Extraction
6.1.1 Water-based paint
Weigh about 0.25 g of the mixed sample (accurate to 0.0001 g), place it in a 25 mL colorimetric tube with a stopper, and use ethyl acetate (4.1)
Dilute to the mark. After mixing on the vortex mixer (5.3), the ultrasonic cleaner (5.4) extracts for 15 minutes and transfers to a 25 mL stopper.
Centrifuge the tube at a speed of 4 000 r/min for 8 min. Accurately pipette 1 mL of the supernatant, blow dry with nitrogen, and accurately add 1 mL of acetonitrile (4.2)
Dissolve. Filter with a 0.22 μm organic phase filter membrane (4.7), and the filtrate is used for liquid chromatography-mass spectrometry/mass spectrometry.
6.1.2 Solvent-based coatings
Weigh about 0.25 g of the mixed sample (accurate to 0.0001 g), place it in a 25 mL colorimetric tube with a stopper, and dilute with acetonitrile (4.2)
To the scale. After mixing on the vortex mixer (5.3), the ultrasonic cleaner (5.4) extracts for 15 minutes and transfers to a 25 mL stoppered centrifuge tube.
Centrifuge at a speed of 4 000 r/min for 8 min, take the supernatant and filter it with a 0.22 μm organic phase filter (4.7), and use the filtrate for liquid chromatography-quality
Spectro/mass spectrometer determination.
6.2 Determination
6.2.1 Chromatographic reference conditions
Since the test results depend on the instrument used, the general parameters of chromatography/mass spectrometry cannot be given. The following parameters have been proven
It is appropriate to test.
a) Chromatographic column. C18 column, 50 mm×2.1 mm (inner diameter), 1.8 μm, or equivalent;
b) Column temperature. 35 ℃;
c) Injection volume. 1 μL;
d) Mobile phase. A-water, B-acetonitrile;
e) See Table 1 for gradient elution conditions;
f) Flow rate. 0.3 mL/min.
6.2.2 Reference conditions for mass spectrometry
Since the test results depend on the instrument used, the general parameters of mass spectrometry cannot be given. The following parameters have been proven to be tested
Try is appropriate. The parameters of the electrospray ion source (ESI) are shown in Table 2, and the monitoring ion pair and collision energy are shown in Table 3.
6.2.3 Qualitative determination
Determine the sample and standard working solution according to the above conditions. If the retention time of the mass chromatographic peak of the sample is consistent with that of the standard, it is allowed
The deviation is less than ±2.5%; the relative abundance of the qualitative ion pair is consistent with the relative abundance of the standard working solution with the same concentration, and the relative abundance allows
If the allowable deviation does not exceed the range specified in Table 4, it can be judged that there is a corresponding measured object in the sample.
Table 4 The maximum allowable deviation of relative ion abundance during qualitative confirmation
Relative ion abundance/% ＞ 50 ＞ 20~50 ＞ 10~20 ≤ 10
Maximum allowable deviation/% ±20 ±25 ±30 ±50
6.2.4 Quantitative determination
Draw a standard working curve with the peak area of the target compound as the ordinate and the concentration as the abscissa, and quantify by external standard method. Standard working solution
The response value of the analyte in the sample solution should be within the linear response range of the instrument. If the content exceeds the range of the standard curve, use acetonitrile (4.2)
Analyze after diluting to appropriate concentration. Under the above chromatographic conditions, refer to Appendix A for the multiple reaction monitoring (MRM) chromatogram of the standard solution
Figure A.1.
6.2.5 Blank test
Except that no sample is added, all follow the above steps.
6.3 Result calculation
Calculate the content of the substance to be tested in the sample according to formula (1).
6.4 Precision
6.4.1 Repeatability
The same operator uses the same instrument to perform normal and correct experimental methods for the same substance under constant experimental conditions.
The difference between the two consecutive measurement results obtained is not more than 10% of the arithmetic mean of the two measurement values.
6.4.2 Reproducibility
In different laboratories, the same operator uses the same equipment and uses the same test method to test the same object in parallel twice.
The absolute difference of the determined result is not more than 15% of the arithmetic mean of the two measured values.
Appendix A
(Informative appendix)
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