GB/T 37363.2-2019 English PDF (GB/T37363.2-2019)

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GB/T 37363.2-2019: Determination of biocides content of coating materials - Part 2: Determination of diuron content
GB/T 37363.2-2019
Determination of biocides content of coating materials - Part 2. Determination of diuron content
ICS 87.040
G50
National Standards of People's Republic of China
Determination of biocide content in paints
Part 2. Determination of diuron content
Part 2.Determinationofdiuroncontent
Published on.2019-03-25
2020-02-01 implementation
State market supervision and administration
China National Standardization Administration issued
Foreword
GB/T 37363 "Determination of Biocide Content in Coatings" is divided into the following sections.
--- Part 1. Determination of isothiazolinone content;
--- Part 2. Determination of diuron content;
This part is the second part of GB/T 37363.
This part is drafted in accordance with the rules given in GB/T 1.1-2009.
This part was proposed by the China Petroleum and Chemical Industry Federation.
This part is under the jurisdiction of the National Coatings and Pigments Standardization Technical Committee (SAC/TC5).
This section drafted by. CNOOC Changzhou Coating Chemical Research Institute Co., Ltd., China Shipbuilding Industry Corporation 725th Research Institute Building
Door Materials Research Institute, Zhonghua Paint (Shenzhen) Co., Ltd., Thor Special Chemicals (Zhenjiang) Co., Ltd., AVIC Baimu New Material Technology Engineering
Co., Ltd., Shenzhen Guangtian Environmental Protection Coating Co., Ltd., Hebei Chenyang Industry and Trade Group Co., Ltd., Hebei Jiabaoli Coating Co., Ltd.
Quality of Guangdong Province Zhuhai Quality Measurement Supervision and Inspection Institute, Sanshu Paint Co., Ltd., Shanghai Jianke Inspection Co., Ltd., Heilongjiang Province
Supervised Testing Institute.
The main drafters of this section. Li Jinying, Li Guangdong, Liu Xiaoling, Wu Zhaomin, Sun Lide, Wang Zhi, Zhang Yeping, Xu Xinxiang, Gao Ting, Hu Zhongyuan,
Ye Caiping, Yang Dongmei, Peng Yongsen, Yuan Jun.
Determination of biocide content in paints
Part 2. Determination of diuron content
Cautions - Personnel using this section should have hands-on experience in formal laboratory work. This section does not point out all possible security questions.
question. It is the responsibility of the user to take appropriate safety and health measures and to ensure compliance with the conditions set by the relevant national regulations.
1 Scope
This part of GB/T 37363 specifies the determination of diuron [N-(3,4-dichlorobenzene) in paints by liquid chromatography-mass spectrometry/mass spectrometry.
Principle of base content, reagents and materials, equipment, samples, test procedures, number of tests
According to processing, detection limits, precision, test reports.
This section applies to the determination of diuron content in paints. The determination of the content of diuron in the raw materials for paint film and coating can also refer to this
section.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
GB/T 3186 Paint, varnish and paint and varnish raw materials sampled
GB/T 6682-2008 Analytical laboratory water specifications and test methods
GB/T 12806-2011 laboratory glass instrument single standard line volumetric flask
GB/T 12807-1991 Laboratory glass instrument indexing pipette
GB/T 12808-2015 laboratory glass instrument single line suction tube
3 Principle
The diuron in the sample was extracted by a combination of ultrasonic extraction and centrifugation using methanol as the extraction solvent. After the extract is fixed to volume, use
Liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) was used to quantify retention time and selected ion characterization by external standard method.
Note. Other approved suitable solvents can also be selected as the extraction solvent.
4 reagents and materials
Unless otherwise specified, only reagents identified as analytically pure and above purity and those meeting the requirements of GB/T 6682-2008 are used in the analysis.
First grade water.
4.1 Methanol. Chromatographically pure.
4.2 Ammonium acetate. chromatographically pure.
4.3 Formic acid. chromatographically pure.
4.4 Diuron. The mass fraction is not less than 99%.
4.5 Microporous membrane. pore size 0.22μm.
4.6 Stainless steel metal screen. 0.5mm aperture.
5 instruments
5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometry (LC-MS/MS) with reversed-phase column.
5.2 Ultrasonic extractor. power ≥ 500W.
5.3 High-speed centrifuge. The speed is above 12000r/min, and the temperature can be controlled.
5.4 Balance. Accuracy 0.1mg.
5.5 Volumetric flask. suitable specifications, GB/T 12806-2011A.
5.6 Indexing pipette. suitable size, GB/T 12807-1991A class.
Note. Other pipetting equipment with the same accuracy as the requirements, such as piston pipettes, can also be used.
5.7 Single-line pipette. suitable specifications, GB/T 12808-2015A.
Note. Other pipetting equipment with the same accuracy as the requirements, such as piston pipettes, can also be used.
6 samples
Sampling according to the provisions of GB/T 3186, can also be sampled according to the agreed method, the sampling amount is determined according to the inspection needs.
7 test steps
7.1 Parallel test
Do two tests in parallel.
7.2 Sample preparation
Stir the sample evenly [If the sample is solid, the sample can be pulverized at room temperature with a pulverizing device and used with a pore size of 0.5 mm stainless steel.
Is a sieve (4.6) sieved, weigh about 2.5g of sample, accurate to 0.1mg, placed in a 25mL volumetric flask (5.5), record the mass m of the sample, with a
The alcohol (4.1) was diluted to the mark, and the sample was thoroughly dispersed by shaking to prepare a sample solution, and the volume V was recorded. Ultrasonic
After ultrasonic extraction for 205 minutes, remove about 7 mL of the above solution into the centrifuge tube (or adjust the centrifuge according to the actual situation).
The volume of the solution is centrifuged under the condition that the temperature of the centrifuge chamber does not exceed 25 ° C, and the supernatant A appears in the upper layer. If the centrifugal effect is not good, there is no
Layering can increase the speed or increase the centrifugation time. The supernatant A was filtered with a 0.22 μm microporous membrane (4.5), and the filtrate B was retained for extraction.
Take the solution (7.7).
When selecting other solvents as the extraction solvent, use a single-line pipette (5.7) to remove 1 mL of the clear solution A in a 10 mL volumetric flask (5.5).
Medium, make up to the mark with methanol (4.1). Take appropriate amount of the above solution, filter with 0.22 μm microporous membrane (4.5), and retain filtrate C for extraction.
Determination of the solution (7.7).
7.3 Blank test
The blank test should be performed in parallel with the test and the same test procedure should be used to take the same amount of all reagents, but no sample.
7.4 LC-MS/MS test conditions
Appropriate test conditions are selected based on the performance of the LC-MS/MS used and the actual conditions of the sample.
Since the test results depend on the instrument used, the pervasive parameters for chromatographic and mass spectrometry cannot be given and are listed in Appendix A, A.1.
The parameters have been proven to be applicable to the test.
7.5 Preparation of standard working solution
Weigh about 0.02 g of diuron (4.4) to the nearest 0.1 mg, and dilute to the mark with methanol (4.1) in a 100 mL volumetric flask. Adopt
Step by step dilution method, use the indexing pipette (5.6) or single-line pipette (5.7) to remove the above solution in a suitable volumetric flask (5.5), with a
The alcohol (4.1) is diluted with the above solution to a suitable concentration of diuron standard working solution.
Note 1. The concentration range of diquat standard working solution can be adjusted according to the instrument and sample used.
Note 2. A known concentration of certified diuron standard solution can also be used directly.
7.6 Drawing a standard working curve
The standard working solution of diuron (7.5) was determined by liquid chromatography-mass spectrometry/mass spectrometry. Every standard working solution
Two times, the peak area is averaged, and the relative deviation should be no more than 5%. Record according to quantitative selection of ions and qualifier ions (see Table A.1)
Multi-reaction monitoring (MRM) chromatogram, with the peak area (minus the peak area of diuron in the unspiked working solution) as the ordinate, corresponding standard work
The solution concentration is plotted on the abscissa and the standard working curve is drawn. The standard working curve should include at least 5 diuron standard working solutions (7.5).
The linear correlation coefficient R2 of the standard working curve should be greater than 0.995, otherwise the new standard operating curve should be redrawn.
7.7 Determination of extraction solution
The filtrate B or the filtrate C was tested under the same instrument test conditions as the standard working curve (7.6). Record multiple reaction monitoring (MRM)
Chromatogram, peak area integration for quantitatively selected ions (see Table A.1) (deducting the peak area of diuron in the blank test), using external standard method
Quantitative. If the content of diuron in filtrate B or filtrate C exceeds the standard working curve range, it can be diluted with methanol (4.1).
Take the determination of the solution.
8 test data processing
The content of diuron in the sample is calculated by the mass fraction w of diuron, and the value is expressed in milligrams per kilogram (mg/kg), calculated according to formula (1).
w=ρ×
V×F
(1)
In the formula.
ρ---the mass concentration of diuron read from the standard working curve, in micrograms per milliliter (μg/mL);
V---the volumetric volume of the test solution, in milliliters (mL);
F---the dilution factor of the test solution;
m---The mass of the sample in grams (g).
Calculate the average of the results of the two parallel test tests and report the results as an average. When the measured value is less than 100mg/kg, the result table
One after the decimal point; when the measured value is greater than or equal to 100mg/kg and less than 1000mg/kg, the result is reported as an integer value;
When the fixed value is greater than or equal to 1000 mg/kg, the result is reported by multiplying the three significant digits by the power of the power.
9 Detection limit
The detection limit of diuron was 1 mg/kg.
10 precision
10.1 Repetitive limit (r)
In the same laboratory, the same equipment is used by the same operator, according to the same test method, and the same object is measured in a short time.
The relative deviation between the two test results obtained by testing independently of each other is not more than 10%, and the relative deviation is greater than 10%, and the case is not more than 5%.
As a prerequisite.
10.2 Reproducibility limit (R)
In different laboratories, different operators use different devices, and the same test method is independent of the same test object.
The relative deviation of the two independent test results obtained by the test is not more than 20%, and the relative deviation is greater than 20%, and the case is not more than 5%.
premise.
11 test report
The test report should at least give the following aspects.
---test subject;
--- the extraction solvent used;
---result;
--- Observed anomalies;
--- Test date.
Appendix A
(informative appendix)
Liquid chromatography-mass spectrometry/mass spectrometer reference conditions
A.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer Reference Conditions
A.1.1 Column. C18 reversed phase column, 2.1 mm × 50 mm, 1.8 μm.
A.1.2 Flow rate. 0.3mL/min.
A.1.3 Column temperature. 35 °C.
A.1.4 Injection volume. 1 μL.
A.1.5 Atomizing gas. nitrogen, purity ≥95%.
A.1.6 Drying gas temperature. 350 °C.
A.1.7 Dry gas flow rate. 9L/min.
A.1.8 Atomizing gas pressure. 344737.85Pa (50psi).
A.1.9 Collision gas. high purity nitrogen, purity ≥99.999%.
A.1.10 Mobile phase. water [5mmol/L ammonium acetate, formic acid volume fraction 0.1%] methanol (30 70).
A.1.11 Mass Spectrometry Ion Source. Electrospray ion source (ESI).
A.1.12 Ionization mode. positive ion scanning.
A.1.13 Capillary voltage. 3000V.
A.1.14 Monitoring method. Multiple reaction monitoring (MRM), the monitoring conditions are shown in Table A.1.
Table A.1 Multiple reaction monitoring conditions for diuron
Compound name
Parent ion
m/z
Child ion
m/z
Collision energy
(CE)/eV
De-clustered voltage /
Acceleration voltage /
Diuron
232.8 72.1a 26 105 7
232.8 159.8 18 105 7
a Quantitative product ions.
A.2 Chromatogram of liquid chromatography-mass spectrometry/mass spectrometer
The multi-reaction monitoring (MRM) chromatogram of diuron is shown in Figure A.1.
Figure A.1 Multi-Reaction Monitoring (MRM) chromatogram of diuron