HG 3631-1999 4.5% highly effective cypermethrin emulsifiable concentrate
Some standard content:
HG3631--1999
The product quality control items and analytical methods for active ingredient content determined in this standard are formulated with reference to the pesticide specifications of the Food and Agriculture Organization of the United Nations (FAO) and the liquid chromatography analytical method of cypermethrin of the Council for International Pesticide Analysis Cooperation (CIPAC), and in combination with the actual situation of domestic production.
This standard is proposed by the Policy and Regulations Department of the State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of Shenyang Institute of Chemical Industry. The main drafting unit of this standard: Shenyang Institute of Chemical Industry. The participating drafting units of this standard: Zhongshan Kaida Fine Chemical Co., Ltd. and Tianjin Pesticide Co., Ltd. The main drafters of this standard; Jiang Yi, Ma Yaguang, Xing Jun, Wu Zhijian. 1272
Chemical Industry Standard of the People's Republic of China
4.5% Beta-cypermethrin EC
4.5% Beta-cypermethrin Other names, structural formulas and basic physical and chemical parameters of emulsifiable concentrates are as follows: ISO common name: Beta-cypermethrin CIPAC digital code: 332
HG3631—1999
Chemical name: (S)-α-cyano-3-phenoxybenzyl (1R, 3R)-3-(2,2-difluorovinyl)-2,2- Dimethylcyclopropanecarboxylate and (R)-α-cyano-3-phenoxyphenyl (1S, 3S)-3~(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate and (S)-α-cyano-3-phenoxybenzyl (1R, 3S)-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate and (R)-α-cyano-3-phenoxybenzyl (1S, 3R)-3-(2,2-difluorovinyl)-2,2-dimethyl Cyclopropanecarboxylate Structural formula:
(S)(1R,3R)-isomer
(R)(1S,3S)-isomer
(S)(1R,3S)-isomer
(R).(1S,3R)isomer
Approved by the State Administration of Petroleum and Chemical Industry on 1999-06-16CN
Implemented on 2000-06-01
Empirical formula: C22H1gCl 2NO
HG3631-1999
Relative molecular weight: 416.31 (according to the 1993 international relative atomic mass) Biological activity: insecticidal
Melting point: 63~65℃
Solubility (g/L, 20℃): 1×10-5 in water; 9 in hexane; 370 in xylene, easily soluble in alcohol, ketone, aromatic hydrocarbons Stability: diastereomerization occurs under alkaline conditions, and hydrolysis occurs in strong alkaline media. Stable under weak acid and neutral conditions, stable to air and sunlight, and good thermal stability.
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of 4.5% highly effective cypermethrin emulsifiable concentrate. This standard applies to 4.5% highly effective cypermethrin emulsifiable concentrate prepared by dissolving the highly effective flucythrinate technical drug that meets the standard with an emulsifier in a suitable solvent.
2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T1600—1979 (1989) Determination of moisture content of pesticides GB/T 1601-1993 Determination of pH value of pesticides GB/T1603—1979 (1989) Determination of stability of pesticide emulsions GB/T1604—1995 Acceptance rules for commercial pesticides GB/T1605—1979 (1989) Sampling methods for commercial pesticides GB3796—1983 General rules for pesticide packaging
GB4838-1984 Packaging of emulsifiable concentrate pesticides
3 Requirements
3.1 Appearance: Stable homogeneous liquid, without visible suspended matter and sediment. 3.24.5% highly effective cypermethrin emulsifiable concentrate shall meet the requirements of Table 1. Table 14.5% highly effective flucythrinate emulsifiable concentrate control items Index items
Highly effective cypermethrin content, %
Water content, %
Emulsion stability (diluted 200 times)
Low temperature stability
Hot storage stability
Note: Low temperature stability and hot storage stability tests shall be conducted at least once every 6 months 4 Test methods
4.1 Sampling
Perform according to the "sampling of emulsions and liquid states" method in GB/T1605-1979 (1989). The sampled packages are determined by the random number table method 1274
pieces, and the final sampling volume shall be no less than 100mL. 4.2 Identification test
HG 3631—1999
4.2.1 High performance liquid chromatography: This identification test can be carried out simultaneously with the determination of the content of highly effective cypermethrin. Under the same chromatographic operating conditions, the relative difference between the retention time of two chromatographic peaks in the sample solution and the retention time of the highly effective cis- and highly effective trans-chromatographic peaks of highly effective cypermethrin in the standard solution should be within 1.5%. 4.2.2 Infrared spectroscopy: There should be no significant difference in the infrared spectra of the separated sample and the standard sample in the wave number range of 4000-400 cm-1 (see Figure 1.
Figure 1 Infrared spectrum of highly effective cypermethrin standard sample 4.3 Determination of highly effective cyanamide content
4.3.1 High performance liquid chromatography external standard method
4.3.1.1 Method summary
The sample is dissolved in n-hexane, and a mixed solvent of n-hexane/anhydrous ether is used as the mobile phase. A stainless steel column filled with silica gel and an ultraviolet detector (230 nm), and the highly effective nitrogen fluthrin in the sample was analyzed and determined by normal phase HPLC. 4.3.1.2 Reagents and solutions
N-hexane: chromatographic grade.
Anhydrous ether.
Mobile phase: n-hexane + anhydrous ether = 98 + 2 (volume ratio), the mobile phase is filtered through a filter membrane and degassed in an ultrasonic bath for 20 minutes. Highly effective chlorpyrifos standard: known content, greater than or equal to 99.0%. 4.3.1.3 Instruments and equipment
High performance liquid chromatograph: with variable wavelength ultraviolet detector. Chromatographic column: 150 mm × 3. 9 mm (id) stainless steel column, filled with Nova-Pak SiOz5 μm filler. Chromatographic data processor.
Quantitative injection tube: 5 μL.
Ultrasonic cleaner.
Filter: The pore size of the filter membrane is about 0.5μm. 4.3.1.4 High performance liquid chromatography operating conditions
Mobile phase: n-hexane + anhydrous ether + 98 + 2 (volume ratio). Flow rate: 1. 0 mL/min.
Column temperature: room temperature.
Detection wavelength: 230nm.
Injection volume: 5μL.
Retention time (min):
HG 3631—1999
Low efficiency cis [(R)-α, (1R)-cis + (S)-α (1S)-cis about 5.2; high efficiency cis [(S)-α, (1R)-cis + (R)-α, (1S)-cis 7 about 5.9; low efficiency trans [(R)-α, (1R)-trans + (S)-α, (1S)-trans about 6.7; high efficiency trans [(S)-α, (1R)-trans + (R)-α, (1S)-trans] about 7.5. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect (see Figure 1 Low efficiency cis, 2 1—High-efficiency anti-form; 3—Low-efficiency trans-form; 4—High-efficiency trans-form Figure 2 High-efficiency cypermethrin HPLC chromatogram (external standard method) 4.3.1.5 Determination steps
a) Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of high-efficiency cypermethrin standard, place it in a 50mL volumetric flask, dissolve it with n-hexane and dilute it to the mark, and shake it well.
b) Preparation of sample solution
Weigh 0.05g (accurate to 0.0002g) of sample containing high-efficiency cypermethrin, place it in a 50mL volumetric flask, first add a few drops of chloroform to dissolve it, then dissolve it with n-hexane and dilute it to the mark, and shake it well. c) Determination
Under the above operating conditions, after the instrument baseline is set, inject several injections of standard solution continuously until the relative change in the peak area of cypermethrin (high-efficiency cis + high-efficiency trans) between two adjacent injections is less than 1.5%, and then perform determination in the order of standard solution, sample solution, sample solution, and standard solution.
4.3.1.6 Calculation
Average the peak areas of the two sample solutions (high-efficiency cis + high-efficiency trans) and the peak areas of the two standard solutions (high-efficiency cis + high-efficiency trans) before and after the sample. 1276
HG 3631—1999
The high-efficiency cypermethrin content (X1) expressed as mass percentage is calculated according to formula (1): AzmiP
-the average value of the peak area of high-efficiency cypermethrin (high-efficiency cis + high-efficiency trans) in the standard solution; Where: A,
the average value of the peak area of high-efficiency cypermethrin (high-efficiency cis + high-efficiency trans) in the sample solution; A2
m1—-the mass of the high-efficiency cypermethrin standard sample, g; m2——the mass of the sample, g;
-the mass percentage of high-efficiency cypermethrin in the standard sample, %. 4.3.1.7 Allowable difference
Take the arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 0.2%. 4.3.2 High performance liquid chromatography internal standard method (arbitration method) 4.3.2.1 Method summary
The sample is dissolved in ethyl acetate/n-hexane mixed solvent containing methyl benzoate (internal standard), and the ethyl acetate/n-hexane mixed solvent is used as the mobile phase. The normal phase high performance liquid chromatography separation and determination are carried out on a chromatographic column filled with Hypersil SiO, 5 μm. 4.3.2.2 Reagents and solutions
Highly effective cypermethrin standard: known content, greater than or equal to 99.0%. Internal standard: methyl benzoate, which shall not contain impurities that interfere with the analysis. N-hexane: chromatographic grade.
Ethyl acetate: chromatographic grade.
Mobile phase: n-hexane + ethyl acetate-99+1 (volume ratio), filtered through a 0.45μm filter membrane and ultrasonicated for 15min. Internal standard solution Weigh 3.8g of methyl benzoate in a 1L volumetric flask, dissolve it with mobile phase and shake it to volume. 4.3.2.3 Instruments and equipment
High performance liquid chromatograph: with variable wavelength detector. Chromatographic column: 200 mmX4.6 mm (id) stainless steel column, filled with Hypersil SiO, 5 μm filler. Chromatographic data processor.
Filter: The pore size of the filter membrane is about 0.45μm.
Quantitative injection tube: 5μL.
4.3.2.4 Liquid chromatography operating conditions
Mobile phase: n-hexane + ethyl acetate-99+1 (volume ratio). Flow rate: 1.0 mL/min.
Detection wavelength: 278nm.
Column temperature: room temperature (temperature change should not exceed 2°C). Injection volume: 5uL.
Retention time (min):
Methyl benzoate (internal standard) about 4.5;
Low efficiency cis [(R)-α, (1R)-cis + (S)-α, (1S)-cis] about 7.8; high efficiency cis [(S)-α, (1R)-cis + (R)-α, (1S)-cis about 9.2; low efficiency trans [(R)-α, (1R)-trans + (S)-α, (1S)-trans about 10.3; high efficiency trans [(S)-α, (1R)-trans + (R)-α, (1S)-trans about 11.3. The above operating conditions can be adjusted appropriately according to different instruments to obtain the best effect (see Figure 3). 1277
4.3.2.5 Determination steps
HG3631—1999
1—Internal standard; 2—Low-efficiency cis-form 3—High-efficiency cis-form; 4—Low-efficiency trans-form; 5—High-efficiency trans-form Figure 3 High-efficiency cypermethrin HPLC chromatogram (internal standard method) a) Preparation of standard solution
Weigh 0.05 g (accurate to 0.0002 g) of high-efficiency cypermethrin standard sample, put it into a 15 mL stoppered glass bottle, add 10 mL of internal standard solution with a pipette, dissolve and shake.
b) Preparation of sample solution
Weigh 0.05 g (accurate to 0.0002 g) of sample containing high-efficiency cypermethrin, put it into a 15 mL stoppered glass bottle, add 10 mL of internal standard solution with the same pipette as in a), dissolve and shake. c) Determination
Under the above operating conditions, after the instrument baseline is stable, inject several injections of standard solution continuously until the relative change of the peak area ratio of the high-efficiency cypermethrin (high-efficiency cis + high-efficiency trans) and the peak area ratio of the internal standard in two adjacent injections is less than 1.5%, and then perform determination in the order of standard solution, sample solution, sample solution, and standard solution. 4.3.2.6 Calculation
Average the peak area ratio of the high-efficiency cypermethrin (high-efficiency cis + high-efficiency trans) and the peak area ratio of the internal standard in the two injections of sample solution and the peak area ratio of the high-efficiency flucythrin (high-efficiency cis + high-efficiency trans) and the peak area ratio of the internal standard in the two injections of standard solution before and after the sample. The content of highly effective cypermethrin (X2) expressed as mass percentage is calculated according to formula (2): X2 = r2m;P
· (2)
is the average value of the peak area ratio of highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the standard solution and the peak area ratio of the internal standard; where; ri
r2 is the average value of the peak area ratio of the highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the sample solution and the peak area ratio of the internal standard; m) is the mass of the highly effective cypermethrin standard, g;
mz is the mass of the sample, g,
P is the mass percentage of highly effective cypermethrin in the standard sample, %. 4.3.2.7 Allowable difference
Take the arithmetic mean as the determination result. The difference between two parallel determination results should not exceed 0.2%. 4.4 Determination of moisture
4.4.1 Determination method
Carry out according to the Karl Fischer method in GB/T1600. It is allowed to use a moisture meter with equivalent accuracy. 4.4.2 Allowable difference
Take the arithmetic mean as the determination result. The difference between two parallel determination results should not exceed 0.15%. 4.5 Determination of pH value
Carry out according to GB/T1601.
4.6 Test of emulsion stability
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the surface and no precipitation on the bottom. 4.7 Low temperature stability test
4.7.1 Method summary
HG 3631—1999
The sample is kept at 0℃ for 1h, and the precipitation of solid and oily matter is recorded. Continue to store at 0℃ for 7 days, centrifuge and separate, let the solid precipitate settle, and record its volume.
4.7.2 Instruments and equipment
Refrigerator: (0±1)℃.
Centrifuge tube: 100mL, the scale on the bottom of the tube is accurate to 0.05mL. Centrifuge: Matching with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL sample and add it to the centrifuge tube, cool it to (0±1)℃ in the refrigerator, keep the centrifuge tube and its contents at (0±1)℃ for 1h, stir once every 15min, each time for 15s, check and record whether there is solid or oily precipitation. Put the centrifuge tube back into the refrigerator and continue to place it at (0±1)℃ for 7d. After 7 days, take out the centrifuge tube, let it stand for 3 hours at room temperature (not exceeding 20℃), and centrifuge for 15 minutes (the relative centrifugal force at the top of the tube is 500-600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL), and the precipitate is qualified if it does not exceed 0.3mL. 4.8 Thermal stability test
4.8.1 Instruments and equipment
Constant temperature box (or constant temperature water bath): (54±2)℃. Bottle (or glass bottle with a stopper that can still be sealed at 54℃). Medical syringe: 50 mL.
4.8.2 Test steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and seal it with a high-temperature flame (to avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed container in a metal container, and then place the metal container in a constant temperature box for 14 days. Take it out, wipe the outside of the container clean and weigh it separately. For samples with unchanged mass, test the specified items within 24 hours. The content of highly effective cypermethrin after storage shall not be less than 95% of the content measured before storage, and the lower limit of pH value shall not be less than 3.5. 4.9 Inspection and acceptance of products
Inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportationbZxz.net
5.1 The marking, labeling and packaging of 4.5% highly effective cypermethrin emulsifiable concentrate shall comply with the relevant provisions of GB3796 and GB4838, and shall have a production license (production permit) number and trademark. 5.24.5% highly effective flucythrinate emulsifiable concentrate shall be packaged in glass bottles or high-viscosity ester bottles with inner stoppers and bottle caps. The net content of each bottle is 100, 250, 450, or 500 mL. The bottles shall be closely packed in plastic or wooden boxes with leather covers, corrugated paper, or foam plastic pads. The net content of each box shall not exceed 10 kg.
5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 4.5% highly effective cypermethrin emulsifiable concentrate packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: This product is a moderately toxic insecticide that can penetrate through the skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of 4.5% highly effective cypermethrin emulsifiable concentrate is 2 years from the date of production. 1279
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