Some standard content:
HG3630--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 for 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 the 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 Minyi, Ma Yaguang, Xing Jun, and Wu Zhijian. 1265
Chemical Industry Standard of the People's Republic of China
High-efficiency flucythrin technical concentrate
Beta-cypermethrin technical concentrate The other names, structural formulas and basic physicochemical parameters of the active ingredient of this product, high-efficiency cypermethrin, are as follows: ISO Generic name: Beta-cypermethrinCIPAC digital code: 332
HG3630-1999
Chemical name: (S)-α-Cyano-3-phenoxybenzyl (1R, 3R)-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate and (R)-α-Cyano-3-phenoxy (1S, 3S)-3-(2,2-difluorovinyl)-2,2-dimethylcyclopropanecarboxylate and (S)-α-Cyano-3-phenoxyphenyl (1R, 3S)-3-(2,2-difluorovinyl)-2,2-dimethylcyclopropanecarboxylic acid Ester and (R)-α-cyano-3-phenoxyphenyl (1S, 3R)-3-(2,2-difluorovinyl)-2,2-dimethylcyclopropanecarboxylate Structural formula:
(S)(1R, 3R)-isomer
(R)(1S, 3S)-isomer
(S)(1R, 3S)-isomer
(R)(1S, 3R)-isomer
National Petroleum and Chemical Industry Week 1999-06-16 Approved 1266
2000-06-01 Implementation
Empirical formula: C22H1gC12NO3
HG 3630-1999
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 acid, ketone and 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
1 Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of highly effective cypermethrin technical concentrate. This standard applies to highly effective cypermethrin technical concentrate composed of highly effective cypermethrin and impurities generated during its production. 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 are subject to revision, 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 in pesticides GB/T 1601—1993 Determination of pH value in pesticides GB/T1604—1995 Acceptance rules for commercial pesticides GB/T1605—1979 (1989) Sampling methods for commercial pesticides GB3796—1983 General rules for pesticide packaging
3 Requirements
3.1 Appearance: Stable homogeneous transparent liquid. 3.2 High-efficiency cypermethrin technical concentrate shall meet the requirements of Table 1. Table 1 Control Items of High-efficiency Cypermethrin Technical Concentrate Index Items
High-efficiency Cypermethrin Content, %
Moisture Content, %
4 Test Method
4.1 Sampling
Perform according to the "emulsifiable concentrate and liquid state" method in GB/T1605-1979 (1989). The sampling packages are determined by the random number table method, and the final sampling volume should be no less than 100mL.
4.2 Identification Test
4.2.1 High-performance liquid chromatography: This identification test can be carried out simultaneously with the determination of high-efficiency flucythrinate content. 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 high-cis-isomer and high-trans-isomer chromatographic peaks of high-efficiency flucythrinate 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).
HG 36301999
Figure 1 Infrared spectrum of the standard sample of highly effective cypermethrin 4.3 Determination of highly effective cypermethrin 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 n-hexane/anhydrous ether is used as the mobile phase. A stainless steel column with silica gel as the filler and an ultraviolet detector (230 nm) are used to separate and determine the highly effective cypermethrin in the sample by normal phase high performance liquid chromatography. 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. High-efficiency cypermethrin standard sample: known content, greater than or equal to 99.0%. 4.3.1.3 Instruments and equipment
High-performance liquid chromatograph: with variable wavelength UV 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: 5μL.
Ultrasonic cleaner.
Filter: The pore size of the filter membrane is about 0.5 μm. 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: 230 nm.
Injection volume: 5μL.
Retention time (min):
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 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 1268
4.3.1.5 Determination steps
HG 3630—1999
1-Low efficiency cis; 2-High efficiency cis; 3-Low efficiency trans; 4-High efficiency trans Figure 2 High performance liquid chromatogram of high efficiency flucyanate technical concentrate (external standard method) a) Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of high efficiency chlorpyrifos standard, place it in a 50mL volumetric flask, dissolve and dilute to the scale with n-hexane, and shake well.
b) Preparation of sample solution
Weigh a sample containing 0.05 g (accurate to 0.000 2 g) of highly effective cypermethrin, place it in a .50 mL volumetric flask, dissolve it with n-hexane and dilute it to the mark, and shake it.
c) Determination
Under the above operating conditions, after the baseline of the instrument is stable, continuously inject several injections of standard solution until the peak area change of highly effective cypermethrin (highly effective cis + highly effective 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 highly effective cypermethrin (highly effective cis + highly effective trans) in the two injections of sample solution and the peak areas of highly effective cypermethrin (highly effective cis + highly effective trans) in the two injections of standard solution before and after the sample. The highly effective cypermethrin content expressed as mass percentage (X,) is calculated according to formula (1): Xr
wherein: A1 — the average peak area of cypermethrin (high-efficiency cis + high-efficiency trans) in the standard solution, the average peak area of cypermethrin (high-efficiency cis + high-efficiency trans) in the sample solution; A2
— the mass of the high-efficiency flucythrinate standard, g, mi-
— the mass of the sample, g,
— the mass fraction of high-efficiency cypermethrin in the standard sample, %. 1
4.3.1.7 Allowable difference
HG 3630—1999
The arithmetic mean is taken as the determination result. The difference between two parallel determination results shall not exceed 0.7%. 4.3.2 High Performance Liquid Chromatography Internal Standard Method (Arbitration Method) 4.3.2.1 Method Summary
The sample is dissolved in a mixed solvent of ethyl acetate/n-hexane containing methyl benzoate (internal standard), and the ethyl acetate/n-hexane mixed solvent is used as the mobile phase. The normal phase liquid spectral separation and determination are carried out on a chromatographic column filled with Hypersil SiO, 5 μum. 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 must 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 15 minutes. Internal standard solution: weigh 3.8g of methyl benzoate into a 1L volumetric flask, dissolve it with the 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 mm × 4.6 mm (id) stainless steel column, filled with HypersilSiO, 5 μm filler. Chromatographic data processor.
Filter: The pore size of the filter membrane is about 0.45 μm.
Quantitative injection tube: 5 μL.
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: 278 nm.
Column temperature: room temperature (temperature change should not exceed 2°C). Injection volume: 5 μL.
Retention time (min):
Methyl benzoate (internal standard) about 4.5;
Low efficiency cis L(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). 5
1--Internal standard; 2-Low cis-isomer: 3-High cis-isomer; 4-Low trans-isomer: 5-High trans-isomerFigure 3 High-efficiency cypermethrin HPLC chromatogram (internal standard method)4.3.2.5 Determination steps
a) Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of high-efficiency flucythrinate standard sample, put it into a 15mL stoppered glass bottle, add 10mL of internal standard solution with a pipette, dissolve and shake well.
b) Preparation of sample solution
HG 3630-1999
Weigh 0.05g (accurate to 0.0002g) of sample containing high-efficiency cypermethrin, put it into a 15mL stoppered glass bottle, add 10mL of internal standard solution with the same pipette as in a), dissolve and shake well. c) Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several injections of standard solution until the relative change of the peak area ratio of the two adjacent injections of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard 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 two injections of sample solution of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard, and the peak area ratio of the two injections of standard solution before and after the sample of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard, respectively. The content of highly effective cypermethrin expressed as mass percentage (X,) is calculated according to formula (2): X, = r2m;P
Wherein: r-
-the average value of the ratio of the peak area of highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the standard solution to the peak area of the internal standard; r2-the average value of the ratio of the peak area of highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the sample solution to the peak area of the internal standard; mt the mass of the highly effective cypermethrin standard, g, m2 the mass of the sample, g;
P-the mass percentage of highly effective cypermethrin in the standard,%. 4.3.2.7 Allowable difference
Take its arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 0.7%. 4.4 Determination of moisture
4.4.1 Determination method
The determination shall be carried out according to the Karl Fischer method in GB/T1600, and it is allowed to use a moisture analyzer with equivalent accuracy. 4.4.2 Allowable difference
Take its arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 0.10%. 4.5 Determination of pH value
Perform according to GB/T1601.
4.6 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 transportation
5.1. The marking, labeling and packaging of highly effective cypermethrin technical concentrate shall comply with the provisions of GB3796. As a highly effective cypermethrin technical concentrate in the circulation field, it shall also have a production license number and trademark. 5.2 Highly effective cypermethrin technical concentrate shall be packaged in clean and dry galvanized iron drums, and the net content of each drum shall not exceed 100kg. 5.3 According to user requirements or ordering agreements, other forms of packaging may be used, but they must comply with the relevant provisions of GB.3796. 5.4 The packages of highly effective cypermethrin technical concentrate should be stored in a ventilated and dry warehouse. 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 toxic substance and can penetrate through the skin. When using it, you should wear protective gloves and a gas mask. After applying the medicine, you should immediately wash it with soap and water. If poisoning is found, 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 highly effective cypermethrin technical concentrate is 1 year from the date of production. 12718; 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). 5
1--Internal standard; 2-Low cis-isomer: 3-High cis-isomer; 4-Low trans-isomer: 5-High trans-isomerFigure 3 High-performance liquid chromatogram of highly effective cypermethrin (internal standard method)4.3.2.5 Determination steps
a) Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of highly effective flucythrinate standard sample, put it into a 15mL stoppered glass bottle, add 10mL of internal standard solution with a pipette, dissolve and shake well.
b) Preparation of sample solution
HG 3630-1999
Weigh 0.05g (accurate to 0.0002g) of sample containing highly effective cypermethrin, put it into a 15mL stoppered glass bottle, add 10mL of internal standard solution with the same pipette as in a), dissolve and shake well. c) Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several injections of standard solution until the relative change of the peak area ratio of the two adjacent injections of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard 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 two injections of sample solution of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard, and the peak area ratio of the two injections of standard solution before and after the sample of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard, respectively. The content of highly effective cypermethrin expressed as mass percentage (X,) is calculated according to formula (2): X, = r2m;P
Wherein: r-
-the average value of the ratio of the peak area of highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the standard solution to the peak area of the internal standard; r2-the average value of the ratio of the peak area of highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the sample solution to the peak area of the internal standard; mt the mass of the highly effective cypermethrin standard, g, m2 the mass of the sample, g;
P-the mass percentage of highly effective cypermethrin in the standard,%. 4.3.2.7 Allowable difference
Take its arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 0.7%. 4.4 Determination of moisture
4.4.1 Determination method
The determination shall be carried out according to the Karl Fischer method in GB/T1600, and it is allowed to use a moisture analyzer with equivalent accuracy. 4.4.2 Allowable difference
Take its arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 0.10%. 4.5 Determination of pH value
Perform according to GB/T1601.
4.6 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 transportation
5.1. The marking, labeling and packaging of highly effective cypermethrin technical concentrate shall comply with the provisions of GB3796. As a highly effective cypermethrin technical concentrate in the circulation field, it shall also have a production license number and trademark. 5.2 Highly effective cypermethrin technical concentrate shall be packaged in clean and dry galvanized iron drums, and the net content of each drum shall not exceed 100kg. 5.3 According to user requirements or ordering agreements, other forms of packaging may be used, but they must comply with the relevant provisions of GB.3796. 5.4 The packages of highly effective cypermethrin technical concentrate should be stored in a ventilated and dry warehouse. 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 toxic substance and can penetrate through the skin. When using it, you should wear protective gloves and a gas mask. After applying the medicine, you should immediately wash it with soap and water. If poisoning is found, 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 highly effective cypermethrin technical concentrate is 1 year from the date of production. 12718; 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). 5
1--Internal standard; 2-Low cis-isomer: 3-High cis-isomer; 4-Low trans-isomer: 5-High trans-isomerFigure 3 High-performance liquid chromatogram of highly effective cypermethrin (internal standard method)4.3.2.5 Determination steps
a) Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of highly effective flucythrinate standard sample, put it into a 15mL stoppered glass bottle, add 10mL of internal standard solution with a pipette, dissolve and shake well.
b) Preparation of sample solution
HG 3630-1999
Weigh 0.05g (accurate to 0.0002g) of sample containing highly effective cypermethrin, put it into a 15mL stoppered glass bottle, add 10mL of internal standard solution with the same pipette as in a), dissolve and shake well. c) Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several injections of standard solution until the relative change of the peak area ratio of the two adjacent injections of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard 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 two injections of sample solution of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard, and the peak area ratio of the two injections of standard solution before and after the sample of highly effective cypermethrin (highly effective cis + highly effective trans) and the peak area ratio of the internal standard, respectively. The content of highly effective cypermethrin expressed as mass percentage (X,) is calculated according to formula (2): X, = r2m;P
Wherein: r-
-the average value of the ratio of the peak area of highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the standard solution to the peak area of the internal standard; r2-the average value of the ratio of the peak area of highly effective cypermethrin (high-efficiency cis + high-efficiency trans) in the sample solution to the peak area of the internal standard; mt the mass of the highly effective cypermethrin standard, g, m2 the mass of the sample, g;
P-the mass percentage of highly effective cypermethrin in the standard,%. 4.3.2.7 Allowable difference
Take its arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 0.7%. 4.4 Determination of moisture
4.4.1 Determination method
The determination shall be carried out according to the Karl Fischer method in GB/T1600, and it is allowed to use a moisture analyzer with equivalent accuracy. 4.4.2 Allowable difference
Take its arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 0.10%. 4.5 Determination of pH valuewwW.bzxz.Net
Perform according to GB/T1601.
4.6 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 transportation
5.1. The marking, labeling and packaging of highly effective cypermethrin technical concentrate shall comply with the provisions of GB3796. As a highly effective cypermethrin technical concentrate in the circulation field, it shall also have a production license number and trademark. 5.2 Highly effective cypermethrin technical concentrate shall be packaged in clean and dry galvanized iron drums, and the net content of each drum shall not exceed 100kg. 5.3 According to user requirements or ordering agreements, other forms of packaging may be used, but they must comply with the relevant provisions of GB.3796. 5.4 The packages of highly effective cypermethrin technical concentrate should be stored in a ventilated and dry warehouse. 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 toxic substance and can penetrate through the skin. When using it, you should wear protective gloves and a gas mask. After applying the medicine, you should immediately wash it with soap and water. If poisoning is found, 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 highly effective cypermethrin technical concentrate is 1 year from the date of production. 1271
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