Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2611-94
Methomyl technical
Published on April 4, 1994
Ministry of Chemical Industry of the People's Republic of ChinaWww.bzxZ.net
Implemented on October 1, 1994
Chemical Industry Standard of the People's Republic of China
Other names, structural formulas and basic physicochemical parameters of methomyl are as follows: ISO common name: Methomyl
CIPAC digital code: 264
Chemical name: 1-(Methylthio)ethylideneaminomethylcarbamate Structural formula:
CH:NH-COO-N = CSCHs
Empirical formula: CH10N20,S
Relative molecular mass: 162.2 (according to the 1989 international relative atomic mass) Biological properties: systemic insecticide
Melting point: 78~79℃
Vapor pressure (25℃): 666.6×10-5Pa
Solubility (g/L, 25℃): water 58; methanol 1000; acetone 730; ethanol 420. HG2611-94
Stability: stable in solid state, stable in neutral and slightly acidic media, slowly decomposed in alkaline solution, and easily decomposed in moist soil. 1 Subject content and scope of application
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage requirements of methomyl technical. This standard applies to methomyl technical composed of methomyl technical and impurities generated during production, which shall be free of foreign impurities and added modifiers.
2 Reference standards
GB/T601 Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB/T1600 Determination of moisture content in pesticides
GB/T1601 Determination of pH value of pesticides
Pesticide acceptance rules
GB/T1604
Commercial pesticide sampling methods
GB/T1605
GB3796 General rules for pesticide packaging
3 Technical conditions
3.1 Appearance: This product should be white to light yellow crystalline powder. 3.2 The technical material of methomyl shall meet the following requirements: Approved by the Ministry of Chemical Industry of the People's Republic of China on April 4, 1994, and implemented on October 1, 1994
Methomyl content, %(m/m)
Water, %(m/m)
Acetone insoluble matter, %(m/m)
4 Test method
HG2611-94
Superior quality
Unless otherwise specified, the reagents used in this test are all analytically pure, and the water meets the requirements of grade 3 water in GB/T6682. 4.1 Determination of methomyl
4.1.1 Identification test
Qualified product
Liquid chromatography This identification test can be carried out simultaneously with the determination of methomyl content. The retention time of the main chromatographic peak of the sample solution and the retention time of methomyl in the standard solution under the same conditions should have a deviation within 1.5%. Infrared spectroscopy: Infrared scanning is performed in the wave number range of 200 to 4000 cm-1. There should be no significant difference in the infrared absorption spectra of the sample and the standard sample.
4.1.2 Determination of methomyl content
4.1.2.1 High performance liquid chromatography internal standard method (arbitration method)4.1.2.1.1 Method summary
The sample is dissolved in methanol, ethylene glycol phenyl ether is used as the internal standard, methanol + water (40 + + 60) is used as the mobile phase and the ultraviolet detector (225nm) is used to determine the methomyl technical by reverse phase liquid chromatography. 4.1.2.1.2 Reagents and solutions
Methanol (GB/T683), filtered through a G5 glass sand core filter funnel; Methomyl standard sample: known content ≥98.0% m/m); internal standard: ethylene glycol phenyl ether, which should not contain impurities that interfere with analysis; water: freshly made double distilled water;
Internal standard solution: 3.7g ethylene glycol phenyl ether methanol solution. 4.1.2.1.3 Instruments
High performance liquid chromatograph: with variable wavelength UV detector; Chromatographic column: 20cmX4.6mm (ID) stainless steel column, filled with Spherisorb Cs (30/127) 10um (or other brands of C, C18 bonded stationary phase), the number of theoretical plates per meter should not be less than 30,000; filter: the pore size of the filter membrane is about 0.45um;
Injector: 50uL;
Chromatographic processor.
4.1.2.1.4 Chromatographic operating conditions
Mobile phase: methanol + water = 40 + 60 (V/V); Flow rate: 1mL/min;
Column temperature: room temperature ± 2°C;
Detection wavelength, 225nm;
Sensitivity: 0.05 full scale absorbance unit; Injection volume: 10uL;
Retention time: methomyl 4.1min; ethylene glycol phenyl ether 7.2min. The above liquid chromatography conditions are typical operating parameters. The operating parameters can be appropriately adjusted according to the characteristics of the instrument to obtain the best effect. 2
4.1.2.1.5 Determination steps
a. Preparation of standard solution
HG2611—94
Figure 1 High performance liquid chromatography of methomyl technical
1-Methhomyl; 2-Ethylene glycol phenyl ether
Weigh about 0.10g (accurate to 0.0002g) of methomyl standard sample and place it in a 50mL volumetric flask, dilute to the mark with methanol, and shake well. Accurately transfer 10mL of the solution to a 50mL volumetric flask, add 10mL of internal standard solution with a pipette, dilute to the mark with methanol, and shake well. b. Preparation of sample solution
Weigh about 0.10g of sample containing methomyl (accurate to 0.0002g), place it in a 50mL volumetric flask, dilute to the mark with methanol, and shake well. Accurately transfer 10mL of the solution to a 50mL volumetric flask, add 10mL of internal standard solution with a pipette, dilute to the mark with methanol, and shake well. c. Determination
Under the selected chromatographic conditions, after the instrument is stable, repeat the injection of the standard solution and calculate the repeatability of the relative response values of each needle. When the relative response value of two adjacent needles changes less than 1%, perform liquid chromatography analysis in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
4.1.2.1.6 Calculation
Average the measured ratios of the peak areas of methomyl to the internal standard in a, d and b, c respectively. The mass percentage X of methomyl is calculated according to formula (1):
X,= 72m;P
Wherein: - the average value of the peak area ratio of methomyl to the internal standard in the standard solution; r2 - the average value of the peak area ratio of methomyl to the internal standard in the test solution; m1 - the mass of the standard, g;
m2 - the mass of the test sample, g;
P - the percentage content of the standard, (m/m). 4.1.2.1.7 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1%. Take the average value as the result. (1)
4.1.2.2 HPLC external standard method
4.1.2.2.1 Method summary
HG2611-94
The sample was dissolved in methanol, and the methomyl technical was separated and determined by reversed phase liquid chromatography using methanol + water (40 + 60) as the mobile phase and a UV detector (235nm).
4.1.2.2.2 Reagents
Methanol (GB/T683), filtered through a G5 glass frit filter funnel; methomyl standard sample: known content ≥ 98.0% (m/m); water: freshly prepared double distilled water.
4.1.2.2.3 Instruments
High performance liquid chromatograph: with variable wavelength UV detector; Chromatographic column: 20cm×4.6mm (ID) stainless steel column, filled with SpherisorbCa (30/127) 10um, or other brands of Cs, C1a bonded stationary phase;
Filter: filter membrane pore size is about 0.45um;
Injector: 50uL.
4.1.2.2.4 Chromatographic operating conditions
Mobile phase: methanol decahydrate = 40+60 (V/V); Flow rate: 1mL/min;
Detection wavelength, 235nm;
Column temperature: room temperature ± 2℃;
Injection volume: 10uL;
Retention time: methomyl: 4.1min.
The above HPLC operating conditions are typical operating parameters. The operating parameters can be adjusted appropriately according to the characteristics of different instruments to obtain the best results.
Figure 2 HPLC chromatogram of methomyl technical
4.1.2.2.5 Determination steps
a. Preparation of standard solution
Weigh about 0.10g of methomyl standard (accurate to 0.0002g), placed in a 50mL volumetric flask, diluted to the mark with methanol, and shake well. Accurately transfer 10mL of the above solution to a 50mL volumetric flask, dilute to the mark with methanol, and shake well. b. Preparation of sample solution
HG 261194
Weigh a sample of the original drug containing about 0.10g of methomyl (accurate to 0.0002g), place it in a 50mL volumetric flask, dilute to the mark with methanol, and shake well. Accurately transfer 10mL of the above solution to a 50mL volumetric flask, dilute to the mark with methanol, and shake well. c. Determination
Under the above operating conditions, after the instrument is stable, continuously inject several needles of standard solution, calculate the repeatability of the relative response value of each needle, and when the relative response value of two adjacent needles changes by less than 1%, perform liquid chromatography analysis in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard sample solution.
4.1.2.2.6 Calculation
Average the peak areas of methomyl in a, d and b, c respectively, and calculate the mass percentage of methomyl X2 according to formula (2): X2
In the formula, A1 is the average value of the peak area of methomyl in the standard sample solution; A2 is the average value of the peak area of methomyl in the sample solution; m1-
the mass of the methomyl standard sample, 8;
the mass of the methomyl sample, g;
P is the percentage of the methomyl standard sample, (m/m). 4.1.2.2.7 Allowable difference
The difference between the results of two parallel determinations should not be greater than 1%. Take the average value as the result. 4.2 Determination of moisture
Determine according to GB/T1600 (it is allowed to use a trace moisture meter with equivalent accuracy for determination). 4.3 Determination of pH value
Determination shall be carried out in accordance with GB/T1601.
4.4 Determination of acetone insoluble matter
4.4.1 Reagents
Acetone (GB/T686), chemically pure.
4.4.2 Apparatus
Erlenmeyer flask: 250mL;
Gooch crucible or glass sand core crucible: No. 3;
Oven: 110℃.
4.4.3 Determination steps
Weigh 10g of sample (accurate to 0.01g) and put it into an Erlenmeyer flask, add 40mL of acetone, and shake the Erlenmeyer flask until all soluble matter is dissolved. Filter out the solution with a crucible that has reached a constant weight, then wash the Erlenmeyer flask with 60mL of acetone three times, and filter it by suction. Dry it in an oven at 110℃ for 30min, take it out, cool it to room temperature, and weigh it. The mass percentage of acetone insoluble matter Xs is calculated according to formula (3): ml-mo×100
Wherein: m1——the mass of the crucible and insoluble matter after constant weight, g; mo———the mass of the crucible, g;
m——the mass of the sample, g.
5 Inspection rules
5.1 Sampling method
HG2611—94
Sampling is carried out in accordance with the "raw powder sampling" method in GB/T1603. The sampling package is determined by random method; the final sampling volume should be not less than 250g.
5.2 Acceptance rules
Acceptance is carried out in accordance with GB/T1604 standard.
6 Marking, packaging, transportation and purchase and storage
6.1 The marking and packaging of methomyl technical shall comply with the relevant provisions of GB3796 and shall be marked with a trademark. 6.2 The original drug of methomyl should be packaged in iron barrels, wooden barrels or woven bags lined with plastic bags, and the net weight of each barrel (bag) should not exceed 50kg. 6.3 During transportation and storage, it should be strictly protected from moisture and sunlight, and good ventilation should be maintained. It should not be mixed with food, seeds, and feed, and should avoid contact with the skin and prevent inhalation through the mouth and nose.
6.4 The package should be stored in a ventilated and dry warehouse. 6.5 Safety: In addition to the corresponding toxicity mark on the instruction manual or packaging container, there should also be the following description of toxicity: Methomyl is a highly toxic carbamate insecticide, which is toxic if inhaled and can be fatal if swallowed. When using this product, avoid direct contact with the skin and eyes, and do not inhale dust and spray. All operations should be carried out in a ventilated place, and appropriate protective measures should be taken for the skin and eyes. In case of contact, rinse with water for 15 minutes, then wash the skin with soap and water, and receive medical treatment. Atropine is a special antidote. Additional Notes:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and Shandong Pesticide Research Institute and Jining Chemical Experimental Plant participated in the drafting. The main drafters of this standard are Zhao Xinxin, Liu Guoxiu, Zhang Xiaobo, Wu Yanfeng, Zhu Jianhua, and Hua Peilin.5 Safety: In addition to the corresponding toxicity mark, the following toxicity instructions should be included in the instructions for use or packaging containers: Methomyl is a highly toxic carbamate insecticide, which is toxic if inhaled and fatal if swallowed. Avoid direct contact with skin and eyes when using this product, and do not inhale dust and spray. All operations should be carried out in a ventilated area, and appropriate protective measures should be taken for skin and eyes. In case of contact, rinse with water for 15 minutes, then wash the skin with soap and water, and seek medical treatment. Atropine is a specific antidote. Additional instructions:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry, and Shandong Pesticide Research Institute and Jining Chemical Experimental Plant participated in the drafting. The main drafters of this standard are Zhao Xinxin, Liu Guoxiu, Zhang Xiaobo, Wu Yanfeng, Zhu Jianhua, and Hua Peilin. 65 Safety: In addition to the corresponding toxicity mark, the following toxicity instructions should be included in the instructions for use or packaging containers: Methomyl is a highly toxic carbamate insecticide, which is toxic if inhaled and fatal if swallowed. Avoid direct contact with skin and eyes when using this product, and do not inhale dust and spray. All operations should be carried out in a ventilated area, and appropriate protective measures should be taken for skin and eyes. In case of contact, rinse with water for 15 minutes, then wash the skin with soap and water, and seek medical treatment. Atropine is a specific antidote. Additional instructions:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry, and Shandong Pesticide Research Institute and Jining Chemical Experimental Plant participated in the drafting. The main drafters of this standard are Zhao Xinxin, Liu Guoxiu, Zhang Xiaobo, Wu Yanfeng, Zhu Jianhua, and Hua Peilin. 6
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