other information
drafter:Zhao Xinxin, Liu Guoxiu, Zhang Xiaobo, Wu Yanfeng, Zhu Jianhua, Hua Peilin
Drafting unit:Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry, Shandong Pesticide Research Institute, Jining Chemical Experimental Plant
Focal point unit:Technology of Shenyang Chemical Research Institute, Ministry of Chemical Industry
Proposing unit:Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China
Publishing department:Ministry of Chemical Industry of the People's Republic of China
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2612—94
Methomyl EC
Published on April 4, 1994
Ministry of Chemical Industry of the People's Republic of China
Implemented on October 1, 1994
Chemical Industry Standard of the People's Republic of China
Methomyl EC
Subject Content and Scope of Application
HG2612—94
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage requirements for methomyl EC. This standard applies to EC prepared by dissolving methomyl technical and emulsifier in a suitable solvent. Cited standards
GB/T1600
GB/T1601
GB/T1603
GB/T1604
GB/T1605
GB3796
GB4838
HG2611
Technical conditions
Method for determination of moisture content of pesticides
Method for determination of pH value of pesticides
Method for determination of stability of pesticide emulsions
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
Emulsifiable concentrate pesticide packaging
Methamidocarb technical
3.1 Appearance: Homogeneous liquid, without visible suspended matter and precipitation. 3.2 Methomyl emulsifiable concentrate shall meet the following requirements: Item
Methomyl content, %(m/m)
Water, %(m/m)
Emulsion stability (diluted 200 times)
Low temperature stability\)
Hot storage stability\)
Note, 1) Test at least once every 3 months.
Test method
Unless otherwise specified, all reagents used in this test are analytically pure. 4.1 Determination of methomyl
4.1.1 Identification test
Same as 4.1.1 of HG2611.
4.1.2 Determination of methomyl content
4.1.2.1 High performance liquid chromatography internal standard method (arbitration method) Approved by the Ministry of Chemical Industry of the People's Republic of China on April 4, 1994, and implemented on October 1, 1994
4.1.2.1.1 Summary of the method
Same as 4.1.2.1.1 of HG2611.
4.1.2.1.2 Reagents and solutions
Same as 4.1.2.1.2 of HG2611.
4.1.2.1.3 Instruments
Same as 4.1.2.1.3 of HG2611.
4.1.2.1.4 Chromatographic operating conditions
Same as 4.1.2.1.4 of HG2611.
4.1.2.1.5 Determination steps
a. Preparation of standard solution
HG2612—94
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 (accurate to 0.0002g) of methomyl emulsifiable concentrate sample and place it in a 50mL volumetric flask, add 10mL of internal standard solution with a pipette, dilute to the mark with methanol, and shake well. c. Determinationbzxz.net
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the standard solution, calculate the repeatability of the relative response value of each needle, and 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 peak area ratios of methomyl to the internal standard in a, d and b, c respectively, and calculate the mass percentage X1 of methomyl according to formula (1):
Wherein: - the average value of the peak area ratios of methomyl to the internal standard in the standard solution; 72 - the average value of the peak area ratios of methomyl to the internal standard in the test solution; mi
- the mass of the standard, 8;
- the mass of the test sample, g;
- 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 exceed 1%. 4.1.2.2 High Performance Liquid Chromatography External Standard Method
4.1.2.2.1 Method Summary
Same as 4.1.2.2.1 of HG2611.
4.1.2.2.2 Reagents
Same as 4.1.2.2.2 of HG2611.
4.1.2.2.3 Apparatus
Same as 4.1.2.2.3 of HG2611.
4.1.2.2.4 Chromatographic Operating Conditions
Same as 4.1.2.2.4 of HG2611.
4.1.2.2.5 Determination steps
1) Preparation of standard solution
HG2612-94
Weigh about 0.10g (accurate to 0.0002g) of methomyl standard, 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. 2) Preparation of sample solution
Weigh about 0.10g (accurate to 0.0002g) of methomyl emulsifiable concentrate, place it in a 50mL volumetric flask, dilute to the mark with methanol, and shake well. 3) 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 less than 1%, perform liquid chromatography analysis in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
4.1.2.2.6 Calculation
Average the peak areas of methomyl in a, d and b, c respectively, and calculate the mass percentage of methomyl X: according to formula (2): AzmiP
X2-5Aim2
Wherein: A1—average value of the peak area of methomyl in the standard solution; A2—average value of the peak area of methomyl in the sample solution; ml—mass of methomyl standard sample, g;
m2—mass of methomyl sample, g;
P—percentage of methomyl standard sample, (m/m). 4.1.2.2.7 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1% (m/m); take the average value and report it as the result. 4.2 Determination of moisture
Determine according to the Karl Fischer method in GB/T1600 (it is allowed to use a micro-moisture meter with equivalent accuracy). 4.3 Emulsion stability test
Perform according to GB/T1603. It is qualified if there is no floating oil on the top, no sinking oil or precipitation on the bottom. 4.4 Determination of pH value
Determine according to GB/T1601.
4.5 Low temperature stability test
Put 50mL of sample in a 100mL beaker, cool to 0±1℃ by appropriate method, and keep it at this temperature for 1h. During this period, stir slowly with a glass rod from time to time. It is qualified if there is no solid or oily precipitation. 4.6 Thermal storage stability test
4.6.1 Apparatus
Thermostatic box (or 54℃ constant temperature water bath), 54±2℃; Ampoule (or glass bottle with a stopper that can still be sealed at 54℃) 50mL; Medical syringe, 50mL.
4.6.2 Test steps
Use a syringe to inject about 30mL of the emulsifiable concentrate sample into a clean Ampoule (or glass bottle) (avoid the sample from contacting the bottleneck), place the Ampoule in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (to avoid solvent volatilization). Seal at least 2 bottles and weigh them separately. Place the sealed ones in a metal container, and then place the metal container in a 54±2℃ thermostatic box (or water bath) for 14 days. Take out the samples that have not changed in weight and weigh them separately. Test the active ingredient content, moisture, pH value, emulsion stability and other items within 24 hours. The test results show that except for the active ingredient content of 3
HG2612-94
, which can be relatively reduced by 5%, other indicators should meet the standard requirements. 5 Inspection rules
5.1 Sampling method
Follow the "sampling of emulsions and liquid states" in GB/T1605. Determine the sampling package by random method; the final sampling volume should be no less than 250g (or 250mL).
5.2 Acceptance rules
Acceptance shall be conducted in accordance with GB/T1604.
6 Marking, packaging, transportation and purchase and storage
6.1 The marking and packaging of methomyl EC shall comply with the relevant provisions of GB3796 and GB4838. 6.2 Methomyl EC shall be packaged in 250mL or 500mL glass bottles or plastic bottles with inner and outer caps, and the outer packaging shall be in calcium plastic boxes, with the net weight of each box not exceeding 10kg.
6.3 During transportation and storage, moisture and sunlight shall be strictly prevented, good ventilation shall be maintained, and it shall not be mixed with food, seeds, and feed, and contact with the skin shall be avoided, and inhalation through the mouth and nose shall be prevented.
6.4 Packages shall be stored in ventilated and dry warehouses. 6.5 Safety: In addition to the corresponding toxicity mark on the instruction manual or packaging container, the following toxicity description shall also be provided: Methomyl is a highly toxic carbamate insecticide, which is toxic by inhalation and can be lethal. When using this product, avoid direct contact with the skin and eyes, and do not inhale the spray. All operations should be carried out in a ventilated area, 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 seek medical treatment. Atropine is a specific antidote. 6.6 Warranty period: Under the specified storage conditions, the warranty period of methomyl is at least 2 years from the date of production. The content of active ingredients should not be less than 19.7% within one year, and after one year, it should not be less than 19.4% within two years. The moisture, pH value, and emulsion stability should still meet the standard requirements. Additional remarks:
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. 4
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