Some standard content:
National Standard of the People's Republic of China
Methamidophos technical
Other names, structural formulas and physicochemical parameters of the active ingredient methamidophos of this product are as follows: IS common name: Methamidophos
CIPAC digital code: 355
Chemical name: O, S-dimethylthiophosphoramide Structural formula:
-P--NH2
Empirical formula: C, HNO, PS
Relative molecular mass: 141.1 (according to the international relative atomic mass in 1991) Biological properties: insecticide
Melting point: 46.1℃
Vapor pressure (20℃): 2.3×10-5Pa
GB 15954-1995
Replaces GB3724-:83
Solubility (g/L, 20℃): water>1000, dichloromethane>1000, n-hexane 0.1～1, octanol 50～100, toluene 2～5, acetone>200
Stability: half-life at 22C: 70h at pH9, 120h at pH7, 1.8a at pH4. Subject content and scope of application
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for methamidophos technical. This standard applies to methamidophos technical composed of methamidophos and impurities generated in its production, which should be free of foreign impurities. 2 Reference standards
GB190 Dangerous goods packaging marking
GB/T 601
GB/T 603
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents Preparation of preparations and products used in test methods of chemical reagents GB/T1250 Methods for expressing and determining limit values Methods for determining moisture content in pesticides
GB/T 1600
Acceptance rules for pesticides
GB/T 1604
GB/T 1605
Sampling methods for commercial pesticides
GB3796 General rules for pesticide packaging
Approved by the State Administration of Technical Supervision on December 21, 1995 and implemented on August 1, 1996
3 Technical requirements
GB 15954--1995
3.1 Appearance: Colorless to light yellow liquid, or crystalline slurry, should be free of foreign impurities. 3.2 Methamidophos technical shall meet the requirements of the following table: Item
Methamidophos content
Acidity (in H,SO),
4 Test method
%, (m/m)
Unless otherwise specified, the reagents used in this test are analytically pure. Water should meet the third-grade water specifications in GB/T682. 4.1 Determination of methamidophos
4.1.1 Identification test
This identification test can be carried out simultaneously with the determination of methamidophos content. The relative difference between the retention time of the main peak of the sample solution and the retention time of methamidophos of the standard solution under the same conditions of HPLC-
should be within 1.5%. TLC: The R value of the main spot obtained by developing the sample solution and the spot of the control standard solution should be consistent. IR: Mix the separated 1 mg methylamidophos sample (standard sample) with 300 mg KBr and press it into a tablet. Scan the infrared spectrum in the wavelength range of 4000-400 cm1. There should be no obvious difference between the infrared spectra of the sample and the standard. 4.1.2 Determination of methylamidophos content
4.1.2.1 High performance liquid chromatography (arbitration method) 4.1.2.1.1 Summary of the method
The sample is dissolved in water, and water + acetonitrile is used as the mobile phase. Reverse phase high performance liquid chromatography separation is performed on a liquid chromatography column filled with 5μm Ci8 or C:, and the content of the effective ingredient is quantified by the peak area of the external standard method. 4.1.2.1.2 Reagents and solutions
Water: freshly distilled water;
Acetonitrile: chromatographic grade;
Mobile phase: water + acetonitrile = 94 + 6, filtered through a G5 glass sand core filter funnel into a dark bottle, sealed, and stored at low temperature; Methylamidophos standard: known content, ≥99.0%. 4.1.2.1.3 Instruments
High performance liquid chromatograph: with variable wavelength UV detector, chromatographic column: 250mm×4.6mm (id) stainless steel column, filled with 5μm Cig or Cg filler; filter: filter membrane pore size is about 0.5μm;
Micro-injector: 25μL.
4.1.2.1.4 Liquid chromatography operating conditions
Column temperature: room temperature (temperature difference should be less than ±2°C); mobile phase flow rate: 1.5mL/min;
Detector wavelength: 210nm;
Injection volume: 10μL;
Retention time: methylamidophos about 3.7min;
The above liquid chromatography conditions are typical operating parameters. Analysts can make appropriate adjustments to the above operating parameters according to the characteristics of the instrument to obtain the best effect.
4.1.2.1.5 Determination steps
a. Preparation of standard solution
GB15954—1995
Weigh 0.12g of methylamidophos standard sample, accurate to 0.0001g, dissolve it in a 50ml volumetric flask with water and dilute to the scale, and shake well. b. Preparation of sample solution
First, mix the sample. If necessary, heat it in a water bath. Weigh 0.12g of the sample containing methylphosphine to an accuracy of 0.0001g. Place it in a 50mL clean and dry volumetric flask. Dissolve it in water and dilute it to the mark. Shake it well. Filter it with a 0.5μm pore filter. c. Determination
Under the above-mentioned liquid chromatography operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution until the correction factor of two adjacent needles changes by less than 1.5%. Then inject and analyze in the following order: standard solution, sample solution, sample solution, standard solution. 2
Figure 1 Liquid chromatogram of methylamidophos original drug
1-0,0,0-trimethylthiophosphate; 2-methylamidophos; 3-0,0-dimethylthiophosphoramide; 4-unknown impurity 4.1.2.1.6 Calculation
Average the peak areas of methylamidophos in the sample solution and the two standard solutions before and after the sample. The mass percentage of methylamidophos X1 is calculated according to formula (1): X
Average value of the peak area of methylamidophos in the standard solution; Average value of the peak area of methylamidophos in the sample solution; Mass of methylamidophos standard, g;
Mass of monomethylamidophos sample, g;
W——Purity of methylamidophos standard, %.
4.1.2.1.7 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.5%. 4.1.2.2 Thin layer chromatography-iodine titration
4.1.2.2.1 Summary of method
GB 15954-1995
The sample is subjected to thin layer chromatography to separate methylamidophos from impurities. The band containing methylamidophos is scraped off and the content of methylamidophos is determined by iodine titration. 4.1.2.2.2 Reagents and solutions
Ethyl acetate (GB/T3-1226);
Acetone (GB/T 686);
Methanol (GB/T 683);
Glacial acetic acid (GB/T 676);
Sodium hydroxide (GB/T629): 80g/L methanol solution: Iodine standard titration solution: c(1/212)-0.01mol/L, prepare 0.1mol/L solution according to GB/T601, and dilute 10 times; Developing solvent: ethyl acetate+acetone+water=8+4+1; Silica gel G (for thin layer chromatography).
4.1.2.2.3 Apparatus
Chromatography tank
Chromatography plate: 18cm×15cm×0.3cm smooth glass plate; Pipette (calibrate the capacity according to the actual operating conditions): 0.5mL: Glass sand core funnel: G3;
Suction flask: made of hard glass, wall thickness 2mm. 4.1.2.2.4 Determination steps
a. Preparation of chromatography plate
Weigh 10g silica gel G, put it in a glass mortar, add 25mL water (depending on the quality of each batch of silica gel G, it can be increased or decreased appropriately), grind it carefully until it is a uniform paste, immediately pour it on a clean chromatography plate, gently vibrate the glass plate to make the silica gel evenly distributed on the plate without bubbles, put the plate in a horizontal position, solidify it under an infrared lamp or in the air, put it in a 130℃ oven for activation for 40min, cool it down slightly, take it out, and store it in a desiccator filled with silica gel desiccant for later use.
Preparation of sample solution
First, mix the sample evenly. If necessary, heat it in a water bath. Weigh 1.1g of the sample containing methylamidophos to an accuracy of 0.0001g and place it in a 25ml volumetric flask. Dissolve it in methanol and dilute to the mark.c. Thin layer separation
Take an activated chromatography plate, use a 0.5mL pipette to absorb 0.5mL of the sample solution, and spot the sample in a straight line 2.5cm away from the bottom of the chromatography plate (the two ends of the spotting line are 1.5cm away from both sides). After air drying to remove the solvent, stand it upright in a chromatography cylinder containing a developing agent for development (the chromatography plate is immersed in the solvent for about 1 cm). When the front of the solvent rises to about 13 cm from the spot line, take out the plate. When the solvent evaporates to nearly dry, place the plate flat on an uncovered box equipped with a 40W electric lamp to transmit light upward. Use a needle to mark the outline of the methylamidophos band area, and continue to allow the solvent to evaporate completely (or after the solvent evaporates completely, use 10g/mL palladium chloride-ethanol spray to develop the color and determine the methylamidophos band area). Scrape the silica gel in the methylamidophos band area into a sand core funnel, wipe off the silica gel that has not been sucked in with a cotton ball moistened with methanol, and put it into the sand core funnel together. Connect the suction filter to the filtration device with a 100mL iodine volume bottle (as shown in Figure 2), add 10mL methanol to the sand core funnel, stir the silica gel into a paste with a glass rod, filter the filtrate into a 100mL iodine volume bottle under reduced pressure, and repeat the washing twice with 6mL methanol each time. 654
GB 15954—1995
Figure 2 Filtration device diagram
1-sand core funnel; 2-iodine volume flask; 3-filtration flaskAdd 7mL80g/L sodium hydroxide-methanol solution to the above filtrate, alkali hydrolyze in a 30C water bath for 10min, take it out and cool it in an ice bath for 10min, add 10mL glacial acetic acid, immediately plug the bottle stopper, and seal it with methanol, continue to cool for 5min, take it out, wash the bottle stopper with a small amount of methanol, and immediately titrate with 0.01mol/L iodine standard titration solution until light yellow, and the end point is that it does not disappear within 1min. At the same time, take another chromatographic plate and do blank determination in the corresponding area.
4.1.2.2.5 Calculate
the mass percentage of methylamidophos in the sample X2, according to formula (2): X2 = c(V.- V) X 0.1411
wherein: V2-
-the volume of the standard iodine titration solution consumed in titrating the sample solution, mL; V——the volume of the standard iodine titration solution consumed in titrating the blank solution, mL; the actual concentration of the standard iodine titration solution, mol/L; C
m--the mass of the methylamidophos sample contained in 0.5mL of the spotting solution, g; X100-
0.1411-the mass of methylamidophos expressed in grams equivalent to 1.00ml of the standard iodine titration solution [c (1/21,) = 1.000mol/L]. 4.1.2.2.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. 4.2 Determination of moisture
Carry out according to the Karl Fischer method in GB/T1600 (it is allowed to use a micro-moisture meter with equivalent accuracy). 4.3 Determination of acidity
4.3.1 Reagents and solutions
Absolute ethanol (GB/T678);
Sodium hydroxide (GB/T629) standard titration solution c(NaOH)=0.02mol/L; methyl red indicator solution: 1g/L solution.
4.3.2 Operation steps
Weigh 1.5g of methylamidophos technical sample to an accuracy of 0.001g, place it in a 150ml conical flask, add 25mL of absolute ethanol, shake to dissolve the sample, add two drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution until the yellow end point is reached, and perform a blank determination at the same time. 4.3.3 CalculationwwW.bzxz.Net
The acidity X of methamidophos technical expressed as mass percentage shall be calculated according to formula (3): 655
Wherein: V2
GB 15954—1995
c(V2 - V) × 0. 049 × 100
The volume of standard sodium hydroxide solution consumed in titrating the sample solution, mL; The volume of standard sodium hydroxide solution consumed in titrating the blank solution, mL; The actual concentration of standard sodium hydroxide solution, mol/L; m
5 Inspection rules
The mass of the sample, g;
· (3)
The mass of sulfuric acid in grams equivalent to 1.00 mL of standard sodium hydroxide solution [c(NaOH)=1.000°mol/L].
5.1 The method for comparing the measured value with the index shall adopt the rounded value comparison method in GB/T1250. 5.2 Sampling method
The sampling method for emulsion and liquid state in GB/T1605 shall be adopted. The sampling package shall be determined by random method; the final sampling volume shall be not less than 250mL.
5.3 Acceptance rules
Acceptance shall be carried out in accordance with GB/T1604 standard.
6 Marking, packaging, transportation and storage
6.1 The packaging and marking of methyl parathion technical shall comply with the relevant provisions of GB3796, and the product trademark shall be indicated. 6.2 The methyl parathion technical shall be packaged in clean, dry iron drums with inner protective layer, and the net weight of each drum shall not exceed 200kg. 6.3 According to the user's requirements or the agreement reached between the supply and demand parties, other forms of packaging may be used, but they must comply with the relevant requirements of GB3796.
6.4 During storage and transportation, it must be strictly protected from moisture and sunlight, and maintained in good ventilation. It must not be mixed with food, seeds and feed, and avoid contact with the skin and inhalation through the mouth and nose.
6.5 Packages should be stored in ventilated and dry warehouses. 6.6 Safety: Methamidophos is an organophosphorus insecticide. It is toxic if swallowed or inhaled. It can penetrate through the skin. When using this product, protective gloves, gas masks and clean protective clothing should be worn. After application, it should be washed with soap and water immediately. In case of poisoning, a doctor should be consulted and special antidotes such as atropine and antiphosphorus poisoning should be used. Artificial respiration should be performed if necessary. Additional remarks:
This standard was proposed by 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. The main drafters of this standard are Lou Shaowei, Gao Xiaohui, Zhang Pilong, Ruan Shixiang and Pan Dongming. 6561 Reagents and solutions
Absolute ethanol (GB/T678);
Sodium hydroxide (GB/T629) standard titration solution c(NaOH) = 0.02mol/L; Methyl red indicator solution: 1g/L solution.
4.3.2 Operation steps
Weigh 1.5g of methylamidophos technical sample to an accuracy of 0.001g, place it in a 150ml conical flask, add 25mL of absolute ethanol, shake to dissolve the sample, add two drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution until the yellow end point is reached, and perform a blank determination at the same time. 4.3.3 Calculation
The acidity X of methamidophos technical expressed as mass percentage shall be calculated according to formula (3): 655
Wherein: V2
GB 15954—1995
c(V2 - V) × 0. 049 × 100
The volume of standard sodium hydroxide solution consumed in titrating the sample solution, mL; The volume of standard sodium hydroxide solution consumed in titrating the blank solution, mL; The actual concentration of standard sodium hydroxide solution, mol/L; m
5 Inspection rules
The mass of the sample, g;
· (3)
The mass of sulfuric acid in grams equivalent to 1.00 mL of standard sodium hydroxide solution [c(NaOH)=1.000°mol/L].
5.1 The method for comparing the measured value with the index shall adopt the rounded value comparison method in GB/T1250. 5.2 Sampling method
The sampling method for emulsion and liquid state in GB/T1605 shall be adopted. The sampling package shall be determined by random method; the final sampling volume shall be not less than 250mL.
5.3 Acceptance rules
Acceptance shall be carried out in accordance with GB/T1604 standard.
6 Marking, packaging, transportation and storage
6.1 The packaging and marking of methyl parathion technical shall comply with the relevant provisions of GB3796, and the product trademark shall be indicated. 6.2 The methyl parathion technical shall be packaged in clean, dry iron drums with inner protective layer, and the net weight of each drum shall not exceed 200kg. 6.3 According to the user's requirements or the agreement reached between the supply and demand parties, other forms of packaging may be used, but they must comply with the relevant requirements of GB3796.
6.4 During storage and transportation, it must be strictly protected from moisture and sunlight, and maintained in good ventilation. It must not be mixed with food, seeds and feed, and avoid contact with the skin and inhalation through the mouth and nose.
6.5 Packages should be stored in ventilated and dry warehouses. 6.6 Safety: Methamidophos is an organophosphorus insecticide. It is toxic if swallowed or inhaled. It can penetrate through the skin. When using this product, protective gloves, gas masks and clean protective clothing should be worn. After application, it should be washed with soap and water immediately. In case of poisoning, a doctor should be consulted and special antidotes such as atropine and antiphosphorus poisoning should be used. Artificial respiration should be performed if necessary. Additional remarks:
This standard was proposed by 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. The main drafters of this standard are Lou Shaowei, Gao Xiaohui, Zhang Pilong, Ruan Shixiang and Pan Dongming. 6561 Reagents and solutions
Absolute ethanol (GB/T678);
Sodium hydroxide (GB/T629) standard titration solution c(NaOH) = 0.02mol/L; Methyl red indicator solution: 1g/L solution.
4.3.2 Operation steps
Weigh 1.5g of methylamidophos technical sample to an accuracy of 0.001g, place it in a 150ml conical flask, add 25mL of absolute ethanol, shake to dissolve the sample, add two drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution until the yellow end point is reached, and perform a blank determination at the same time. 4.3.3 Calculation
The acidity X of methamidophos technical expressed as mass percentage shall be calculated according to formula (3): 655
Wherein: V2
GB 15954—1995
c(V2 - V) × 0. 049 × 100
The volume of standard sodium hydroxide solution consumed in titrating the sample solution, mL; The volume of standard sodium hydroxide solution consumed in titrating the blank solution, mL; The actual concentration of standard sodium hydroxide solution, mol/L; m
5 Inspection rules
The mass of the sample, g;
· (3)
The mass of sulfuric acid in grams equivalent to 1.00 mL of standard sodium hydroxide solution [c(NaOH)=1.000°mol/L].
5.1 The method for comparing the measured value with the index shall adopt the rounded value comparison method in GB/T1250. 5.2 Sampling method
The sampling method for emulsion and liquid state in GB/T1605 shall be adopted. The sampling package shall be determined by random method; the final sampling volume shall be not less than 250mL.
5.3 Acceptance rules
Acceptance shall be carried out in accordance with GB/T1604 standard.
6 Marking, packaging, transportation and storage
6.1 The packaging and marking of methyl parathion technical shall comply with the relevant provisions of GB3796, and the product trademark shall be indicated. 6.2 The methyl parathion technical shall be packaged in clean, dry iron drums with inner protective layer, and the net weight of each drum shall not exceed 200kg. 6.3 According to the user's requirements or the agreement reached between the supply and demand parties, other forms of packaging may be used, but they must comply with the relevant requirements of GB3796.
6.4 During storage and transportation, it must be strictly protected from moisture and sunlight, and maintained in good ventilation. It must not be mixed with food, seeds and feed, and avoid contact with the skin and inhalation through the mouth and nose.
6.5 Packages should be stored in ventilated and dry warehouses. 6.6 Safety: Methamidophos is an organophosphorus insecticide. It is toxic if swallowed or inhaled. It can penetrate through the skin. When using this product, protective gloves, gas masks and clean protective clothing should be worn. After application, it should be washed with soap and water immediately. In case of poisoning, a doctor should be consulted and special antidotes such as atropine and antiphosphorus poisoning should be used. Artificial respiration should be performed if necessary. Additional remarks:
This standard was proposed by 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. The main drafters of this standard are Lou Shaowei, Gao Xiaohui, Zhang Pilong, Ruan Shixiang and Pan Dongming. 656
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