Some standard content:
HG3626—1999
The product test methods and technical indicators determined in this standard are formulated with reference to the United Nations Food and Agriculture Organization (FAO) pesticide specification "Profenofos emulsifiable concentrate" standard (FAOSpecification461/EC/S/F), and in combination with the actual situation of domestic production enterprises. 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 Chemical Research Institute. The main drafting unit of this standard: Shenyang Chemical Research Institute. Participating drafting units of this standard: Qingdao Pesticide Factory, Nantong Dyeing and Chemical Factory. The main drafters of this standard: Gao Xiaohui, Zhang Pilon, Du Yongqiang, Chen Yue.
Chemical Industry Standard of the People's Republic of China
Profenofos emulsifiable concentrate
Profenofos emulsifiable Other names, structural formulas and basic physical and chemical parameters of concentrates Profenofos are as follows: ISO common name: Profenofos
CIPAC digital code: 461
Chemical name: O-(4-bromo-2-chlorophenyl) O-ethyl S-n-propyl thiophosphate Structural formula:
CH;CH2—O
CH,CH,CH,S
Experimental formula: C,HBrCIO,PS||tt| |Relative molecular weight: 373.6 (according to the 1993 international relative atomic mass) Biological activity: insecticide, acaricide
Vapor pressure (20℃): 1.33×10-°PaSolubility (g/L, 20℃): 0.02 in water; miscible with acetone, toluene, hexane, chloroformStability: easily decomposed in alkaline medium, slowly decomposed under humid conditions1Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of propylbromophos emulsifiable concentrate. HG 3626--1999
This standard applies to 40% propylbromophos emulsifiable concentrate prepared by dissolving propylbromophos technical and emulsifier that meet the standards in a suitable solvent. 2Cited standards
The provisions contained in the following standards constitute the provisions of this standard by 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 method of moisture content of pesticides GB/T1601—1993 Determination method of pH value of pesticides GB/T1603—1979 (1989) Determination method of stability of pesticide emulsions GB/T1604-1995 Acceptance rules for commercial pesticides GB/T1605-1979 (1989) Sampling method for commercial pesticides GB3796-1983 General rules for pesticide packaging
GB4838—1984 Packaging of emulsifiable pesticides
3 Requirements
3.1 Appearance: Stable homogeneous liquid.
3.2 Propylene bromide emulsifiable concentrate shall meet the requirements of Table 1
Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999, implemented on June 1, 2000
Propylene bromide emulsifiable concentrate content, %
Water content, %
Emulsion stability (diluted 200 times)
Low temperature stability
Hot storage stability
HG 3626—1999
Propylene bromide emulsifiable concentrate control item index
Note: Low temperature and hot storage stability tests shall be conducted at least once every six months4
Test method
4.1 Sampling
Carry out in accordance with the "sampling of emulsion and liquid state" method in GB/T1605. The sampling packages shall be determined by the random number table method, and the final sampling volume shall be not less than 250mL.
4.2 Identification test
4.2.1. Gas chromatography: This identification test can be carried out simultaneously with the determination of bromophos content. Under the same chromatographic operating conditions, the relative difference between the retention time of the main peak of the sample solution and the retention time of the chromatographic peak of bromophos in the standard solution should be within 1.5%. 4.2.2 Infrared spectroscopy: There should be no obvious difference in the infrared spectra of the effective components separated from the sample and the standard sample in the wave number range of 4000 to 300 cm-1. The infrared standard spectrum of bromophos is shown in Figure 1. Figure 1 Infrared spectrum of bromophos
4.3 Determination of bromophos content
4.3.1 Summary of method
The sample was dissolved in acetone, triphenyl phosphate was used as internal standard, 3% OV-210/ChromosorbWAWDMCS (180~250um) was used as filler glass column and hydrogen flame ionization detector, and bromophos in the sample was separated and determined by gas chromatography. 4.3.2 Reagents and solutions
Acetone.
Bromophos standard: known content.
Internal standard: triphenyl phosphate, should be free of impurities that interfere with analysis. 1234
Stationary liquid: 0V-210.
HG 3626-1999
Carrier: ChromosorbWAWDMCS (180~250μm). Internal standard solution: weigh 2.5g of triphenyl phosphate, place in a 250mL volumetric flask, add acetone to dissolve, dilute to scale, and shake well. 4.3.3 Instruments and equipment
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1.0 m×3.2 mm (id) glass column or stainless steel column. Column filling: OV-210 coated on Chromosorb WAWDMCS (180～250μm), stationary liquid: (stationary liquid + carrier) = 3:100 (mass ratio).
4.3.4 Preparation of chromatographic column
4.3.4.1 Coating of stationary liquid
Accurately weigh 0.15g of OV-210 stationary liquid into a 250mL beaker, add an appropriate amount (slightly larger than the volume of the carrier) of chloroform to completely dissolve it, pour in 5g of the carrier, shake gently to mix evenly and evaporate the solvent to near dryness, then put the beaker in a 120℃ oven to dry for 1 hour, take it out and cool it to room temperature in a desiccator. 4.3.4.2 Filling of chromatographic column
Connect a small funnel to the outlet of the washed and dried chromatographic column, fill the prepared filler into the column in batches, and tap the column wall continuously until it is filled to 1.5cm from the column outlet. Move the funnel to the entrance of the chromatographic column, plug a small ball of silanized glass wool at the outlet, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, continue to slowly add the filler, and keep tapping the column wall to make it evenly and tightly filled. After filling, plug a small ball of glass wool at the entrance and press it properly to keep the column filler from moving. 4.3.4.3 Aging of the chromatographic column
Connect the entrance of the chromatographic column to the vaporization chamber, and do not connect the detector at the outlet for the time being. Pass the carrier gas (N2) at a flow rate of 15mL/min, raise the temperature to 260℃ in stages, and age at this temperature for 36h. 4.3.5 Gas chromatography operating conditions
Temperature (℃): column temperature 195; vaporization chamber 250; detector chamber 250. Gas flow (mL/min): carrier gas (Nz) 50, oxygen 50; air 500. Injection volume (μL): 0.6.
Retention time (min): 5.2 for propylbromophos; 12.3 for internal standard. 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 results. The gas chromatogram of propylbromophos emulsifiable concentrate is shown in Figure 2.
1—Solvent; 2—propylbromophos; 3—Internal standard
Figure 2 Gas chromatogram of propylbromophos emulsifiable concentrate
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
Weigh 0.1 g of propylbromophos standard (accurate to 0.0002 g), place it in a stoppered glass bottle, add 5 mL of internal standard solution accurately with a pipette, and shake to hook.
4.3.6.2 Preparation of sample solution
Weigh about 0.1 g of sample containing propylbromophos (accurate to 0.000 2 g), place it in a stoppered glass bottle, and accurately add 5 mL of internal standard solution using the same pipette used in 4.3.6.1, and shake well. 4.3.6.3 Determination
HG 3626—1999bzxZ.net
Under the above operating conditions, after the instrument baseline 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 1.0%, determine in the order of standard solution, sample solution, sample solution, and standard solution.
4.3.7 Calculation
Average the ratio of the peak area of propylbromophos to the internal standard in the two needles of sample solution and the two needles of standard solution before and after the sample. The content of bromophos expressed as mass percentage (X,) is calculated according to formula (1): X, r2miP
where: r1-standard solution,The average value of the peak area ratio of bromophos to the internal standard; r2—the average value of the peak area ratio of bromophos to the internal standard in the sample solution; m1—the mass of the bromophos standard sample, g;
—the mass of the sample, g;
P---the mass percentage of bromophos in the standard sample. It is also possible to calculate the correction factor first and then calculate the effective body content in the sample according to the provisions of GB/T4946. 4.3.8 Allowable difference
Take its arithmetic mean as the determination result. The difference between the results of two parallel determinations should not exceed 1.0%. 4.4 Determination of moisture
Carry out according to the Karl Fischer method in GB/T1600. 4.5 Determination of pH value
Carry out according to GB/T1601.
4.6 Emulsion stability test
Carry out according to GB/T1603. Dilute 200 times. If there is no floating oil above, no sinking oil or precipitation below, the test result is qualified. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃ for 1 hour, and the presence of solid and oily matter is recorded. Continue to store at 0℃ for 7 days, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instruments and equipment
Refrigerator: Maintain (0±1)℃.
Centrifuge tube: 100mL, with a scale on the bottom of the tube accurate to 0.05mL. Centrifuge: Matching with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of sample and add it to a centrifuge tube. Cool it to (0±1)℃ in a refrigerator. Keep the centrifuge tube and its contents at (0±1)℃ for 1h. Stir once every 15min for 15s each time. Check and record whether there is any solid or oily matter precipitated. Put the centrifuge tube back into the refrigerator and continue to place it at (0±1)℃ for 7 days. Then take out the centrifuge tube, place it at room temperature (not exceeding 20℃) for 3 hours, and centrifuge it 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). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Hot Storage Stability Test
4.8.1 Instruments and Equipment
Constant Temperature Box (or Constant Temperature Water Bath): (54±2)℃. Ampoule (or stoppered bottle that can still be sealed at 54℃): 50mL. Medical Syringe: 50mL.
4.8.2 Test Procedure
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), and place this ampoule for 1236
HG 3626—1999
Refrigerate in an ice-salt bath and quickly seal with a high-temperature flame (to avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed ampoule in a metal container, and then place the metal container in a (54±2)℃ constant temperature box (or water bath) for 14 days. Take it out and cool to room temperature, wipe the outside of the ampoule and weigh it separately. For samples with no change in mass, conduct a full inspection of propylbromophos EC within 24 hours. After hot storage, the content of the active ingredient in 40% propylbromophos EC should not be less than 9% of the average content measured before hot storage. 1%. 4.9 Inspection and acceptance of products
Inspection and acceptance of products shall comply with the relevant 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 bromophos emulsifiable concentrate shall comply with the relevant provisions of GB3796 and GB4838, and shall also have a trademark and production license number.
5.2 Bromophos emulsifiable concentrate shall be packaged in brown glass bottles with stoppers and caps. Each bottle contains 250g or 500g of net content. External use Use nets, foam plastics, straw or corrugated paper as cushions, and arrange them tightly in calcium plastic boxes, cartons or wooden boxes to prevent damage from impact. No more than 20 bottles per box.
5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 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: In the instruction manual or packaging In addition to the eye-catching toxicity mark, the container should also have toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and first aid measures.
Propylene bromide is a moderately toxic organophosphorus insecticide and acaricide, which is toxic if swallowed or inhaled. Wear protective gloves when using this product, and spray in the direction of the wind. Prevent oral and nasal inhalation. If the product comes into contact with the skin or exposed parts of the body, wash it with soap and water in time. If poisoning occurs, seek medical treatment in time.
5.7 Warranty period: The product should meet the indicators in Table 1 in 3.2 when leaving the factory. Under the specified storage and transportation conditions, the warranty period of propyl bromide emulsifiable concentrate is 2 years from the date of production. Within one month, the propyl bromide content should not be less than 40.0%. From one month to one year, the propyl bromide content should not be less than 37.0%. From one year to two years, the propyl bromide content should not be less than 36.0%. 12373 According to user requirements or order agreements, other forms of packaging can be used, but they must comply with the relevant provisions of GB4838. 5.4 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, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the eye-catching toxicity mark on the instruction manual or packaging container, there should also be toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and first aid measures.
Propylene bromide is a moderately toxic organophosphorus insecticide and acaricide, which is toxic if swallowed or inhaled. Wear protective gloves when using this product, and spray in the direction of the wind. Prevent inhalation through the mouth and nose. If the skin or exposed parts of the body come into contact with this product, wash it with soap and water in time. If poisoning occurs, seek medical treatment in time.
5.7 Warranty period: The product should meet the indicators in Table 1 in 3.2 when it leaves the factory. Under the specified storage and transportation conditions, the warranty period of bromophos emulsifiable concentrate is 2 years from the date of production. Within one month, the bromophos content should not be less than 40.0%. From one month to one year, the bromophos content should not be less than 37.0%. From one year to two years, the bromophos content should not be less than 36.0%.3 According to user requirements or order agreements, other forms of packaging can be used, but they must comply with the relevant provisions of GB4838. 5.4 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, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the eye-catching toxicity mark on the instruction manual or packaging container, there should also be toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and first aid measures.
Propylene bromide is a moderately toxic organophosphorus insecticide and acaricide, which is toxic if swallowed or inhaled. Wear protective gloves when using this product, and spray in the direction of the wind. Prevent inhalation through the mouth and nose. If the skin or exposed parts of the body come into contact with this product, wash it with soap and water in time. If poisoning occurs, seek medical treatment in time.
5.7 Warranty period: The product should meet the indicators in Table 1 in 3.2 when it leaves the factory. Under the specified storage and transportation conditions, the warranty period of bromophos emulsifiable concentrate is 2 years from the date of production. Within one month, the bromophos content should not be less than 40.0%. From one month to one year, the bromophos content should not be less than 37.0%. From one year to two years, the bromophos content should not be less than 36.0%.
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