Some standard content:
HG3625—1999
The product inspection methods and technical indicators determined in this standard are formulated with reference to the United Nations Food and Agriculture Organization (FAO) pesticide specification "Profenofos Technical" standard (FAOSpecification461/TC/S/F), and combined 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. The participating drafting units of this standard: Qingdao Pesticide Factory, Nantong Dyeing and Chemical Factory. The main drafters of this standard: Gao Xiaohui, Zhang Pilong, Du Yongqiang, Chen Yue.
Chemical Industry Standard of the People's Republic of China
Profenofos Technical
Profenofos technical
Other names, structural formulas and basic physical and chemical parameters of bromophos 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: CnH1sBrCIO,PS||tt ||Relative molecular mass: 373.6 (according to the 1993 international relative atomic mass) Biological activity: insecticide, acaricide
Vapor pressure (20℃): 1.33×10-3Pa
Solubility (20℃): 0.02g/L in water; miscible with acetone, toluene, hexane, chloroform Stability: easily decomposed in alkaline medium, slowly decomposed under humid conditions 1 Scope
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of propylbromophos technical. This standard applies to propylbromophos technical composed of propylbromophos and impurities generated in its production. 2 Referenced standards
HG 3625—1999
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) Method for determination of moisture content 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
GB4838—1984 Packaging of emulsifiable concentrate pesticides
GB/T 4946-1985
Terms for gas chromatography
3 Requirements
3.1 Appearance: Stable homogeneous brown-yellow liquid. 3.2 Profenofos technical shall meet the requirements of Table 1. Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999, and implemented on June 1, 2000
Propylene bromophos content, %
Free bromophenol, %
Water, %
4 Test methods
4.1 Sampling
HG 3625 -- 1999
Table 1 Control Items of Propylene Bromophos Technical
Superior Grade
First Grade
Qualified Grade
According to the "Sampling of Liquid State" method in GB/T1605. The sampling packages are determined by the random number table method, and the final sampling volume should be not less than 250 mL.
4.2 Identification test
4.2.1 Gas chromatography: This identification test can be carried out simultaneously with the determination of propyl bromide 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 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 in the sample and the standard sample in the wave number range of 4000~300cm-1. The infrared standard spectrum of propyl bromide is shown in Figure 1. Figure 1 Infrared spectrum of propyl bromide
4.3 Determination of propyl bromide content
4.3.1 Method summary
The sample is dissolved in acetone, triphenyl phosphate is used as the internal standard, and a glass column filled with 3% OV-210/ChromosorbWAWDMCS (180~～250um) and a hydrogen flame ionization detector are used to separate and determine the propyl bromide in the sample by gas chromatography. 4.3.2 Reagents and solutions
Acetone.
Propylene bromide standard: known content.
Internal standard: triphenyl phosphate, should be free of impurities that interfere with the analysis. Stationary liquid: 0V-210.
Carrier: ChromosorbWAWDMCs (180~250μm). Internal standard solution: weigh 2.5g of triphenyl phosphate, place in a 250mL volumetric flask, add appropriate amount of acetone to dissolve, dilute to scale, and shake well. 4.3.3 Instruments and equipment
HG3625-
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1.0m×3.2mm(id) glass column or stainless steel column. -1999
Column filling: OV-210 coated on ChromosorbWAWDMCS (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 (more 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, 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 filling material 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 lightly covering the column wall to make it evenly and tightly filled. After filling, plug a small ball of glass wool at the inlet end and press it properly to keep the column filler from moving. 4.3.4.3 Aging of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, and do not connect the detector at the outlet end 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 rate (mL/min): nitrogen (N2) 50, hydrogen 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 technical is shown in Figure 2.
1 --Solvent, 2-propylbromophos; 3-Internal standard 4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
Figure 2 Gas chromatogram of propylbromophos technical
Weigh 0.1 g of propylbromophos standard (accurate to 0.000 2 g), measure it into a stoppered glass bottle, add 5 mL of internal standard solution accurately with a pipette, and shake it.
4.3.6.2 Preparation of sample solution
Weigh about 0.1g of sample containing bromophos (accurate to 0.0002g), place it in a stoppered glass bottle, and accurately add 5mL of internal standard solution using the same pipette used in 4.3.6.1, and shake well. 4.3.6.3 Determination
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
HG 3625—1999
Average the ratio of the peak area of bromophos 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, = rem;PbZxz.net
the average value of the peak area ratio of bromophos to the internal standard in the standard solution; where: ri——
r2--in the sample solution,Average value of the peak area ratio of bromophos and internal standard; Mass of bromophos standard, g;
m2——mass of sample, g;
Mass percentage of bromophos in P standard.
4.3.8 Allowable difference
Take the arithmetic mean as the determination result. The difference between two parallel determination results shall not exceed 1.0%. 4.4 Determination of free phenol content in bromophos
4.4.1 Summary of method
(1)
The sample is dissolved in chloroform, and the free bromophenol in the sample is separated and determined by gas chromatography using a glass column filled with 3% OV-210/ChromosorbWAWDMCS (180~250μm) and a hydrogen flame ionization detector. 4.4.2 Reagents and solutions
Blue chloroform
Bromophenol standard: known content, greater than or equal to 99.0%. Stationary liquid: 0V-210.
Carrier: Chromosorb WAW DMCS (180～~250 μm). 4.4.3 Instruments and equipment
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: use the chromatographic column specified in 4.3.3. 4.4.4 Gas chromatography operating conditions
Temperature (℃): column temperature 95; vaporization chamber 150; detector chamber 150. Gas flow rate (mL/min): carrier gas (Nz) 30; hydrogen 35; air 350. Injection volume (μL): 2.
Retention time (min): bromophenol 3.8.
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. The gas chromatogram of bromophenol in the original drug of bromophos is shown in Figure 3. 2
1—Solvent; 2—Bromophenol
Figure 3 Gas chromatogram of bromophenol
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
Weigh 0.05g of standard sample (accurate to 0.0002g), place it in a 10mL volumetric flask, dissolve it with chloroform and dilute it to the mark, and shake it. 4.4.5.2 Preparation of sample solution
Weigh about 0.05g of sample containing bromophenol (accurate to 0.0002g), place it in a 10mL volumetric flask, dissolve it with chloroform and dilute it to the mark, and shake it.
4.4.5.3 Determination
HG 3625—1999
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 change between two adjacent needles is less than 2.0%, perform determination in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak area values of bromophenol in the two needles of sample solution and the two needles of standard solution before and after the sample. The bromophenol content (X2) expressed as a mass percentage is calculated according to formula (2): A2miP
Wherein: A,——the peak area value of bromophenol in the standard solution; A—the peak area value of bromophenol in the sample solution; m1—the mass of the bromophenol standard, g;
m —the mass of the sample, g,
P—the mass percentage of bromophenol in the standard.
4.4.7 Allowable difference
Take its arithmetic mean as the determination result. The difference between the results of two parallel determinations shall not exceed 0.2%. 4.5 Determination of moisture
Carry out according to the Karl Fischer method in GB/T1600. 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the relevant provisions of GB/T 1604. The rounding value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
(2)
5.1 The marking, labeling and packaging of bromophos technical shall comply with the relevant provisions of GB3796 and GB4838, and shall also have the trademark and production license number.
5.2 Bromophos technical shall be packaged in clean, 200kg iron drums with inner protective layer, or in 50kg plastic drums. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Packages shall 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, the instruction manual or packaging container shall also have toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and emergency measures.
Propylene bromophos is a moderately toxic organophosphorus insecticide and acaricide, which is toxic to humans if swallowed or inhaled. Therefore, protective gloves should be worn when using this product. When spraying, it should be done in the direction of the wind to prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If poisoning occurs, seek medical treatment in time.
5.7 Warranty period: The product should meet the various indicators in Table 1. of 3.2 when leaving the factory. Under the specified storage and transportation conditions, the warranty period of propylphosphonium technical is 1 year from the date of production. During the warranty period, the propylphosphonium content should not be less than 95% of the labeled content. 12311 The marking, labeling and packaging of bromophos technical shall comply with the relevant provisions of GB3796 and GB4838, and shall also have the trademark and production license number.
5.2 Bromophos technical shall be packaged in clean, 200kg iron drums with inner protective coating, or in 50kg plastic drums. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Packages shall 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 shall also be toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and emergency measures.
Bromophos is a moderately toxic organophosphorus insecticide and acaricide, which is toxic to people if swallowed or inhaled. Therefore, protective gloves should be worn when using this product. Spray in the direction of the wind to prevent inhalation through the mouth and nose. If the skin or exposed parts of the body come into contact with this product, they should be washed 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. of 3.2 when it leaves the factory. Under the specified storage and transportation conditions, the warranty period of propylphosphonate technical is 1 year from the date of production. During the warranty period, the propylphosphonate content should not be less than 95% of the marked content. 12311 The signs, labels and packaging of bromophos technical shall comply with the relevant provisions of GB3796 and GB4838, and shall also have the trademark and production license number.
5.2 Bromophos technical shall be packaged in clean, 200kg iron drums with inner protective layer, or in 50kg plastic drums. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Packages shall 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 shall also be toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and emergency measures.
Bromophos is a moderately toxic organophosphorus insecticide and acaricide, which is toxic to people if swallowed or inhaled. Therefore, protective gloves should be worn when using this product. Spray in the direction of the wind to prevent inhalation through the mouth and nose. If the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If poisoning occurs, seek medical treatment in time.
5.7 Warranty period: The product should meet the various indicators in Table 1. of 3.2 when leaving the factory. Under the specified storage and transportation conditions, the warranty period of propylphosphonate technical is 1 year from the date of production. During the warranty period, the propylphosphonate content should not be less than 95% of the labeled content. 1231
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