Some standard content:
HG3623-1999
This standard is formulated with reference to the enterprise standard of triflumuron in my country and the actual domestic production situation. The analysis of the active ingredient content in the standard adopts gas chromatography.
This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafting unit of this standard: Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The participating drafting unit of this standard: Zhongshan Kaida Fine Chemical Industry Co., Ltd. The main drafters of this standard: Zhao Xinxin, Xing Hong, Wu Zhijian, Situ Zhenchao, Zhang Gongju. 1213
Chemical Industry Standard of the People's Republic of China
Triflumuron Technical
Plifenate technical
Other names, structural formulas and basic physicochemical parameters of trichloropyralid are as follows: ISO common name: Plifenate (recommended name) Chemical name: 1,1,1-trichloro-2-(3,4-dichlorophenyl) ethyl acetate Structural formula:
Empirical formula: CoH,ClOz
CH-O-CO-CH3
Relative molecular mass: 336.4 (based on the relative atomic mass in 1993) Biological activity: insecticide (for sanitary use)
Melting point: 84.5℃
Vapor pressure (20℃): 1.47×10-5Pa
Solubility (g/L, 20℃): 0.05 in water 600 in cyclohexanone; 10 in isopropanol Stability: easily decomposed in alkaline medium, with good thermal stability 1 Range
HG 3623--1999
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of trichlorfon technical. This standard applies to trichlorfon technical composed of trichlorfon and impurities generated during its production. 2 Referenced standards
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 will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601—1988 Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB/T1250—1989 Method for expressing and determining limit values GB/T1604—1995 Acceptance rules for commercial pesticides GB/T1605-1979 (1989) Sampling methods for commercial pesticides GB3796--1983 General rules for pesticide packaging
GB/T4946—1985 Terminology for gas chromatography 3 Requirements
3.1 Appearance: First-class products are white to slightly yellow powdery solids, and qualified products are light yellow to yellow solids. 3.2 Trichlorobenzyl technical should meet the requirements of Table 1. Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999 1214
Implemented on June 1, 2000
Content of trichlorfon, %
Acetone insoluble matter, %
Acidity (in H2SO,), %
HG3623-1999
Table 1 Control Items and Indicators of Trichlorfon Technical Material First-class Product
Note: Acetone insoluble matter is a random inspection item. During normal production, it shall be inspected at least once every three months. 4 Test Method
4.1 Sampling
Qualified Product
The sampling shall be carried out in accordance with the "technical material sampling" method in GB/T1605-1979 (1989). The sampling packages shall be determined by the random number table method, and the final sampling quantity shall be not less than 250g.
4.2 Identification test
4.2.1 Gas chromatography: This identification test can be carried out simultaneously with the determination of triflumuron content. Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak of the sample solution and the retention time of the chromatographic peak of triflumuron 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 sample and the standard in the wave number range of 4000~~300cm-1 (see Figure 1).
4.3 Determination of trichlorobenzyl
4.3.1 Summary of the method
Infrared spectrum of trichlorobenzyl standard
The sample was dissolved in chloroform, di-n-butyl phthalate was used as the internal standard, and the trichlorobenzyl in the sample was separated and determined by gas chromatography using a glass column filled with 3% OV-101/Chromosorb WHP and a hydrogen flame ionization detector. 4.3.2 Reagents and solutions
Chloroform.
Trichlorobenzyl standard: known content, greater than or equal to 99.0%. Internal standard: di-n-butyl phthalate, which should not contain impurities that interfere with the analysis. Stationary phase: OV-101.
Carrier: Chromosorb WHP (144~177 μm) or other carriers with equivalent performance. Internal standard solution: weigh 2.0g of di-n-butyl phthalate into a 200mL volumetric flask, dissolve it with trifluoromethane and dilute to the mark, shake 1215
4.3.3 Instruments and equipment
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
HG 3623—1999
Chromatographic column: 2 mX2 mm (id) glass or stainless steel column. Column packing: OV-101 coated on Chromasorb WHP (144～177 μm). Stationary liquid: (stationary liquid + carrier) = 3:100 (mass ratio). 4.3.4 Preparation of chromatographic column
a) Coating of stationary liquid
Accurately weigh 0.15 g of OV-101 stationary liquid into a 250 mL beaker, add an appropriate amount (slightly larger than the volume of the carrier) of chloroform to completely dissolve it, pour in 5 g of the carrier, gently shake the beaker by hand to make the carrier completely immersed in the solution, place the beaker under an infrared lamp to heat, shaking the beaker while heating until the solvent evaporates and is almost dry, then place it in a 120°C oven to dry for 2 h, take it out and place it in a desiccator for later use. b) 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 inlet 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 tap the column wall continuously to make it filled evenly and tightly. After filling, also plug a small ball of glass wool at the inlet end, and press it appropriately to keep the column filler from moving. c) Aging of chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, do not connect the outlet end to the detector for the time being, pass the carrier gas (N2) at a flow rate of 20mL/min, raise the temperature to 220℃ in stages, and age at this temperature for at least 24h. 4.3.5 Gas chromatography operating conditions
Temperature (℃): column chamber 180;
vaporization chamber 240,
detector chamber 250.
Gas flow rate (mL/min): carrier gas (N2) 30; hydrogen 40;
air 300.
Retention time (min): triflumuron 8; internal standard (di-n-butyl phthalate) 11. The above operating conditions are typical operating parameters (see Figure 2). According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect.
1--Solvent; 2-Trifluanid; 3-Internal standard (di-n-butyl phthalate) Figure 2 Gas chromatogram of trifluanid original drug
4.3.6 Determination steps
a) Preparation of standard solution
Weigh about 0.1g of trifluanid standard (accurate to 0.0002g), place it in a stoppered glass bottle, use a pipette to accurately add 5mL of internal standard solution, and shake well.
b) Preparation of sample solution
Weigh about 0.1g of sample containing trifluanid (accurate to 0.0002g), place it in a stoppered glass bottle, use a pipette between the pipettes in a) to accurately add 5mL of internal standard solution, and shake well. c) Determination
HG 3623—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 of two adjacent needles changes less than 1.5%, perform determination 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 trichlorfon 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 trichlorfon in the sample expressed as mass percentage (X,) is calculated according to formula (1): X,= rzmiP
Wherein: r1—the average value of the peak area ratio of trichlorfon to internal standard in the standard solution; r2
the average value of the peak area ratio of trichlorfon to internal standard in the sample solution; -the mass of trichlorfon standard, g;
the mass of the sample, g;
P—the mass fraction of trichlorfon in the standard, %. Alternatively, the correction factor f may be calculated first and then the effective content in the sample may be calculated according to the provisions of GB/T4946. 4.3.8 Allowable difference
The arithmetic mean value shall be taken as the determination result. The difference between the results of two parallel determinations shall not exceed 1.0%. 4.4 Determination of solid insoluble matter in acetone
4.4.1 Reagents and solutions
Acetone: dried over anhydrous sodium sulfate.
4.4.2 Instruments and equipment
Conical flask: 250 mL.
Goosenburg crucible or glass crucible: 3*
Oven: (110±2)℃. www.bzxz.net
4.4.3 Determination steps
（1）)
Weigh 10g of the sample (accurate to 0.01g), put it into a conical flask, add 50mL acetone, and shake until all soluble substances are dissolved. Filter the solution with a crucible that has been constant in mass, then wash the conical flask with 60mL acetone three times and filter it. Place the crucible in a 110℃ oven and dry it for 30min, take it out and cool it to room temperature, and weigh it.
The acetone insoluble matter (X,) in the sample expressed as mass percentage is calculated according to formula (2): Xz = ml= mo × 100
The mass of the insoluble matter after the mass is constant, g, where: mi—
mo ---the mass of the crucible, g;
m--the mass of the sample, g.
4.4.4 Allowable difference
Take the arithmetic mean as the determination result. The relative difference between two parallel determination results should not exceed 50%. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution: c(NaOH)=0.02mol/L. Phenolphthalein ethanol indicator solution: 1g/100mL.
4.5.2 Determination steps
(2)
Weigh 1g of the sample (accurate to 0.0002g), place it in a 250mL conical flask, add 50mL acetone, shake to dissolve the sample, then add 20mL water, add 3 to 5 drops of indicator solution, and titrate with sodium hydroxide standard titration solution until red is the end point. 1217
Perform a blank determination at the same time.
HG3623-1999
The acidity of the sample expressed as a mass percentage (X:) is calculated according to formula (3): X_cV-Vo) × 0. 049 × 100
Wu Zhong: c-
actual concentration of sodium hydroxide standard titration solution, mol/L; Vi—-volume of sodium hydroxide standard titration solution consumed by titrating the sample solution, mL; V. Volume of sodium hydroxide standard titration solution consumed by titrating the blank solution, mL; mass of a sample, g;
(3)
0.049The mass of sulfuric acid in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L].
4.5.3 Allowable difference
Take the arithmetic mean as the measurement result. The relative difference between two parallel measurement results should not exceed 50%. 4.6 Inspection and acceptance of products
Should comply with the relevant provisions of GB/T1604. The rounded value comparison method is used for the processing of limit values. 5 Marking, labeling, packaging, purchase and transportation
5.1 The marking, labeling and packaging of trichlorobenzene technical shall comply with the relevant provisions of GB3796. As a technical drug for commodity circulation, it shall also have a trademark and production license number.
5.2 Trichlorobenzene technical shall be packaged in woven bags lined with plastic film, with a net content of 25kg or 50kg per bag. 5.3 Other forms of packaging may be used according to user requirements or ordering agreements, but they must comply with the relevant provisions of GB3796. 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 addition to the corresponding toxicity mark, the following toxicity instructions should be included in the instruction manual or packaging container: Trichlorobenzene is a low-toxic insecticide that is slightly irritating to the eyes and skin. It is toxic if inhaled and can be fatal if ingested by mistake. Protective gloves and protective clothing should be worn when using this product. Rinse the skin thoroughly with clean water or soapy water after application. There is currently no specific antidote for acute poisoning with trichlorobenzene. The main treatment is to completely remove the poison and provide symptomatic treatment. The measures include infusion and taking tranquilizers, large amounts of vitamins and hormones, etc. Those who ingest it by mistake need to have their stomachs washed in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period for the original trichlorobenzene is 2 years from the date of production. 12185 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 addition to the corresponding toxicity mark on the instruction manual or packaging container, there should also be the following description of toxicity: Trichlorobenzene is a low-toxic insecticide, which is slightly irritating to the eyes and skin. It is toxic if inhaled and can be fatal if ingested by mistake. Protective gloves and protective clothing should be worn when using this product. Rinse the skin thoroughly with clean water or soapy water after application. There is currently no specific antidote for acute poisoning with trichlorobenzene. The main treatment is to completely remove the poison and symptomatic treatment. The measures include infusion and taking tranquilizers, large amounts of vitamins and hormones, etc. Those who ingest it by mistake need to have their stomachs washed in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of trichlorobenzene technical is 2 years from the date of production. 12185 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 addition to the corresponding toxicity mark on the instruction manual or packaging container, there should also be the following description of toxicity: Trichlorobenzene is a low-toxic insecticide, which is slightly irritating to the eyes and skin. It is toxic if inhaled and can be fatal if ingested by mistake. Protective gloves and protective clothing should be worn when using this product. Rinse the skin thoroughly with clean water or soapy water after application. There is currently no specific antidote for acute poisoning with trichlorobenzene. The main treatment is to completely remove the poison and symptomatic treatment. The measures include infusion and taking tranquilizers, large amounts of vitamins and hormones, etc. Those who ingest it by mistake need to have their stomachs washed in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of trichlorobenzene technical is 2 years from the date of production. 1218
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