Some standard content:
HG3619—1999
This standard is formulated based on the actual production conditions of technical materials of various manufacturers in my country. The test method for the active ingredient content in this standard is the reverse phase high performance liquid chromatography method, which is equivalent to the normal phase high performance liquid chromatography method adopted by the Council for International Pesticide Analysis Cooperation (CIPAC).
Appendix A of this standard is the appendix of the standard.
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 Chemical Research Institute of the Ministry of Chemical Industry. The main drafting unit of this standard: Hunan Chemical Research Institute. Participating drafting units of this standard: Hunan Haili Chemical Co., Ltd. Test Plant, Changzhou Pesticide Factory, Hunan Linxiang Amino Chemical Factory, Hubei Shalongda Jiangling Pesticide Factory, Wuxi Huishan Pesticide Factory The main drafters of this standard: Fu Deling, Huang Lu, Zhang Zhongze, Wu Yanling, Yu Yanfeng, Zheng Jingyu, Peng Jiping. 1178
Chemical Industry Standard of the People's Republic of China
Fenobucarb technical
Fenobucarb technical
Other names, structures and basic physicochemical parameters of Fenobucarb are as follows:ISO common name: Fenobucarb
CIPAC digital code: 390
Chemical name: 2-sec-butylphenyl methylcarbamate 2-(1-methylpropylphenyl) methylcarbamate Structural formula:
O--CONHCH:
CH--C,Hs
Empirical formula: C12H1NO2
Relative molecular mass: 207.3 (according to the international relative atomic mass in 1993) Biological activity: insecticide
Melting point: 31~32℃
Vapor pressure (20℃): 1.6mPa
HG 3619—1999
Solubility: 610 mg/L (30℃) in water; greater than 1kg/kg at room temperature for acetone, benzene, toluene and xylene. Stability: unstable to alkali and concentrated acid, easily decomposed by heat. 1 Scope
This standard specifies the requirements, test methods, marking, labeling, packaging and storage and transportation of the technical material of Fenbucarb. This standard applies to the technical material of Fenbucarb consisting of Fenbucarb and impurities generated in its production. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard by being referenced 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/T 601-1988 Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents GB/T603-1988 Preparation of preparations and products used in test methods for chemical reagents GB/T1250-1989 Methods for expressing and determining limit values GB/T1600-1979 (1989) Method for determining moisture content in pesticides GB/T1604-1995 Acceptance rules for commercial pesticides GB/T1605-1989 Sampling methods for commercial pesticides GB3796-19832
General rules for pesticide packaging
Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999, and implemented on June 1, 2000
3 Requirements
HG 3619-1999
3.1 Appearance: Light yellow to brown viscous liquid or solid, without visible impurities. 3.2 Fenbucarb technical shall meet the requirements of Table 1. Table 1 Fenbucarb technical control items index
Superior quality
Fenbucarb content, %
O-sec-butylphenol content, %
Water, %
Acidity or alkalinity
Acetone insoluble matter, %
Acidity (in H,SO.), %
Alkalinity (in NaOH), %
Note: Under normal circumstances, acetone insoluble matter is sampled once a quarter. 4 Test method
4.1 Sampling
First-class quality
Qualified quality
Carry out according to the "sampling of emulsion and liquid state" method in GB/T1605-1989. The sampling package is determined by the random number table method, and the final sampling volume should be no less than 250mL.
4.2 Identification test
High performance liquid chromatography: This identification test can be carried out simultaneously with the determination of the content of fambucarb. 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 fambucarb in the standard solution should be within 1.5%. 4.3 Determination of fambucarb content
4.3.1 Summary of the method
The sample is dissolved in methanol, methanol-10 water is used as the mobile phase, a stainless steel column with C1 (5 um) as the filler and a UV detector are used, and the fambucarb in the sample is separated and determined by liquid chromatography using the external standard method. 4.3.2 Reagents and solutions
Methanol: high-grade purity.
Water: distilled twice.
Standard sample of fambucarb: greater than or equal to 99.5%.
4.3.3 Instruments and equipment
High performance liquid chromatograph: with an adjustable wavelength UV detector. Chromatographic data processor.
Chromatographic column: 150mm×4.6mm(id) stainless steel column, filled with Cng(5μm) filler. Injector: 50μL.
Volume flask: 25mL, calibrated and qualified.
Injection loop: 20μL.
4.3.4 Chromatographic operating conditions
Mobile phase: methanol+water=67+33 (volume ratio), filtered (0.45um). Flow rate: 1.2mL/min.
Detection wavelength: 270 nm.
Quantitative method: external standard method.
Temperature: room temperature.
HG 3619—1999
Retention time (min): sec-butylcarb 5.24; o-sec-butylphenol 7.36. The above operating parameters are typical (see Figure 1). The given operating parameters can be adjusted appropriately according to the characteristics of the instrument in order to obtain the best effect. 1-Second-butylcarb; 2-Sec-butylphenol
Figure 1 Liquid chromatography separation diagram of sec-butyl carb technical
4.3.5 Determination steps
4.3.5.1 Preparation of standard solution
Weigh 0.1g of sec-butyl carb standard (accurate to 0.0002g), place it in a 25mL volumetric flask, add 15mL of methanol, vibrate under ultrasonic wave for 1min, then make up to volume with methanol, shake and filter (0.45μg), and the filtrate is used for later use. 4.3.5.2 Preparation of sample solution
Weigh the original drug sample containing 0.1g of fumaric acid (accurate to 0.0002g), place it in a 25mL volumetric flask, add 15mL of methanol, vibrate under ultrasonic for 1min, and then make up to volume with methanol. After spreading evenly, filter (0.45μg), and the filtrate is reserved. 4.3.5.3 Determination
Under the above operating conditions, after the instrument is stable, continuously inject several needles of standard solution, calculate the relative response value of each needle, and when the relative response value of two adjacent needles changes by less than 1.5%, perform determination in the order of standard solution, sample solution, sample solution, and standard solution. 4.3.6 Calculation
Inject and average the fumaric acid peak areas in the two needles of sample solution and the two needles of standard solution before and after the sample. The content of sec-butylcarb expressed as mass percentage (X) is calculated according to formula (1): X, = rm; P
Wherein: r--the average value of the peak area of sec-butylcarb in the standard solution; m1--the mass of the sec-butylcarb standard, g;
the mass of the sample, g3
P--the mass percentage of sec-butylcarb in the standard sample. 4.3.7 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.5%. 4.4 Determination of o-sec-butylphenol content
4.4.1 Summary of the method
The sample is dissolved in methanol, methanol-10 water is used as the mobile phase, a stainless steel column with C1s (5 aum) as the filler and an ultraviolet detector are used, and the o-sec-butylphenol in the sample is separated and determined by high performance liquid chromatography using the external standard method. 4.4.2 Reagents and solutions
Methanol: high purity.
Water: double distilled.
HG 3619--1999
Standard sample: o-sec-butylphenol, known content, greater than or equal to 99.0%. 4.4.3 Instruments and equipment
Volume flask: 25mL, 100mL, calibrated and qualified. Pipette: 1mL, calibrated and qualified.
Others are the same as 4.3.3.
4.4.4 Chromatographic operating conditions
Same as 4.3.4.
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of o-sec-butylphenol standard, place it in a 100mL volumetric flask, dissolve it in methanol and make up to volume, shake well, and take 1.0mL is placed in a 25mL volumetric flask, fixed to volume with mobile phase, shake and filter (0.45um), and the filtrate is used for later use. Note: If the color of the standard solution changes, it cannot be used and needs to be re-prepared. 4.4.5.2 Preparation of sample solution
Same as 4.3.5.2.
4.4.5.3 Determination
Same as 4.3.5.3.
4.4.6 Calculation
Average the peak areas of o-sec-butylphenol in the two sample solutions and the standard solution. The content of o-sec-butylphenol expressed as mass percentage (X,) is calculated according to formula (2) 0. 01 r2miP
Wherein: r-
the average value of the peak area of o-sec-butylphenol in the standard solution; the average value of the peak area of o-sec-butylphenol in the sample solution m -- the mass of the o-sec-butylphenol standard sample, g; m2 -- the mass of the sample, g;
P-the mass percentage of the o-sec-butylphenol standard sample; 0.01-dilution conversion factor.
4.4.7 Allowable difference
The relative deviation of the two determination results shall not exceed 20%. 4.5 Water content determination
Carry out according to the Karl Fischer method in GB/T1600-1989 Pesticide Water Content Determination Method. 4.6 Determination of Acidity (or Alkalinity)
4.6.1 Reagents and solutions
Acetone; analytical grade.
Sodium hydroxide standard titration solution: c(NaOH)=0.02mol/L, prepared and calibrated according to the method specified in GB/T601. Hydrochloric acid standard titration solution: c(HCI)=0.02mol/L, prepared and calibrated according to the method specified in GB/T601. Methyl red ethanol solution indicator: 1g/L, prepared according to the provisions of GB/T 603. 4.6.2 Determination steps
(2)
Weigh 5g of the sample (accurate to 0.01g), place it in a 250mL conical flask, add 30mL of acetone, shake to dissolve, add 30mL of water to mix thoroughly, add 3-4 drops of indicator solution, shake, and titrate with sodium hydroxide standard titration solution (or hydrochloric acid standard titration solution) until the color changes from red to yellow (or from yellow to red). Perform a blank determination at the same time.
4.6.3 Calculation
HG 3619—1999
The acidity of the sample (X3) (in H2SO4) expressed as mass percentage is calculated according to formula (3): X = c(V-Vo) × 0.049 × 100m
The alkalinity of the sample (X,) (in NaOH) expressed as mass percentage is calculated according to formula (4): X, = c(V/-Vo) × 0.040 )
Wherein: c
actual concentration of sodium hydroxide (or hydrochloric acid) standard titration solution, mol/L, volume of sodium hydroxide (or hydrochloric acid) standard titration solution consumed in titrating the sample solution, mL; volume of sodium hydroxide (or hydrochloric acid) standard titration solution consumed in titrating the blank solution, mL; mass of the sample, g;
(3)
and 1.00 mL The mass of sulfuric acid in grams equivalent to the standard titration solution of sodium hydroxide [c(NaOH)=1.000 mol/L:
The mass of sodium hydroxide in grams equivalent to the standard titration solution of hydrochloric acid [c(HCl)-1.000 mol/L.
4.6.4 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed 20%. 4.7 Determination of acetone insoluble matter
4.7.1 Instruments and equipment wwW.bzxz.Net
Erlenmeyer flask: with glass ground joint, 250 mL. Reflux condenser: matched with the Erlenmeyer flask. Glass crucible: 3\.
Oven: (110±2)℃.
Water bath.
4.7.2 Reagents and solutions
Acetone: dried over anhydrous sodium sulfate.
4.7.3 Determination steps
Weigh 10g of the original sample of Fenbucarb (accurate to 0.01g), put it into a conical flask, add 50mL of acetone, and heat it under reflux until all soluble substances are dissolved. Filter the solution with a crucible that has been kept constant in mass, then wash the conical flask and crucible with 60mL of acetone three times, and filter it by suction. Dry it in an oven at 110℃ for 30min, take it out, cool it to room temperature, and weigh it. The content of acetone insoluble matter (Xg) expressed as mass percentage is calculated according to formula (5): Xg= m= mo× 100
Where: m1—the mass of the insoluble matter after the mass is kept constant, g, mo—the mass of the crucible, g,
-the mass of the sample, g.
4.7.4 Allowable difference
The relative deviation of the results of two parallel determinations should not exceed 20%. 4.8 Inspection and acceptance of products
Should comply with the relevant provisions of GB/T1604, and the rounding 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 Fenbucarb technical shall comply with the relevant provisions of GB3796, and shall also have the trademark and production license number. 5.2 Fenbucarb technical is packaged in galvanized iron drums, with a net content of (200 ± 1) kg per drum, and the drum cover must be sealed without leakage. 1183
HG3619-1999
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: This product is a low-grade insecticide and general protective measures can be taken when used. In case of poisoning, atropine sulfate can be used for detoxification and medical treatment can be carried out if necessary.
5.7 Inspection period: Under the specified transportation conditions, the inspection period of the original drug of Fenbucarb shall be calculated from the date of arrival. The inspection and acceptance shall be carried out within three months according to the specified requirements, and the results shall be consistent with the quality requirements. 1184
HG 3619--1999
Appendix A
(Appendix to the standard)
Determination of Fenbucarb content by gas chromatography and determination of o-sec-butylphenol (free phenol) content by colorimetry A1 Gas chromatography method for determination of Fenbucarb content This method can be used for production control analysis.
A1.1 Method Summary
The sample was dissolved in chloroform, and diethyl bis(2-ethylhexanoate) was used as the internal standard. A 1m glass column filled with 5% OV-101/Chromsorb G-AW.DMCS (200-250 μm) and a hydrogen flame detector were used to separate and determine the fenbucarb by gas chromatography. A1.2 Instruments and Equipment
Gas chromatograph: with hydrogen flame ionization detector and glass column head. Chromatographic data processor.
Chromatographic column: 1000mmX3.4mm (id) glass column. Column filling: 5% OV-101/Chromsorb G-AW.DMCS (200-250 μm). Injector: 1 μL.
Volume flask: 10 mL.
Pipette: 1 mL.
A1.3 Reagents and solutions
Chloroform: analytical grade.
Fenbucarb standard: greater than or equal to 99.5%. Internal standard: diethyl oxadicarb, which should not contain impurities that interfere with analysis. Stationary liquid: OV-101.
Carrier: ChromsorbG-AW.DMCS (200~250 μm). Internal standard solution: 100 g/L diethyl oxadicarb chloroform solution, stored in a refrigerator, and can be used only after returning to room temperature. A1.4 Preparation of chromatographic columns
A1.4.1 Application of stationary liquid
Weigh about 0.5g OV-101 in a 200ml beaker, add a little chloroform, stir with a glass rod to completely dissolve OV-101, then add an appropriate amount of chloroform (the solvent should just cover the carrier), and stir well. Pour 10g of the weighed carrier into the beaker at once, place the beaker under an infrared lamp to dry, and gently shake the beaker from time to time to keep it in a uniform state. When the solvent evaporates and is almost dry, place the beaker in a 100℃ oven and dry it for 1 hour.
A1.4.2 Filling of chromatographic column
Connect a funnel to the inlet end of the clean and dry chromatographic column, wrap a clean gauze at the outlet end, and connect it to the vacuum pump with a clean rubber tube. Turn on the vacuum pump, pour the filler in several times from the funnel, and tap the column wall continuously to make the filler fill the chromatographic column tightly and evenly, then plug a small ball of silanized glass wool at each end of the column and press it appropriately to keep the filler from moving. A1.4.3 Aging of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, and temporarily do not connect the outlet end to the detector. Raise the temperature to 250℃ in stages at a carrier gas flow rate of about 20mL/min. After aging at this temperature for at least 24h, connect the outlet end of the column to the detector. A1.5 Gas chromatography operating conditions
Temperature (℃): vaporization chamber 180;
column temperature 155;
detection chamber 180.
Gas flow rate (mL/min): carrier gas (N2) 60; hydrogen 50;
air 500.
Retention time (min): fenbucarb 5.45; internal standard 7.86.
Injection volume: 0.3μL.
Determination method: internal standard method.
A typical gas chromatographic separation diagram is shown in Figure A1.
HG 3619-1999
1-Solvent; 2-Impurity; 3-fenbucarb; 4 Internal standard diagram A1 Gas chromatographic separation diagram of fenbucarb
The above operating parameters are typical. According to the characteristics of the instrument, the given parameters can be appropriately adjusted to obtain the best effect. A1.6 Determination steps
A1.6.1 Preparation of standard solution
Weigh 0.1g of the standard sample of famoxadicarb (accurate to 0.0002g), place it in a 10mL volumetric flask, add 1.0mL of the internal standard solution, and then add 4mL of chloroform, shake well and set aside.
A1.6.2 Preparation of sample solution
Weigh a sample containing about 0.1g of famoxadicarb (accurate to 0.0002g), place it in a 10mL volumetric flask, and perform the following operations in the same manner as A1.6.1. A1.6.3 Determination
Under the above operating conditions, after the instrument is stable, use a microsyringe to inject several needles of the standard solution. When the relative peak height ratio of two adjacent needles changes by less than 1.5%, perform the determination in the order of standard solution, sample solution, sample solution, and standard solution. A1.7 Calculation
Average the ratio of the peak height of the two sample solutions and the two standard solutions before and after the sample solution to the peak height of the internal standard. The content of the second but carb (X) expressed as a mass percentage is calculated according to the formula (A1): r2m,P
wherein: r-
the average value of the peak height ratio of the second but carb to the internal standard in the standard solution; r2——the average value of the peak height ratio of the second but carb to the internal standard in the sample solution, the mass of the second but carb standard sample, g,
m2——the mass of the second but carb sample, g;
P——the mass percentage of the second but carb in the standard sample. A1.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.5%. A2 Colorimetric determination method of o-sec-butylphenol (free phenol) This method can be used for production control analysis.
A2.1 Method Summary
(A1)
O-sec-butylphenol reacts with sodium nitrite under acidic conditions to generate nitroso-o-sec-butylphenol, which forms a yellow wake-type compound after adding methylamine solution. The spectrophotometric determination is carried out at a wavelength of 410nm. A2.2 Reagents and Solutions
Methanol: analytical grade.
Hydrochloric acid: analytical grade.
Sodium nitrite: analytical grade.
30% methylamine solution: analytical grade.
HG 36191999
O-sec-butylphenol standard: content greater than or equal to 99%. Hydrochloric acid solution: 0.1mol/L. Prepared according to the method specified in GB/T601. Sodium nitrite solution: c(NaNO,)=1mol/L. Weigh 1.7g sodium nitrite, place it in a 25mL volumetric flask, dissolve it with water and make up to volume, shake well for later use (prepare and use only on the same day). Standard solution of o-sec-butylphenol: weigh 0.01g o-sec-butylphenol (accurate to 0.0002g), place it in a 100ml volumetric flask, add acetone to dissolve it and make up to volume, shake well for later use.
A2.3 Instruments and equipment
Spectrophotometer.
Thermostatic water bath.
Volume flask: 25mL, 100mL.
Pipette: 0. 5 mL; 2 mL.
Colorimetric tube with stopper: 25mL.
A2.4 Determination steps
Weigh the sample of the original drug of fenbucarb containing 0.0025g of o-sec-butylphenol (accurate to 0.0002g), place it in a 25mL volumetric flask, dissolve it with acetone and make up the volume. Pipette 0.2mL of the test solution into a 25mL colorimetric tube, add 1.5mL of hydrochloric acid solution, add 2mL of sodium nitrite solution along the wall, stir for 1min, place it in a 30℃ water bath for 20min, then add 0.25mL of 30% methylamine solution, dilute it with water to 10mL, and measure the optical density at a wavelength of 410nm with water as the reference solution. At the same time, do a blank experiment.
Take another 0.2mL of o-sec-butylphenol standard solution and measure the absorbance according to the sample determination procedure. A2.5 Calculation
The content of o-sec-butylphenol (X,) expressed as mass percentage is calculated according to formula (A2): X, = 0. 25 EamiP
Wherein: E1——the absorbance measured by standard o-sec-butylphenol minus the absorbance after blank, E2
the absorbance measured by the sample minus the absorbance after blank; the mass of the standard sample, g,
the mass of the sample, g;
P is the mass percentage of the o-sec-butylphenol standard; 0.25——conversion factor.
A2.6 Allowable difference
The relative deviation of the results of two parallel measurements should not exceed 20%. (A2)3 Instruments and equipment
Spectrophotometer.
Thermostatic water bath.
Volume flask: 25mL, 100mL.
Pipette: 0.5 mL; 2 mL.
Colorimetric tube with stopper: 25mL.
A2.4 Determination steps
Weigh the sample of 0.0025g of o-sec-butylphenol (accurate to 0.0002g), place it in a 25mL volumetric flask, dissolve it with acetone and make up the volume. Pipette 0.2mL of the test solution into a 25mL colorimetric tube, add 1.5mL of hydrochloric acid solution, add 2mL of sodium nitrite solution along the wall, stir for 1min, place it in a 30℃ water bath for 20min, then add 0.25mL of 30% methylamine solution, dilute it to 10mL with water, and measure the optical density at a wavelength of 410nm with water as the reference solution. Perform a blank experiment at the same time.
Take another 0.2 mL of o-sec-butylphenol standard solution and measure the absorbance according to the sample determination procedure. A2.5 Calculation
The o-sec-butylphenol content (X,) expressed as mass percentage is calculated according to formula (A2): X, = 0.25 EamiP
Wherein: E1——the absorbance measured by the standard o-sec-butylphenol minus the absorbance after blank, E2
the absorbance measured by the sample minus the absorbance after blank; the mass of the standard sample, g,
the mass of the sample, g;
Pthe mass percentage of the o-sec-butylphenol standard; 0.25——conversion factor.
A2.6 Allowable difference
The relative deviation of the results of two parallel measurements should not be greater than 20%. (A2)3 Instruments and equipment
Spectrophotometer.
Thermostatic water bath.
Volume flask: 25mL, 100mL.
Pipette: 0.5 mL; 2 mL.
Colorimetric tube with stopper: 25mL.
A2.4 Determination steps
Weigh the sample of 0.0025g of o-sec-butylphenol (accurate to 0.0002g), place it in a 25mL volumetric flask, dissolve it with acetone and make up the volume. Pipette 0.2mL of the test solution into a 25mL colorimetric tube, add 1.5mL of hydrochloric acid solution, add 2mL of sodium nitrite solution along the wall, stir for 1min, place it in a 30℃ water bath for 20min, then add 0.25mL of 30% methylamine solution, dilute it to 10mL with water, and measure the optical density at a wavelength of 410nm with water as the reference solution. Perform a blank experiment at the same time.
Take another 0.2 mL of o-sec-butylphenol standard solution and measure the absorbance according to the sample determination procedure. A2.5 Calculation
The o-sec-butylphenol content (X,) expressed as mass percentage is calculated according to formula (A2): X, = 0.25 EamiP
Wherein: E1——the absorbance measured by the standard o-sec-butylphenol minus the absorbance after blank, E2
the absorbance measured by the sample minus the absorbance after blank; the mass of the standard sample, g,
the mass of the sample, g;
Pthe mass percentage of the o-sec-butylphenol standard; 0.25——conversion factor.
A2.6 Allowable difference
The relative deviation of the results of two parallel measurements should not be greater than 20%. (A2)
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