ICS65.10D
Chemical Industry Standard of the People's Republic of China
HG329132972001
Published on January 24, 2002
Implemented on July 1, 2002
Published by the State Economic and Trade Commission
Registration No.: 10081-2002
HG3294—2001
Chapter 3 and Chapter 5 of this standard are regulatory, and the rest are recommendatory. This standard is a revision of the mandatory chemical industry standard "IG3291-1989 Three Tons of Emulsion". The main technical differences between this standard and HG3294-1989 are: the acidity index is changed from less than or equal to 5% to less than or equal to 4%; the emulsion stability is changed from 5 times the screening to 20 times diluted. The control index for oxygen content is added and is now set at less than or equal to 1%. The determination of full stability adopts the International Pesticide Analysis Cooperation (CAC) method. This standard will replace HG329-19 from the month of implementation. 89, This standard was proposed by the former State Administration of Petroleum and Chemical Industry. The National Pesticide Standardization Technical Committee issued this standard. The responsible person for the standard change was Yangzhou Chemical Research Institute. The participating drafting units of this standard are Sichuan Chemical Research and Design Institute, Jiangsu Jianhu County Pesticide Adjuvant Factory, and Jiangsu Zhangjiagang Second Pesticide Factory.
Main contributors: Gong Xiafan, Zhou Duhua, Yu Huixing, Xu Lansheng, Mao Hong: This standard was first published as a professional standard in 1989, and was converted into a mandatory chemical industry standard in 2000, and the terminal number was changed to HE-3294-1989.
This standard is not entrusted to the Secretariat of the National Pesticide Standardization Technical Committee. 27
Chemical Industry Standard of the People's Republic of China
20% Triadimefon Emulsifiable Concentrate
20% Irladimcfon Enulsifiable Other names, structural formulas and basic physical and chemical properties of Cuncentnites triazone are as follows: 1SO4, Irsadimcfon
CIPAC number: 353
Chemical name: 1-(4-chloro-2-nitropropene)-1,1-(1-1,2,4-dimethylbutyl-2-one Structure:
Empirical formula: H.CIN,O
Molecular mass: 28.75<According to 19974 International (About quality) Biological source: soft
Melting point: 33.3
HG3294-2001
Vapor (20%), C.
Decomposition g/1., 20) 0.97 in n-hexene 10~2, isochloroethane greater than 200 in 100*-20C, outside hexane 12 for RMB 40
"Range
This standard defines the requirements, test methods and marking, labeling, packaging and transportation of diazole emulsions. This standard applies to diazole emulsions that are suitable for preparation or use in preparations containing three or more drugs and emulsifiers that meet the standard. 2 Referenced standards
The following referenced standards contain provisions that are applicable to the provisions of this standard by reference in other standards. When this standard was published, the versions shown are valid: All standards are not applicable. In case of non-use of this standard, the parties should explore the possibility of using the following standards to start the new version: GVT601-19B Preparation of standard solution for chemical formulation analysis (quantity analysis) GB160C-7318) Method for determination of pesticide water
B/16(3-19731989) Method for determination of stability of pesticide emulsion 4: H/T1%04—1995 Acceptance criteria for commercial pesticides
G3/T16051979(1989) Sampling method for commercial pesticides GB3716—1999 Pesticide packaging rules
CB4838-2000 Pesticide emulsion packaging
3 Requirements 3.1 The appearance should be a homogeneous liquid without visible slippery substances and sediment. Approved by the National Economic and Trade Commission on January 24, 2002, and implemented on July 1, 2002. Triadimefon emulsifiable concentrate should meet the following requirements: Suitable for use, with a chlorine content of 1%, % moisture content. Acid film is measured in SC. Emulsion reduction certificate: 20% low quality. Storage quality is required. HG 3294—2001. Control items and indicators of triadimefon emulsifiable concentrate. Note: During normal production, low temperature quality and natural string quality tests are performed. Each piece is tested at least once. 4 Test methods 4.1 Sampling
According to GH/T1635-197 (1089)+\sampling method for emulsion and solid state\selection: use random number method to determine the sampling equipment: the final sampling shall be no less than 20ril4.2 Identification test
Gas chromatography, this test can be carried out with the required orientation of triazole: under similar chromatographic operating conditions: the retention time of the sample color peak and the retention time of triazole in the standard sample, the relative difference should be within 1.5%: Liquid chromatography: under suitable chromatographic operating conditions, the retention time of the chromatographic peak of the sample liquid and the retention time of triazole in the standard liquid, the relative difference should be within 1.5%. 4.3 Determination of triadimefon content
4.3.1 Summary of the method
The sample is dissolved in methane, and the triadimefon in the sample is separated and determined by gas chromatography-mass spectrometry using a stainless steel column filled with 0V-1?/h-mosorbAWDMCS and a hydrogen initial ionization detector.
4.3.2 Reagents and probes
Trichloromethane.
Triadimefon standard sample, known to contain more than or equal to 99.9% of the internal standard, dibutyl phthalate or di-n-butyl phthalate, and no impurities to be analyzed. Fixed pressure: 0V-17,
+: Chromnsarb G AW DMCSi_B0--250μm). Internal standard, 12.C9B dibutyl aldehyde or 7.5V K dibutyl ketone diisocyanate was taken in a 1100 ml volumetric flask and dissolved in 2% ethanol to the mark. 4.3.3 Apparatus
Chromatography: flame ionization device, negative ionization processor.
Chromatographic medium: 1 x 3 rmci.d. Non-frequency rigid sample filling: U11 hramogarht AwDMCs (:80~-25um)t. Stationary liquid: (solvent + stationary liquid) = 3:10 mass ratio). 35
4.3.4 Preparation of chromatographic samples
HG324—2001
Prepare 0.5 g of V-17 stationary liquid in 250 ml of flask, add an appropriate amount (slightly larger than the volume of the added solution) of C, stir the solution with a glass shaker to completely degrade V-17, and add 0.5 g of C-17 stationary liquid in 250 ml of flask. Multi-carrier, light aldehyde drug, make it uniform and quick-dry, then keep it in a drying oven at 100℃ for 1h, take it out and put it in a desiccator to cool to room temperature.) Filling of chromatographic column
Connect a small funnel to the port of the washed chromatographic column, and add the prepared filling block into the column. At the same time, gently remove the support wall until it is 1.cm away from the sample outlet. Move the funnel to the inlet of the chromatographic column, seal the outlet with a small piece of silanized cotton, connect it to the vacuum system through a rubber hose, and then add the specified Fill the column with material and gently shake the sample wall continuously to make it evenly distributed and dense. After filling, a small amount of glass is also plugged in the inlet and appropriate pressure is applied to prevent the column filling from being moved.) Aging of the chromatographic column
Connect the chromatographic discharge chamber at the working end to the vaporization chamber and the outlet end to the detector. Introduce carrier gas at a flow rate of 10mL/min (V,). Raise the temperature to 230 in stages and age at the temperature for at least 24h. 4.3.5 Gas phase mixing condition
Column chamber 230, vaporization chamber 230; detector chamber 250. Gas washing volume (ml/min), atmosphere (N) 30. Oxygen 30. Air 300. Retention time (mm): 12:16.3:10. The above operating parameters are typical, and according to the characteristics of different instruments, appropriate test parameters should be applied to the given operating parameters to obtain the typical triazole oil and gas phase color. See Figure 1. 1
一; 2-3 tons of two general two positive" 4-one two normal two positive" 1 sleep milk sleeve gas cabinet color drama
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
Weigh the standard 12g of triazole to an accuracy of 0.0002g), place it in a 25ml volumetric flask, use a transfer scale to add 10ml internal standard box, and shake well.
4.3.6.2 Preparation of sample solution
Weigh 0.12 g of dihydrogen ketone (accurate to 0.1K10 2 g), place in a 25 ml volumetric flask, and mix with 4.3.6.1 Add 1 mL of internal standard in a transfer tube and obtain the result. 4.3.6.3 Determination TEG3294-2001 Replace the above chromatographic operation conditions. After the instrument is stabilized, inject several injections of standard sample continuously and calculate the reproducibility of the corresponding values of each injection. When the change of the relative response value of two adjacent injections is less than 1.2, analyze the standard solution, sample solution, sample filter and standard sample solution in sequence. 4.3.7 Calculation Average the ratio of the peak area of the three responses to the peak of the flash substance in the two injections of sample solution and the two injections of standard sample solution before and after the sample.
The mass fraction of the three mixtures of the sample is X, (%): Calculated according to the formula: x, =
The half-mean of the peak area ratio of the triazole in the standard sample to the internal standard;
The half-mean of the peak area ratio of the triazole in the sample to the internal standard: The mass fraction of the standard sample,
The mass fraction of the triazole in the test sample, %
4.3.8
The difference between the results of two parallel determinations shall not exceed 0.5%. The arithmetic mean value was taken as the determination result. 4.4 Determination of p-chlorophenol content
4.4.1 Method summary
The sample was dissolved in ethyl acetate and ethyl acetate water was used as the mobile phase. The liquid chromatography with a particle size of 1.000 nm and UV detector (370 nm) was used to separate and determine p-chlorophenol in the sample by reverse phase high performance chromatography. The external standard method was used. 4.4.2 Formula: Acrylic acid and chlorinated water.
Water·freshly distilled water.
Mobile phase: CFCN·TI,) 49::1, filtered through a 45-pore light filter membrane and purged in an ultraviolet vortex for 10 smin.
Compare with a known standard sample, etc.
4. 4.3 Equipment
High efficiency phase-loss chromatograph: external detector with adjustable wavelength spectral column t25cmX4.cmm (id> stainless steel Note. Lichrospher-()DS field filled with internal particles. Particle size 5in by wave bath clarification
drop filter: filter membrane pore size o.ipn:
4.4.4 High-efficiency liquid chromatography working conditions
flow CHCN: HO = 43: 51
flow rate: .L/min:
Note: room temperature, humidity,
grid measurement wavelength: 276nm.
injection volume: 101,
retention time: about 5.5mm for onion phenyl ester. The above parameters are typical and can be selected. According to the instrument, the chromatographic notes and the given parameters should be adjusted appropriately to obtain the best results. A typical chromatographic analysis of the chlorinated acid in the emulsifiable concentrate is shown in Figure 2. 4.4.5 Preparation steps 4.4.5.1 Preparation of standard sample HG3294-2001 1 Chlorophenol step. 2-3-1 Chlorophenol in the emulsifiable concentrate Take 0.0 g (accurate 0.0002 e) of the standard sample by pulse, place in a 50 mL volumetric medium, dilute with ethyl acetate, make up to volume, and insert a spoon. Use a micropipette to transfer 1 mL of the above solution, place in a 30 mL volumetric bottle, dilute to the mark with ethyl acetate, and insert a spoon. 4.4. 5.2 Preparation of sample solution
Weigh a sample containing 2.01 μg of parachlorobenzene (accurate to .U2s), add 55 ml of the sample solution, add about 49 mM ethyl acetate degradation test phase, and place the solution in an ultrasonic bath for bacteria detection. After the solution returns to the specified temperature, add ethyl acetate to the specified rate, mix well, and filter through a 0.45 μm pore light membrane.
4.4.5.3 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continuously test the number of needles and melt. , until the area difference between the two adjacent needles is less than 1.5%, then sample and analyze in the order of standard reduction, sample liquid reduction, and sample solution reduction. 4.4.6 Calculation
The peak segments of the two needle sample solution and the peak segments of the standard sample before and after the sample are respectively calculated to be the mass fraction X (%) of the paraben in the sample, and calculated according to formula (2): X
· The average of the peak areas of the paraben in the standard sample reduction: Where A, -
sample The average area of the peak of chlorophenol in the droplet is: The mass of the standard sample·g:
The mass of the sample R:
IIG32942001
The mass of the standard sample is the mass of the nitrogen-resistant sample. 4.5 Determination of water content
According to GB/16W-195 (1053) "Carl Microhugh\ method, the determination is allowed to be made with appropriate accuracy. 4.6 Determination of micromolarity
4.6.1 Reagents and solutions ||tt ||Sodium hydroxide standard titration solution (Na2O3=.03ml/L, prepared according to GB/T6u1-158a4.1. Red ethanol solution: 2 finger kill,
4.6.2 Determination step
Weigh 0.0002g of sample 2 and put it in a 250TL round bottle. Add 100L of liquid to make the sample uniformly dissolved, draw 2 indicator, use sodium hydroxide standard to determine the full point when the indicator changes from red to yellow, and make a vacuum determination at the same time.
4.6.3 Calculation
The estimated acidity X (%) expressed in terms of the pressure base is calculated using the following formula: X = sV. Ye3x6.045x11
Volume---volume of sodium hydroxide standard titrant consumed in titration of sample solution, ml.W.
Volume of sodium hydroxide auxiliary standard titrant consumed in titration of blank solution, ml.E:
Comparison with 1.00mL emulsification potential standard titrantThe parameters that can be selected on the sheet are typical and can be adjusted according to the instrument performance. The chromatographic parameters and the given working parameters can be adjusted appropriately to obtain the best results. A typical chromatographic analysis of the chlorinated acid in the emulsifiable concentrate is shown in Figure 2.2
4.4.5 Preparation steps
4.4.5.1 Preparation of standard sample
HG3294-2001
1 Chlorophenol step. 2-3 sitting reward
Figure 2 Three-dimensional chromatographic analysis of chlorinated phenol in emulsifiable concentrate Take 0.0g of the chlorinated phenol standard sample (accurate 0.0002e), place in a 50ml tube, dilute with ethyl acetate, make up to volume, and insert a spoon. Use a micropipette to transfer 1UmL of the above solution, put it in a 30mL bottle, dilute to the mark with ethyl acetate, and insert a spoon.4.4. 5.2 Preparation of sample solution
Weigh a sample containing 2.01 μg of parachlorobenzene (accurate to .U2s), add 55 ml of the sample solution, add about 49 mM ethyl acetate degradation test phase, and add the sample solution in an ultrasonic bath. After the solution returns to the specified temperature, add ethyl acetate to the specified rate, mix well, and filter through a 0.45 μm pore light membrane.
4.4.5.3 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continue to observe the number of needles and melt until When the area difference between two adjacent injections is less than 1.5%, the samples are injected and analyzed in the order of standard reduction, sample liquid reduction, and sample dissolution. 4.4.6 Calculation
The peak segments of the two injections of sample solution and the peak segments of the sample before and after the sample are respectively averaged to obtain the mass fraction X (%) of the sample, and calculated according to formula (2): X
· The average of the peak areas of the sample dissolution and the sample dissolution: Where A, -
The peak area of the sample dissolution The average of the peak area of chlorophenol is: The mass of the standard sample·g:
The mass of the sample R:
IIG32942001
The mass of the standard sample is selected for nitrogen resistance. 4.5 Determination of water content
According to GB/16W-195 (1053) "Carl Microhugh\ method, the determination is allowed to be made with appropriate accuracy. 4.6 Determination of micromol
4.6.1 Reagents and solvents
Sodium hydroxide Standard titration solution (Na2O3 = 0.03 ml/L, prepared according to GB/T6u1-158a4.1. Red ethanol solution: 2 finger killing,
4.6.2 Determination step
Weigh 20.0002g of sample and place it in a 250TL beaker. Add 100L of liquid to make the sample uniformly dissolved, draw 2 indicator, use sodium hydroxide to determine the full point when the red turns to yellow, and make a vacuum determination at the same time.
4. 6.3 Calculation
The estimated acidity X (%) expressed in terms of the pressure base is calculated by the following formula: X = sV. Ye3 x 6. 045 x 11
Volume of sodium hydroxide standard titrant consumed in titration of sample solution, ml.W.
Volume of sodium hydroxide auxiliary standard titrant consumed in titration of blank solution, ml.W.
Volume of sodium hydroxide auxiliary standard titrant consumed in titration of blank solution, ml.E:
Comparison with 1.00mL emulsification potential standard titrantThe parameters that can be selected on the sheet are typical and can be adjusted according to the instrument performance. The chromatographic parameters and the given working parameters can be adjusted appropriately to obtain the best results. A typical chromatographic analysis of the chlorinated acid in the emulsifiable concentrate is shown in Figure 2.2
4.4.5 Preparation steps
4.4.5.1 Preparation of standard sample
HG3294-2001
1 Chlorophenol step. 2-3 sitting reward
Figure 2 Three-dimensional chromatographic analysis of chlorinated phenol in emulsifiable concentrate Take 0.0g of the chlorinated phenol standard sample (accurate 0.0002e), place in a 50ml tube, dilute with ethyl acetate, make up to volume, and insert a spoon. Use a micropipette to transfer 1UmL of the above solution, put it in a 30mL bottle, dilute to the mark with ethyl acetate, and insert a spoon.4.4. 5.2 Preparation of sample solution
Weigh a sample containing 2.01 μg of parachlorobenzene (accurate to .U2s), add 55 ml of the sample solution, add about 49 mM ethyl acetate degradation test phase, and add the sample solution in an ultrasonic bath. After the solution returns to the specified temperature, add ethyl acetate to the specified rate, mix well, and filter through a 0.45 μm pore light membrane.
4.4.5.3 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continue to observe the number of needles and melt until When the area difference between two adjacent injections is less than 1.5%, the samples are injected and analyzed in the order of standard reduction, sample liquid reduction, and sample dissolution. 4.4.6 Calculation
The peak segments of the two injections of sample solution and the peak segments of the sample before and after the sample are respectively averaged to calculate the mass fraction X (%) of the sample to benzene, and the mass fraction X (%) is calculated according to formula (2): X
· The average of the peak areas of the sample to benzene in the standard reduction: Where A, -
The peak area of the sample to benzene in the standard reduction: The average of the peak area of chlorophenol is: The mass of the standard sample·g:
The mass of the sample R:
IIG32942001
The mass of the standard sample is selected for nitrogen resistance. 4.5 Determination of water content
bzxZ.net According to GB/16W-195 (1053) "Carl Microhugh\ method, the determination is allowed to be made with appropriate accuracy. 4.6 Determination of micromol
4.6.1 Reagents and solvents
Sodium hydroxide Standard titration solution (Na2O3 = 0.03 ml/L, prepared according to GB/T6u1-158a4.1. Red ethanol solution: 2 finger killing,
4.6.2 Determination step
Weigh 20.0002g of sample and place it in a 250TL beaker. Add 100L of liquid to make the sample uniformly dissolved, draw 2 indicator, use sodium hydroxide to determine the full point when the red turns to yellow, and make a vacuum determination at the same time.
4. 6.3 Calculation
The estimated acidity X (%) expressed in terms of the pressure base is calculated using the following formula: X = sV. Ye3 x 6. 045 x 11
Volume of sodium hydroxide standard titrant consumed in titration of sample solution, ml.W.
Volume of sodium hydroxide standard titrant consumed in titration of blank solution, ml.W.
Volume of sodium hydroxide auxiliary standard titrant consumed in titration of blank solution, ml.E:
Comparison with 1.00mL emulsification potential standard titrant
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