Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2463.3-93
Buprofezin EC
Published on 1993-07-05
Ministry of Chemical Industry of the People's Republic of ChinabzxZ.net
Implemented on 1994-01-01
Chemical Industry Standard of the People's Republic of China
Buprofezin
Subject Content and Scope of Application
HG 2463.3-93
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for Buprofezin EC. This standard applies to Buprofezin EC prepared from Buprofezin technical with suitable emulsifiers, solvents and cosolvents. Active ingredient: Buprofezin
Chemical name; 2-tert-butylimino-3-isopropyl-5-phenyl-3,4,5,6-tetrahydro-2H-1,3,5-thiadiazin-4-one Structural formula:
Molecular formula: C16H23NOS
CH(CHs)2
NC(CHs)
Relative molecular weight: 305.5 (according to the international relative atomic mass in 1989) Reference standard
GB/T1600
GB/ T1603
GB1604
GB1605
GB3796
GB4838
3 Technical requirements
Method for determination of moisture content in pesticides
Method for determination of stability of pesticide emulsions
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
Emulsifiable concentrate pesticide packaging
3.1 Appearance: Yellow-brown to red-brown liquid, without obvious visible sediment. 3.2
Buprofezin emulsifiable concentrate shall meet the following requirements: Item
Buprofezin content, %
Acidity (in HSO,), %
or alkalinity (in NaOH), %
Water, %
Emulsion stability (diluted 500 times)
Low temperature stability\)
Hot temperature stability\》
Note: 1) Test at least once every six months.
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 1993
Implementation on January 1, 1994
4 Test methods
4.1 Determination of appearance
Visual inspection
4.2 Determination of thiophanate-methyl content
4.2.1 Summary of method
HG2463.3—93
The sample was dissolved in toluene, and thiophanate-methyl was separated and determined by gas chromatography using a stainless steel column filled with 5% ovV-101/GasChromQ and a flame ionization detector, with n-tricosane as the internal standard. 4.2.2 Reagents and solutions
Toluene (GB684);
Internal standard: n-tricosane (should not contain impurities that interfere with the analysis); dicyclohexyl phthalate (should not contain impurities that interfere with the analysis); stationary phase: 0V-101;
Carrier: GasChromQ180~250um (60~80 mesh); Buprofezin standard: known content, greater than 98.0% Internal standard solution: weigh 8g of n-tricosane in a 250mL volumetric flask, dissolve it with toluene, dilute to the scale, and shake well. 4.2.3 Instruments
Gas chromatograph: with flame ionization detector; recorder: full scale range 5mV (or chromatographic microprocessor) micro-injector: 10uL,
Chromatographic column: 1m long, 2mm inner diameter stainless steel column, filled with 5% oV-101/GasChromQ180~250um. 4.2.4 Preparation of chromatographic column
4.2.4.1 Coating of stationary liquid:
Accurately weigh 0.5g OV-101 and place it in a 250mL 24* standard mouth round bottom flask, add enough toluene to dissolve OV-101 completely, add a certain amount (about 10g) of carrier according to the ratio of the stationary liquid, and just be immersed in the stationary liquid solution. Use a rotary evaporator for coating. Under reduced pressure, start the rotary evaporator and heat it with a water bath until the solvent evaporates to near dryness, then place it in a 120℃ oven and dry it for 2 hours. Take it out, cool it, and sieve it.
4.2.4.2 Filling of the chromatographic column:
Connect a small funnel to the inlet of the cleaned and dried stainless steel column, plug an appropriate amount of glass wool (after silanization treatment) into the outlet, wrap it with gauze, and connect it to the vacuum pump through a rubber tube. Start the vacuum pump, add the column filling material in batches from the funnel, and tap the column tube continuously to make the filling material uniform. After the chromatographic column is tightly filled, stop the vacuum pump, plug a small ball of glass wool at the inlet, and press it appropriately to prevent the filling material from moving. 4.2.4.3 Aging of chromatographic column:
Connect the inlet end of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the outlet end to the detector for the time being. Pass nitrogen at a flow rate of about 15mL/min, increase the temperature to 250℃ in stages, and age at this temperature for at least 24h. After cooling down, connect the outlet end of the column to the detector. 4.2.5 Gas chromatography operating conditions
Column chamber: 190℃;
Vaporization chamber: 240℃;
Detection chamber: 220℃;
Gas flow rate
Carrier gas (nitrogen): 10mL/min, column head pressure 0.12MPa; Hydrogen: 30mL/min;
Air: 600mL/min;
Retention time
Buprofezin about 9min;
n-tricosane about 17min,
dicyclohexyl phthalate about 24min.
HG2463.3—93
The above operating conditions are typical operating parameters. When adopting this standard, the given operating parameters can be appropriately adjusted according to the characteristics of different instruments in order to obtain the best effect.
4.2.6 Determination steps
4.2.6.1 Preparation of standard solution
Weigh about 0.12g (accurate to 0.2mg) of thiazide standard sample into a stoppered glass bottle, accurately add 5mL of internal standard solution with a pipette to dissolve the sample, shake well and wait for measurement.
4.2.6.2 Preparation of sample solution
Weigh about 0.6g (accurate to 0.2mg) of sample into a stoppered glass bottle, accurately add 5mL of internal standard solution with a pipette to dissolve the sample, shake well and wait for measurement.
4.2.6.3 Determination
HG2463.3—93
Under the chromatographic operating conditions specified in 4.2.5, after the instrument is stable, inject several needles of standard solution until the peak height ratio of two adjacent needles is basically stable, and analyze in the following order: standard solution, sample solution, sample solution, standard solution. Use a micro-injector to inject an appropriate amount of the solution to be tested each time. On the chromatograms of the two standard solutions and the sample solution, the difference between the peak height (peak area) ratio of thiazinone and the internal standard divided by the average value should not be greater than 1.5%, otherwise repeated injection is required. 4.2.6.4 Result calculation
Calculate the peak height (peak area) ratio of the two sample solutions and the two standard solutions before and after the sample respectively. The mass percentage of thiazinone in the sample (x,) is calculated according to formula (1):
Where 1 is the average value of the peak height (peak area) ratio of thiazinone and the internal standard in the sample solution; T2 is the average value of the peak height (peak area) ratio of thiazinone and the internal standard in the standard solution; mi is the mass of the sample, g;
m2 is the mass of the standard, g;
is the mass percentage of the standard.
4.2.6.5 Allowable difference
The absolute difference between two parallel determinations should not be greater than 0.5%. 4.3 Determination of pH
4.3.1 Reagents and solutions
Sodium hydroxide (GB629) standard titration solution: c(NaOH)=0.05mol/L; hydrochloric acid (GB622) standard titration solution: c(HC1)=0.05mol/L; methyl red (HG3-958) ethanol solution: 1g/L; bromocresol green (HG3-1220) ethanol solution: 1g/L; anhydrous ethanol (GB678);
Mixed indicator solution: take 2mL1g/L methyl red and 10mL1g/L bromocresol green and mix them evenly. 4.3.2 Determination steps
Weigh 2g of sample (accurate to 0.2mg), place in a 250mL conical flask, add 50mL of anhydrous ethanol, add 5 to 6 drops of mixed indicator solution, titrate with 0.05mol sodium hydroxide standard titration solution to light green as the end point, and do a blank determination at the same time. If the test solution is alkaline, it is necessary to titrate with 0.05mol/L hydrochloric acid standard titration solution to yellow as the end point, and also do a blank determination. The mass percentage of free acid (X2) is calculated according to formula (2): X100=4. 9c(V,-V)
c(V,-V.)0.049
wherein: c-
actual concentration of sodium hydroxide standard titration solution, mol/L; -volume of sodium hydroxide standard titration solution consumed in titration blank, mL; V1-volume of sodium hydroxide standard titration solution consumed in titration sample, mL; m sample weight, g;
0.049-mass of sulfuric acid in grams equivalent to 1.00mL of sodium hydroxide standard titration solution (c(NaOH)=1.000mol/L).
mass percentage of free alkali (X:) is calculated according to formula (3): Xs=ciV-Vo)0. 040_4. 00r(V:-V)m
actual concentration of hydrochloric acid standard titration solution, mol/L; where: C-
V. ——Volume of standard hydrochloric acid solution consumed in titration blank, mL; V2—Volume of standard hydrochloric acid solution consumed in titration sample, mL; 4
m Sample weight, g;
HG2463.3—93
0.040——Mass of sodium hydroxide expressed in grams equivalent to 1.00mL standard hydrochloric acid solution (Cc(HCI)=1.000mol/L). 4.4 Determination of water content
Carry out according to the Karl Fischer method in GB/T1600. 4.5 Emulsion stability test
Take 0.2mL emulsifiable concentrate and carry out according to GB/T1603. 4.6 Low temperature stability test
Put 50g of sample in a 100mL beaker, put it in a refrigerator or ice bath, maintain the temperature at 0±1℃, and leave it for 1h. During the storage period, stir once every 15 minutes, each time for 30 seconds, and check whether there is oil or crystal precipitation in the cup. If there is no oil or crystal precipitation, it is qualified. 4.7 Hot Storage Stability Test
4.7.1 Instrument
Oven: temperature control accuracy is ± 2℃ (or constant temperature water bath); syringe: capacity is 30mL, long neck;
Medical syringe: volume is greater than 10mL.
4.7.2 Determination steps
Use a medical syringe to absorb about 30mL of sample and inject it into a clean syringe (do not let the sample touch the neck of the syringe); place the syringe in an ice salt bath and seal it with a gas lamp (to avoid solvent evaporation), and seal at least 2 bottles. After weighing the sealed syringe, put it into a metal container first, and then place it in a 54±2℃ oven and store it for 14 days. After taking out the Anyan from the oven, cool it and weigh it for leak test. If there is no leakage, all inspection items can be completed within 24 hours. After hot storage, the various indicators of thiamethoxam emulsifiable concentrate should still meet the requirements of this standard. 5 Inspection rules
5.1 Sampling method: Sampling should be carried out according to the "Sampling of emulsions and liquid states" method in GB1605. The sampling package is determined by random method, and the final sampling volume should be not less than 250g.
5.2 Acceptance rules: GB1604 standard shall be implemented. 6 Marking, packaging, transportation and storage
6.1 The marking and packaging of thiamethoxam emulsifiable concentrate shall comply with the relevant provisions of GB3796 and GB4838. 6.2 The thiamethoxam emulsifiable concentrate is packaged in brown glass bottles, with a net weight of 100g per bottle. The outer packaging is a calcium plastic box, with a net weight of 5kg per box. 6.3 Storage and transportation shall be carried out in accordance with the relevant provisions of GB4838.
6.4 Warranty period: Under the storage conditions specified in this standard, the warranty period of buprofezin EC is at least two years from the date of production. During the warranty period, all indicators of buprofezin EC shall still meet the requirements of this standard. Additional remarks:
This standard was proposed by the Science and Technology Department of the 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. This standard was drafted by the Shanghai Pesticide Factory of Asia Pacific Agrochemical (Group) Company. The main drafters of this standard are Zhu Peiming, Wen Lili, Wang Yunsheng, and Zhu Dengwu. 5
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