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Professional Standard of the People's Republic of China
ZBG25017—90
Pyragon Blast Emulsion
Published on April 11, 1990
Published by the Ministry of Chemical Industry of the People's Republic of China and implemented on January 1, 1991
Professional Standard of the People's Republic of China
Pyragon Blast Emulsion
Subject Content and Scope of Application
ZBG25017—90
This standard specifies the technical requirements, inspection methods, inspection rules, and packaging, marking, transportation and storage requirements of Pyragon Blast Emulsion. This standard applies to Pyragon Blast Emulsion prepared from Pyragon Blast Technical Drug and suitable emulsifiers and solvents. Active ingredient: Rice Blast Lin
Chemical name, 1,3-dithiolane-2-ylidenemalonic acid diisopropyl ester Molecular formula: C12H18O,S2
Structural formula:
Relative molecular mass: 290.40 (international atomic weight in 1987) Reference standard
Method for determination of moisture content in pesticides
GB1600
GB1603
3 Method for determination of stability of pesticide emulsions
8 Packaging of emulsifiable concentrate pesticides
GB4838
3 Technical requirements
CH(CH)2
CH(CHa)2
3.1 Appearance: Orange-yellow or reddish-brown homogeneous liquid, without suspended matter or precipitation. 3.2 The rice blast-butyl emulsifiable concentrate shall also meet the following index requirements: Index name
Rhizoma blast-butyl content, % (m/m)
Water, % (m/m)wwW.bzxz.Net
Acidity (calculated as H2SO4), % (m/m)
Emulsion stability (diluted 200 times)
Low temperature stability 1)
Hot storage stability 2)
Note: 1) and 2) are random inspection items.
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 11, 1990 30% EC
40% EC
Implemented on January 1, 1991
4 Test methods
4.1 Determination of rice blast content
4.1.1 Summary of method
ZBG25017—90
The sample was dissolved in chloroform and determined by gas chromatography on a 5% SE-30 column using n-docosane as the internal standard using a hydrogen flame ionization detector.
4.1.2 Reagents and solutions
Standard sample of rice blast: known content, ≥99.0%; a.
n-Docosane: must not contain impurities that interfere with the chromatographic analysis; b.
Chloroform (GB682);
Stationary liquid: SE-30;
e. Carrier ChromosorbWAWDMCS, 6080 mesh; fF
Internal standard solution: accurately weigh about 2.2g of n-docosane in a 1000mL volumetric flask, dissolve and dilute to the scale with chloroform, and shake well;
Standard sample solution: accurately weigh about 0.09g (accurate to 0.0002g) of standard sample of rice blast, place it in a 25mL stoppered glass bottle, accurately add 20mL of internal standard solution with a pipette, and shake well. 4.1.3 Instruments
a. Gas chromatograph: hydrogen flame ionization detector; b. Chromatographic column: 1m long, 3mm inner diameter glass column (or stainless steel column), filled with 5% SE-30/ChtomosorbWAWDM-CS (60-80 mesh);
c. Recorder: 5mV (or use a data processor); d. Micro-injector: 10uL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
4.1.4.1.1 Coating of stationary liquid: Weigh 0.38g of stationary liquid into a 250mL beaker, add about 38mL of chloroform, and stir with a glass rod to completely dissolve the stationary liquid. After adding .g of 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, and shake the beaker while heating until the solvent evaporates and is almost dry. Then place it in a 120℃ oven to dry for 2 hours, take it out and put it in a desiccator for later use. 4.1.4.1.2 Filling of chromatographic column: Connect a small funnel to the inlet end of the cleaned and dried glass column (or stainless steel column), wrap the outlet end with gauze, and connect it to the vacuum pump with a rubber tube. Turn on the vacuum pump, pour the column filling material from the funnel in batches, and tap the tube wall continuously to make the filling material fill the chromatographic column evenly and tightly. Remove the chromatographic column and plug the two ends of the column with an appropriate amount of silanized glass wool. 4.1.4.1.3 Aging of chromatographic column: Connect the inlet end of the chromatographic process to the vaporization chamber, and do not connect the outlet end to the detector first. Slowly increase the temperature to 250℃ in stages at a carrier gas flow rate of about 15mL/min, and age it at this temperature for at least 48 hours. After cooling, connect the column outlet to the detector. 4.1.4.2 Chromatographic operating conditions
Column chamber: 195℃;
Vaporization chamber: 265℃;
Detector: 265℃;
Gas flow rate
Carrier gas (N,): 35mL/min
Hydrogen: 40mL/min;
Air: 300mL/min
Sensitivity: 2X10-\,
Paper speed: 3mm/min;
Injection volume: 1uL;
Retention time
Rice blasting agent is about 8.2min;
Internal standard is about 11.6min.
ZBG25017—90
The above chromatographic conditions are typical operating conditions, which can be adjusted appropriately according to the characteristics of the instrument to obtain the best effect. Gas chromatogram of rice blast emulsifiable concentrate
1-rice blast emulsifiable concentrate, 2-n-docosane
4.1.4.3 Preparation of sample solution
Weigh about 0.09g of rice blast emulsifiable concentrate sample (accurate to 0.0002g) containing rice blast emulsifiable concentrate, place it in a 25mL glass bottle with a cover, accurately add 20mL of internal standard solution with a pipette, and shake well.
4.1.4.4 Determination
After the instrument is stable, repeatedly inject 1uL of rice blast emulsifiable concentrate standard solution until the peak height ratio of two adjacent needles is basically stable (the change is within 1.5%), and then analyze in the following order:
a. Standard solution, b. Sample solution, c. Sample solution, d. Standard solution. 4.1.4.5 Calculation
Average the obtained peak height ratios of a, d and b, c, and calculate the mass percentage content of isoflurane in the sample according to formula (1): X1: Xi-
T.·mi·P
Ti·m2
ZBG25017-90
Wherein: 1——the average value of the peak height ratios of isoflurane to the internal standard in the standard solution; T2——the average value of the peak height ratios of isoflurane to the internal standard in the sample solution; m1——the weighed amount of isoflurane standard sample, gm2——the weighed amount of isoflurane sample, g; P——the percentage content of isoflurane standard sample, %. 4.1.5 Allowable difference
The difference between the two determination results: 30% emulsifiable concentrate should not be greater than 0.8%; 40% emulsifiable concentrate should not be greater than 1.0%4.2 Determination of moisture
Determine according to the Karl Fischer method in GB1600. 4.3 Determination of acidity
4.3.1 Reagents and solutions
a. 95% ethanol (GB679);
Standard titration solution of sodium hydroxide (GB629): c(NaOH)=0.02mol/L; c. Bromocresol green-methyl red indicator solution: Mix 3 parts of 1g/L bromocresol green ethanol solution with 1 part of 2g/L methyl red ethanol solution, shake well and mix. 4.3.2 Operation steps
Weigh 3-4g of sample (accurate to 0.001g) into a 250mL conical flask, add 60mL of 95% ethanol and 10 drops of mixed indicator solution, and titrate with sodium hydroxide standard titration solution until the color turns grass green, which is the end point. At the same time, perform a blank determination. 4.3.3 Calculation
The acidity X2 of the rice blast emulsifiable concentrate expressed in mass percentage is calculated according to formula (2): X,=-V:-V/)×0. 049,
wherein: c--actual concentration of sodium hydroxide standard titration solution, mol/L; V2--volume of sodium hydroxide standard titration solution consumed by titration sample, mL; V1--volume of sodium hydroxide standard titration solution consumed by titration blank, mL; m--sample weight of rice blast emulsifiable concentrate, g;
(2)
0.049--mass of sulfuric acid in grams equivalent to 1.00mL sodium hydroxide standard titration solution Cc(NaOH)=1.000mol/L).
4.4 Determination of emulsion stability
The determination is carried out according to GB1603, and the dilution factor is 200 times. 4.5 Low temperature stability
4.5.1 Apparatus
Ice water bath or constant temperature refrigerator: control the temperature to 0±1℃. 4.5.2 Operation steps
Weigh about 50g of sample into a 100mL beaker, put it in a refrigerator or ice water bath, maintain the temperature at 0±1℃, and leave it for 1h. During the placement period, stir once every 15min, and stir for 0.5min each time. Check whether there is solid or oily matter precipitated in the cup. If not, it is qualified. 4.6 Determination of thermal storage stability
4.6.1 Instrument
a. Constant temperature box or constant temperature water bath: temperature control accuracy is 54±2℃; b. An: capacity is about 50mL, long neck.
4.6.2 Determination
Use a medical syringe to absorb about 30mL of sample and inject it into a clean An Yan (do not let the sample touch the neck of the An Yan), place this An Yan in an ice salt bath, and seal it with a gas lamp (try to avoid solvent evaporation), and seal at least two bottles. Place the sealed container in a beaker and place it in a constant temperature incubator or water bath at 54±2℃ for 14 days. After taking out the container, all inspection items should be completed within 24 hours. The test results and various indicators should still meet the requirements of this standard.
5 Inspection rules
5.1 The quality supervision and inspection department of the manufacturer should inspect the blast-resistant emulsifiable concentrate. Low temperature stability and heat storage stability are random inspection items, which should be inspected at least once every three months. The manufacturer should ensure that all blast-resistant emulsifiable concentrates shipped out of the factory meet the requirements of this standard. Each batch of blast-resistant emulsifiable concentrate shipped out of the factory should be accompanied by a quality certificate.
5.2 The user has the right to verify the quality of the blast-resistant emulsifiable concentrate received in accordance with the provisions of this standard and check whether the various indicators meet the requirements of this standard.
5.3 The amount of each batch of blast-resistant emulsifiable concentrate should not exceed the capacity of the storage tank before packaging. 5.4 Sampling method: Take samples from 5% of the total number of each batch, and the small batch shall not be less than 3 pieces. Mix the samples evenly, take about 250g, and pack them into two clean, dry brown glass bottles with ground stoppers, seal them, and label them. Send one copy to the quality inspection department and keep one copy. 5.5 If some indicators in the test results do not meet the requirements of this standard, re-samples should be taken from twice the amount of packages for re-testing. Even if only one indicator is unqualified in the re-test results, the entire batch of rice blast emulsifiable concentrate is unqualified. 5.6 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation; or the statutory inspection agency can conduct arbitration analysis according to the methods specified in this standard.
6 Marking, packaging, transportation and purchase and storage
6.1 The marking and packaging of rice blast emulsifiable concentrate shall comply with the relevant provisions of GB4838. 6.2 During storage and transportation, it must be strictly protected from sunlight and well ventilated. It must not be mixed with food, seeds, and feed, and must avoid contact with the skin and inhalation through the mouth and nose.
6.3 The storage period of rice blast emulsifiable concentrate is 2 years. Within 2 years, the content, moisture, acidity, and emulsion stability still meet the index requirements. Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry. This standard is technically managed by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Zhao Xinxin and Wu Yanfeng. 5
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