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Professional Standard of the People's Republic of China
ZBG25016—90
Pyrroblastic acid technical
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
W Professional Standard of the People's Republic of China
Pyrroblastic acid technical
1 Subject content and scope of application
ZBG25016—90
This standard specifies the technical requirements, inspection methods, inspection rules, and packaging, marking, transportation and storage requirements of Pyrroblastic acid technical. This standard applies to Pyrroblastic acid technical.
Active ingredient: Pyrroblastic acid
Chemical name: 1,3-dithiolane-2-ylidenemalonic acid diisopropyl ester. Molecular formula: C12H18O,S2
Structural formula:
Relative molecular mass: 290.40 (1987 international atomic weight) Reference standards
GB1600
GB1605
GB3796
3 Technical requirements
Method for determining moisture content in pesticides
Method for sampling commercial pesticides
General rules for pesticide packaging
3.1 Appearance: Yellow to brownish yellow solid, without visible foreign impurities. 3.2 The original drug of rice blast should also meet the following index requirements: Index name
Superior grade
Rice blast content
Acidity (in H2SO)
Acetone insoluble matter1)
Note: 1) is a random inspection item.
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 11, 1990O-CH(CH3)2
O-CH(CH:)2
%(m/m)
First-class product
Qualified product
Implemented on January 1, 1991
W.bzsoso:com4 Inspection method
4.1 Determination of rice blasting agent content
4.1.1 Summary of method
ZBG25016—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
Rhizoctonia pyrochlore standard sample: known content, ≥99.0%, b.
n-Docosane: must not contain impurities that interfere with the chromatographic analysis, c.
Chloroform (GB682);
Stationary liquid: SE-30;bzxZ.net
Carrier: ChromosorbWAWDMCS, 180~250μm (60~80 mesh); e.
Internal standard solution: accurately weigh about 2.2g of n-docosane in a 1000mL volumetric flask, dissolve it with chloroform and dilute to the scale, shake well;
Standard sample solution: accurately weigh about 0.09g (accurate to 0.0002g) of the standard sample of Rhizoctonia pyrochlore, place it in a 25mL stoppered glass bottle, use a pipette to accurately add 20mL of the internal standard solution, shake well. 4.1.3 Instruments
&. 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/Chromosorb WAWDMCS (180~250μm) filler;
c. Recorder: 5mV (or data processor) d. Micro-injector 10μL.
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, stir with a glass rod to completely dissolve the stationary liquid. Add 7.0g of carrier, shake the beaker gently 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 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 column 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 (N2): 35mL/min
Hydrogen: 40mL/min;
Air: 300mL/min,
Sensitivity: 2X10-\,
Paper speed: 3mm/min,
Ww.bzsoso:comInjection volume: luL.
Retention time
Rice blasting agent is about 8.2min;
Internal standard is about 11.6min.
ZBG25016—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 the original drug of rice blasting
Rice blasting; 2-20
4.1.4.3 Preparation of sample solution
Weigh a sample of the original drug containing about 0.09g of rice blasting (accurate to 0.0002g), place it in a 25mL glass bottle with a cover, and 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 the standard solution of rice blasting until the peak height ratio of the 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 peak height ratios of a, d and bc, and calculate the mass percentage of isothiocyanate in the sample according to formula (1): X1: Xi--2·mi·p
Ti·m2
Wherein: Xi—the average value of the peak height ratios of isothiocyanate to the internal standard in the standard solution, T2—the average value of the peak height ratios of isothiocyanate to the internal standard in the sample solution; m
—the sample weight of isothiocyanate standard sample, g, (1)
W.m2—the sample weight of isothiocyanate sample, g;
ZBG25016-90
P—the percentage content of isothiocyanate standard sample, %. 4.1.5 Allowable difference
The difference between the results of the second determination should not exceed 1.5%. 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);
b. Sodium hydroxide (GB629) standard titration solution: 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 and shake the spoon. 4.3.2 Operation steps
Weigh 1~2g of sample (accurate to 0.001g) in a 250mL conical flask, add 60mL 95% ethanol and 10 drops of mixed indicator solution, and titrate with sodium hydroxide standard titration solution until grass green is the end point. Perform blank determination at the same time. 4.3.3 Calculate the acidity X2 of the original drug of rice blasticide expressed as a mass percentage according to formula (2): c(V2-V)X0.049
Wherein: c-the actual concentration of the standard sodium hydroxide titration solution, mol/L, V2-the volume of the standard sodium hydroxide titration solution consumed by the titration sample, mL, V.-the volume of the standard sodium hydroxide titration solution consumed by the titration blank, mL; m-
the original drug of rice blasticide The sample weight of the drug, g;
- The mass of sulfuric acid in grams equivalent to 1.00mL of sodium hydroxide standard titration solution (c(NaOH)=1.000mol/L) 0.049-
4.4 Determination of acetone insoluble matter
4.4.1 Instruments and reagents
Glass sand core crucible: G3
Suction filter bottle: 500mL,
c Acetone (GB686): chemically pure.
4.4.2 Determination steps
Wash and dry the G3 glass sand core crucible to constant weight (accurate to 0.0002g), and then put it on a 500mL suction filter bottle. Weigh about 10g of sample (accurate to 0.01g), put it into a conical flask, add 100mL acetone, shake the conical flask to dissolve all solubles, and then transfer all to a crucible, filter under vacuum, wash the crucible with 60mL acetone three times, and then filter for another 5 minutes. Dry the crucible and the filter residue at 110℃ to constant weight (accurate to 0.0002g). The mass percentage of acetone insoluble matter X3 is calculated according to formula (3): mz-ml×100.
Where: m1—mass of the sand core crucible after constant weight, g; m2
—total mass of the crucible and acetone insoluble matter after constant weight, g, m—sample weight, g.
（3）
W.5 Inspection rules
ZBG25016—90
5.1 The technical material of Pyrochlore should be inspected by the quality supervision and inspection department of the manufacturer. Acetone insoluble matter is a random inspection item, and random inspection should be carried out at least once a week. The manufacturer should ensure that all Pyrochlore technical materials shipped out of the factory meet the requirements of this standard. Each batch of Pyrochlore technical materials shipped out of the factory should be accompanied by a quality certificate.
5.2 The user unit has the right to verify the quality of the Pyrochlore technical materials received in accordance with the provisions of this standard and check whether the various indicators meet the requirements of this standard.
5.3 The quantity of each batch of Pyrochlore technical materials should not exceed the capacity of the storage tank before packaging. 5.4 The sampling method should be carried out in accordance with GB1605.
5.5 If any of the indicators in the test results do not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. Even if only one indicator in the re-test results is unqualified, the entire batch of rice blasting agent 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 storage
6.1 The packaging and marking should comply with the relevant provisions of GB3796. 6.2 The rice blasting agent should be packaged in clean, dry iron drums with a protective layer inside. The net weight of each drum should not exceed 200kg. Other forms of packaging can also be used according to user requirements.
6.3 During storage and transportation, it must be strictly protected from sunlight and maintained in good ventilation. It must not be mixed with food, seeds, and feed to avoid contact with the skin and prevent inhalation through the mouth and nose.
Additional instructions:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry. This standard is under the technical supervision of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by 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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