Some standard content:
ICS65.100
Registration No.: 10933-2002
Chemical Industry Standard of the People's Republic of China
HG3285—2002
Replaces HG3285-1981
Iprobenfos Technical
Published on September 28, 2002
Iprobenfos Technical
Iprobenfos Technical
Issued on September 28, 2002
Implemented on June 1, 2003
Before publication by the State Economic and Trade Commission of the People's Republic of China
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. This standard replaces the mandatory industry standard HG3285-1981 "Iprobenfos Technical". The main difference between this standard and HG32851981 is: the foreword is added.
The mass fraction of Iprobenfos is changed from greater than or equal to 80.0% to greater than or equal to 90.0%. The moisture index was changed from less than or equal to 0.5% to less than or equal to 0.4%. - The acid content control index and inspection method were added. - The acceptance period was increased.
This standard was proposed by the Policy and Regulations Department of the former State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of the National Pesticide Standardization Technical Committee (CSBTS/TC133). The responsible drafting unit of this standard is Shenyang Chemical Research Institute, and the participating drafting units of this standard are Shanghai Pesticide Factory and Zhejiang Jiahua Industrial Co., Ltd. The main drafters of this standard are Gao Xiaohui, Jiu Yankun, Deng Changhua, and Fu Fengju. This standard was first issued in 1981. This is the first revision. The Secretariat of the National Pesticide Standardization Technical Committee is entrusted with the interpretation of this standard. (13)
HG3285--2002
Iprobenfos technical
Other names, structural formulas and basic physicochemical parameters of the active ingredient Iprobenfos in this product are as follows: ISO common name: Iprobenfos
CIPAC digital code: 393
Chemical name: 00 diisopropyl-S-conothioic acid phosphorothioate Structural formula:
（CH,）2CHO
PSCH2-
（CHa).CHO
Empirical formula: CHzO.PS
Relative molecular mass: 288.3 (according to the 1997 International Standard for Relative Molecular Weight) =Atomic mass) Biological activity: Bactericidal
Boiling point: 126℃/5.332Pa
Vapor pressure (20℃): 0.247mPa
Relative density (20℃): 1.103
HG3285-2002
Solubility (20℃): 430mg/L in water, soluble in acetone, alcohols, benzene, hexane, chloroform and other organic solvents Stability: Decomposed by alkali, DTso (in water, pH4~9) is 7230h~7793h1 Range
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of Isoblast. This standard applies to Isoblast technical composed of Isoblast and impurities generated in its production. 2 Normative referencesbzxZ.net
The clauses in the following documents become the clauses of this standard through reference in this standard. For any dated referenced document, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties reaching an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any undated referenced document, the latest version shall apply to this standard. GB/T601 Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB/T1600 Method for determination of moisture content in pesticides
GB/T1604 Acceptance rules for commercial pesticides
GB/T1605 Sampling method for commercial pesticides
GB3796 General rules for pesticide packaging
3 Requirements
3.1 Appearance: It should be a light yellow oily liquid. At low temperatures, there will be precipitation of precipitates. 3.2 The control indicators of the technical material of Ipropathorium should meet the requirements of Table 1. (15)
HG3285—2002
Mass fraction of Isoblast, %
Water, %
Acidity (in H,SO.), %
Test method
4.1 Sampling
Control index of Isoblast technical
Carry out in accordance with the "liquid preparation sampling" method in GB/T1605. The sampling package is determined by the random number table method, and the final sampling volume should be not less than 200mL.
4.2 Identification test
4.2.1 Gas chromatography: This identification test can be carried out simultaneously with the determination of the mass fraction of Isoblast. 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 Isoblast in the standard solution should be within 1.5%.
4.2.2 Infrared spectroscopy: There should be no obvious difference between the infrared spectra of the active ingredients separated from the sample and the standard sample in the wave number range of 4000cm-1 to 800cm-1. The infrared standard spectrum of the standard sample of Yiwenjing is shown in Figure 1.60
4.3 Determination of the mass fraction of Yiwenjing
4.3.1 Summary of the method
Figure 1 Infrared spectrum of Yiwenjing
The sample is dissolved in acetone, and dibutyl phthalate or diallyl phthalate is used as the internal standard. A glass column or stainless steel column filled with 5%SE-30/Chro-mosorbWAWDMCS (180um~250μm) and a hydrogen flame ionization detector are used to separate and determine the Yiwenjing in the sample by gas chromatography. 4.3.2 Reagents and solutions
Acetone.
Non-standard sample of rice blast: known mass fraction greater than or equal to 99.0%. 2
Internal standard: dibutyl phthalate or diallyl phthalate, should be free of impurities that interfere with analysis. Stationary liquid: SE-30.
Carrier: ChromosorbWAWDMCS (180μm~250μm). HG32852002
Internal standard solution: weigh 2.0g of dibutyl phthalate or diallyl phthalate, place in a 100mL volumetric flask, add appropriate amount of acetone to dissolve, dilute to scale, and shake well. 4.3.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1.0m×3.2mm(id) glass column or stainless steel column. Column filling: SE-30 is coated on ChromosorbWAWDMCS (180μm~250μm), stationary liquid: (stationary liquid + ten carriers) = 5:100.
4.3.4 Preparation of chromatographic columns
4.3.4.1 Coating of stationary liquid
Accurately weigh 0.5g of SE-30 stationary liquid into a 250mL beaker, add an appropriate amount (slightly larger than the volume of the carrier) of chloroform to completely dissolve it, pour in 9.5g of the carrier, shake gently to mix evenly and evaporate the solvent to near dryness, then put the beaker in a 120℃ oven to dry for 1h, take it out and cool it in a desiccator to room temperature. 4.3.4.2 Filling of chromatographic columns
Connect a small funnel to the outlet of the washed and dried chromatographic column, and fill the prepared filling into the column in batches, while constantly tapping the column wall until it is filled to 1.5cm from the column outlet. Move the funnel to the entrance of the chromatographic column, plug a small ball of silanized glass wool at the outlet, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, continue to slowly add the filler, and tap the column wall continuously to make it evenly and tightly filled. After filling, plug a small ball of glass wool at the entrance and press it properly to prevent the column filler from moving. 4.3.4.3 Aging of the chromatographic column
Connect the entrance of the chromatographic column to the vaporization chamber, do not connect the outlet to the detector for the time being, pass the carrier gas (Nz) at a flow rate of 15mL/min, raise the temperature to 260℃ in stages, and age at this temperature for 48h. 4.3.5 Gas chromatography operating conditions
Temperature (℃): Column temperature 155
Vaporization chamber 200
Detector chamber 200
Gas flow rate (mL/min): Carrier gas (Nz) 30 Hydrogen 40
Air 400
Injection volume (μL): 0.4
Retention time (min): Isoblastine 5.7. Internal standard 9.5 The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The typical gas chromatogram of Isoblastine technical is shown in Figure 2. (17)
HG3285--2002
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
1 Solvent: 2-isocyanate + 3-dibutyl phthalate Figure 2 Gas chromatogram of isoflavone technical
Weigh 0.1 g of isoflavone standard sample (accurate to 0.0002g), place it in a stoppered glass bottle, use a pipette to accurately add 5mL of internal standard solution and shake well.
4.3.6.2 Preparation of sample solution
Weigh about 0.1g of sample containing Irvine Blast Net (accurate to 0.0002g), place it in a stoppered glass bottle, use the same pipette used in 4.3.6.1 to accurately add 5mL of internal standard solution and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the relative response value of each needle, and wait until the relative response value of Irvine Blast Net of two adjacent needles changes less than 1.5%. Determination is carried out in the order of standard solution, sample solution, sample solution, and standard solution.
4.3.7 Calculation
Average the ratio of the peak area of Isoblast to the internal standard in the two sample solutions and the two standard solutions before and after the sample.
The mass fraction of Isoblast in the sample (%) is calculated according to formula (1): rmP
Where:
——the average value of the peak area ratio of Isoblast to the internal standard in the standard solution; the average value of the peak area ratio of Isoblast to the internal standard in the sample solution; r2
ml——the mass of the Isoblast standard sample, in grams (g); the mass of the sample, in grams (g);
P——the mass fraction of Isoblast in the standard sample, expressed in %. 4.3.8 Allowable difference
The difference between the results of two parallel determinations should not be greater than 1.0%. Take the arithmetic mean as the determination result. 4.4 Determination of moisture
HG3285-2002
Carry out according to the "Karl Fischer method" in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Ethanol: 50% aqueous solution by volume.
Standard sodium hydroxide titration solution c(NaOH) = 0.02mol/L; prepared according to GB/T601. Methyl red indicator solution: 2g/L ethanol solution. 4.5.2 Determination steps
Weigh 1g of sample (accurate to 0.0002 g), placed in a 250mL conical flask, add 30mL of ethanol solution, and shake to dissolve the sample. Add 3 drops of indicator solution and titrate with 0.02mol/L sodium hydroxide standard titration solution until orange-yellow is the end point. Perform a blank determination at the same time.
The acidity w (%) of the sample expressed as the mass fraction of sulfuric acid (H.SO,) is calculated according to formula (2): c(V/-V.)×0.049
Where:
The actual concentration of the sodium hydroxide standard titration solution, in moles per liter (mol/L); V,——the consumption of the sodium hydroxide standard titration solution in titrating the sample solution The volume of the standard titration solution of sodium hydroxide is expressed in milliliters (mL); V. — The volume of the standard titration solution of sodium hydroxide consumed in the titration blank is expressed in milliliters (mL); m — The mass of the sample is expressed in grams (g);
0.049 — The mass of sulfuric acid in grams equivalent to 1.00mL of the standard titration solution of sodium hydroxide [c(NaOH)=1.000mol/L].
4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. 5 Marking, labeling, packaging, storage and transportation
5. 1 The marking, labeling and packaging of Isoblast technical shall comply with the provisions of GB3796. 5.2 Isoblast technical shall be packaged in clean steel drums with inner protective layer, with net content of 200kg per drum; or in plastic drums, with net content of 50kg per drum.
5.3 Other forms of packaging may be used according to user requirements or ordering agreement, but they must comply with the provisions of GB3796. 5.4 Packages shall be stored in ventilated and dry warehouses. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin and eyes, and prevent inhalation through mouth and nose.
HG 3285—2002
5.6 Safety: Isoblast is a low-toxic fungicide. Protective gloves should be worn when using this product. Spray in the direction of the wind to prevent inhalation from the mouth and nose: After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. In case of poisoning, please consult a doctor in time. 5.7 Acceptance period: The acceptance period of Isoblast technical is one month. From the date of delivery, the product quality acceptance should be completed within one month, and all indicators should meet the standard requirements.7 Acceptance period: The acceptance period for Isopropanol technical is one month. From the date of delivery, the product quality acceptance shall be completed within one month, and all indicators shall meet the standard requirements.7 Acceptance period: The acceptance period for Isopropanol technical is one month. From the date of delivery, the product quality acceptance shall be completed within one month, and all indicators shall meet the standard requirements.
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