Some standard content:
ICS65.100
Registration No.: 10929-2002
Chemical Industry Standard of the People's Republic of China
HG3304--2002
Replaces HG3304--1990
Isoprothiolane Technical
Published on September 28, 2002
Isoprothiolane Technical ...
HG3304--2002
一 The classification of technical indicators has been cancelled. The mass fraction of rice blasting agent has been changed from ≥70.0% for qualified products to ≥90.0%, the water content has been changed from ≤0.5% to ≤0.2%, and the acetone insoluble matter has been changed from ≤0.2% to ≤0.1%.
The acceptance period has been increased.
一 The analytical conditions of the capillary gas chromatography method for the mass fraction of rice blasting agent have been supplemented and listed in the informative appendix. Appendix A of this standard is an informative appendix.
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. The participating drafting units of this standard are Sichuan Chemical Research and Design Institute, Hunan Tianyu Pesticide Chemical Group Co., Ltd., and Zhejiang Linghua Group Co., Ltd.
Drafters of this standard: Zhao Xinxin, Xing Hong, Ma Ling, Wu Quanhong, Ling Jinhe. This standard was first issued in April 1990.
This standard is the first revision.
This standard is entrusted to the Secretariat of the National Pesticide Standardization Technical Committee for interpretation. (53)
Pyrrochlore Technical
Other names, structural formulas and basic physicochemical parameters of the active ingredient Pyrrochlore in this product are as follows: ISO common name: Isoprothiolane
CIPAC digital code: 456
Chemical name, 1,3-dithiolane-2-ylidenemalonic acid diisopropyl ester Structural formula:
CH(CH）
Empirical formula: C2H1sO.S
Relative molecular mass: 290.4 (according to the 1997 International Relative Atomic Mass Standard (calculated) Biological activity: bactericidal
Melting point: 50℃~54.5℃
Boiling point 167℃~169℃/66.5Pa
Solubility (g/L, 20℃): 0.048 in water, easily soluble in organic solvents such as benzene, alcohol, acetone HG3304——2002
Stability: stable under normal storage conditions and in neutral and slightly acidic media; slowly decomposes in alkaline aqueous media 1 Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of the original drug of rice blast. This standard applies to the original drug of rice blast composed of rice blast and impurities generated in its production. 2 Normative references
The provisions in the following documents become the provisions 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/T1600 Determination of moisture content in pesticides
GB/T1604 Acceptance test for commercial pesticides
GB/T1605 Sampling method for commercial pesticides
GB3796 General rules for pesticide packaging
3 Requirements
3.1 Appearance: yellow body, no visible foreign impurities. 3.2 The control indicators of the technical material of rice blast should meet the requirements of Table 1. (55)
HG3304-2002
Mass fraction of rice cancer, %
Water content, %
Acidity (in terms of H, SO.) %
Mass fraction of acetone insoluble matter, %
Table 1 Control Items and Indicators of Rice Blasting Agent
aUnder normal production conditions, the mass fraction of acetone insoluble matter shall be inspected at least once every three months. 4 Test Methods
4.1 Sampling
The sampling shall be carried out in accordance with the method of "sampling of commercial technical materials" in GB/T1605. The sampling packages shall be determined by the random number table method, and the final sampling volume shall be not less than 100g.
4.2 Identification Test
Gas chromatography: This identification test can be carried out simultaneously with the determination of the mass fraction of rice blasting agent. 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 the rice cancer-resistant in the standard solution should be within 1.5%. Infrared spectroscopy: There should be no obvious difference between the infrared spectra of the sample and the standard in the wavenumber range of 4000cm-1~400cm-1 (see Figure 1.
4.3 Determination of the mass fraction of rice blast-resistant
4.3.1 Summary of the method
Figure 1 Infrared spectrum of rice blast-resistant standard
The sample is dissolved in chloroform, and n-docosane is used as the internal standard. A hydrogen flame ionization detector is used to separate and determine the gas on a 5% SE-30 column.
Capillary gas chromatography with a separation degree that meets the requirements can also be used for determination. For chromatographic operating conditions, see Appendix A. 4.3.2 Reagents and solutions
Chloroform.
Standard sample of rice blast-resistant: a known mass fraction greater than or equal to More than 99.0%. n-Dodecane: It must not contain impurities that may interfere with the chromatographic analysis. Stationary phase: SE-30.
Carrier: ChromosorbWAWDMCS, 180μm~250μm (or other carriers with equivalent performance). HG3304~2002
Internal standard solution: weigh about 2.4g of n-dodecane in a 1000ml volumetric flask, dissolve it with chloroform and dilute to the scale, and shake well. 4.3.3 Instruments
Gas chromatograph: hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1mX3mm(id) glass column (or stainless steel column). Column filling: 5%SE-30/ChromosorhWAWDMCS(18 0pμm~250μm), stationary liquid: (stationary liquid + carrier) = 5:100.
Microinjector: 10μL.
4.3.4 Preparation of chromatographic column
4.3.4.1 Coating of stationary liquid
Accurately weigh 0.38g of SE-30 stationary liquid into a 250mL beaker, add an appropriate amount (slightly larger than the volume of the carrier) of trinitroform to completely dissolve it, pour in 7g of the carrier, shake the beaker gently by hand to make the carrier completely immersed in the liquid, place the beaker under an infrared lamp to heat, shake the beaker while heating, until the solvent evaporates and is almost dry, then place it in a 120℃ oven to dry for 2h, take it out and place it in a desiccator for later use. 4.3.4.2 Filling of chromatographic column
Pick up a small bucket of washed and dried At the outlet of the dry chromatographic column, fill the prepared filler into the column in batches, and tap the column wall continuously until it is filled to 1.5 cm from the column outlet. Move the funnel to the inlet 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 filled evenly and tightly. After filling, also plug a small ball of glass wool at the inlet end and press it appropriately to prevent the column filler from moving. 4.3.4.3 Aging of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, do not connect the outlet end to the detector first, pass the carrier gas (N) at a flow rate of 20 mL/min, raise the temperature to 250°C in stages, and age at this temperature for at least 24 hours. 4.3.5 Gas chromatography operating conditions
Temperature (℃): Column chamber 195
Vaporization chamber 265
Detector chamber 265
Gas flow rate (mL/min): Carrier gas (N,) 35 Hydrogen 40
Air 300
Injection volume (μL): 1.0
Retention time (min): Blasticide 4.6; Internal standard (n-docosane) 6.8 The above operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of Blasticide technical is shown in Figure 2. (57)
HG3304-—2002
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
1—Solvent; 2-Rhizobactam, 3—Internal standard (n-docosane) Figure 2 Gas chromatogram of Rhizobactam original drug
Weigh about 0.1g of Rhizobactam standard sample (accurate to 0.0002g), place it in a stoppered glass bottle, use a pipette to accurately add 20mL of internal standard solution and shake.
4.3.6.2 Preparation of sample solution
Weigh about 0.1g of sample containing Rhizobactam (accurate to 0.0002g), place it in a stoppered glass bottle, use the same pipette as in 4.3.6.1 to accurately add 20mL of internal standard solution and shake. 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 when the relative response value of two adjacent needles changes less than 1.5%, perform determination 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 Jiewenling to the internal standard in the two needles of sample solution and the two needles of standard solution before and after the sample. The mass fraction w (%) of rice blast is calculated according to formula (1): u
Wherein:
The average value of the peak area ratio of rice blast to internal standard in the standard solution; the average value of the peak area ratio of rice blast to internal standard in the sample solution: (58)
m——the mass of the rice blast standard, in grams (g); m—the mass of the sample, in grams (g); P-the mass fraction of rice blast in the standard, expressed in %. HG3304--2002
It is also possible to calculate the correction factor first and then calculate the effective body mass fraction in the sample according to the provisions of GB/T4946 "Terms of Gas Chromatography".
4.3.8 Allowable Difference
The difference between two parallel determination results should not exceed 1.5%. 4.4 Determination of Water
Determine according to the Karl Fischer method in GB/T1600. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution: c(NaOH)=0.02mol/L. 95% ethanol. bzxZ.net
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. 4.5.2 Determination steps
Weigh 1.5g of the sample (accurate to 0.0002g), place it in 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 grass green color is the end point. Perform a blank determination at the same time. The acidity wz (%) of the sample expressed as the mass fraction of sulfuric acid (H2SO4) is calculated according to formula (2): c(V2-V2)X0.049
Wherein:
-actual concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L); V2-volume of sodium hydroxide standard titration solution consumed by titrating the sample solution, in milliliters (mL); V2-volume of sodium hydroxide standard titration solution consumed by titrating the blank solution, in milliliters (mL); m mass of the sample, in grams (g); (2)
0.049-mass of sulfuric acid in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L].
4.5.3 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed ±25%. The arithmetic mean shall be taken as the determination result. 4.6 Determination of the mass fraction of acetone insoluble matter
4.6.1 Reagents
Acetone.
4.6.2 Apparatus
Erlenmeyer flask: 250mL.
Glass sand core: G3.
Suction filter flask: 500mL.
Oven: 110℃±2℃.
4.6.3 Determination steps
Weigh 10g of the sample (accurate to 0.01g), place it in a 250mL Erlenmeyer flask, add 100mL of acetone, and shake until all soluble matter is dissolved. Use the filtered solution that has reached a constant weight, and then wash the crucible with 60mL of acetone three times, and filter it by suction. Place the crucible in an oven to dry for 30min, take it out, cool it to room temperature, and weigh it.
The mass fraction of acetone insoluble matter in the sample, ws (%), is calculated according to formula (3): m-mo
HG3304~2002
Wherein:
ml~-The mass of the crucible and the insoluble matter after constant weight, in grams
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