Some standard content:
ICS65.100
Registration No.: 10934-2002
Chemical Industry Standard of the People's Republic of China
HG3286-2002
Replaces HG3286-1981
Iprobenfos Emulsifiable Concentrates2002-09-28 Issued
Implemented on 2003-06-01
Issued 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 chemical industry standard HG3286-1981 "Iprobenfos Emulsifiable Concentrate". The main differences between this standard and HG3286-1981 are: 1. The foreword is added.
HG3286--2002
- The concentration of the sodium hydroxide standard solution used in the acidity analysis method was changed from 0.1N to 0.02mol/L. - The water content was changed from less than or equal to 0.5% to less than or equal to 0.4%. - The dilution multiple of emulsion stability was changed from 500 times to 200 times. - The low temperature stability index was added.
- The heat storage stability index was added.
- The warranty period was added. The warranty period of Isoblastine EC is two years from the date of production. During the warranty period, the mass fraction of Isoblastine in 40% and 50% Isoblastine EC should not be less than 39.0% and 48.5%, and other indicators meet the standard requirements. 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: Shenyang Chemical Research Institute. The drafting organizations of this standard are Shanghai Pesticide Factory and Zhejiang Jiahua Industrial Co., Ltd. The main drafters of this standard are Gao Xiaohui, Zhi Yankun, Deng Changhua and Fu Fengju. This standard was first issued in 1981.
This standard is entrusted to the Secretariat of the National Technical Committee for Pesticide Standardization for interpretation. (23)
Iprobenfos EC
Other names, structural formulas and basic physicochemical parameters of Iprobenfos, the active ingredient of this product, are as follows: ISO common name: Iprobenfos
CIPAC digital code: 393
Chemical name: O,O diisopropyl-S-sinyl thiophosphate Structural formula:
(CHa)2CHO
(CH,)2CHO
Empirical formula: CHaO,PS
Relative molecular mass: 288.3 (according to the 1997 International Standard for Relative Atomic Mass (dosage meter) Biological activity: bactericidal
Boiling point: 126℃/5.332Pa
Vapor pressure (20℃): 0.247mPa
Relative density (20℃): 1.103
Solubility (20℃): 430mg/L in water; soluble in acetone, alcohols, benzene, hexane, acetone and other organic solventsStability: decomposed by alkali, DT5 (in water, pH4~9) is 7230h~7793h1Range
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of Isoblasting Emulsion. HG3286—2002
This standard applies to Isoblasting Emulsion prepared by dissolving Isoblasting technical drug and emulsifier that meet the standards in a suitable solvent. 2 Normative references
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 Determination of moisture content in pesticides
GB/T1603 Determination of stability of pesticide emulsions GB/T 1604
Acceptance rules for commercial pesticides
Sampling methods for commercial pesticides
GB/T1605
GB4838 Packaging of pesticide emulsions
3 Requirements
3.1 Appearance: It should be a stable homogeneous liquid without visible suspended matter and precipitation. 3.2 The control indicators of Isopropylamine emulsion should meet the requirements of Table 1. (25)
HG3286—2002
Mass fraction of Isoblast, %
Water, %
Acidity (in H2SO4), %
Emulsion stability (dilution 200 times)
Low temperature stability
Hot storage stability
Table 1 Control item index of Isoblast emulsifiable concentrate
50% emulsifiable concentrate
Low temperature stability and hot storage stability test Under normal production conditions, the test shall be conducted at least once every three months. 4
Test method
4.1 Sampling
40% emulsifiable concentrate
The test shall be conducted in accordance with the "Sampling of liquid preparations" method 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 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: Isoblast is separated from the interfering components by thin layer chromatography [silica gel, developing solvent, hexane/acetone (75+25), Rf=0.04~0.05, and there should be no obvious difference in the infrared spectrum of the effective component separated from the sample and the standard sample in the wave number range of 4000cm-1~800cm-1. The infrared standard spectrum of the standard sample of Isoblast is shown in Figure 1.60
4.3 Determination of the mass fraction of Isoblast
4.3.1 Method summary
Figure 1 Infrared spectrum of the standard sample of Isoblast
HG3286-2002
The sample is dissolved in acetone, dibutyl phthalate or diallyl phthalate is used as the internal standard, and a glass column or stainless steel column filled with 5% SE-30/Chro-mosorbWAWDMCS (180μm~250μm) and a hydrogen flame ionization detector are used to perform gas chromatography separation and determination of Isoblast in the sample. 4.3.2 Reagents and solutions
Acetone.
Standard sample of Isoblast: known mass fraction is greater than or equal to 99.0%. Internal standard: dibutyl phthalate or diallyl phthalate, which should be free of impurities that interfere with the analysis. Stationary liquid: SE-30.
Carrier: ChromosorbWAwDMCS (180μm25oμm). Internal standard solution: weigh 2.0g of dibutyl phthalate or diallyl phthalate, place it in a 100mL volumetric flask, add appropriate amount of acetone to dissolve, dilute to the scale, and shake well. 4.3.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1.0mX3.2mm(id) glass column or stainless steel column. Column filling: SE-30 coated on ChromosorbWAwDMCS (180μm~250μm), stationary liquid: (stationary liquid + carrier) = 5:100.
4.3.4 Preparation of chromatographic column
4.3.4.1 Coating of stationary liquid
Accurately weigh 0.5g 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 to room temperature in a desiccator. 4.3.4.2 Filling of chromatographic column
Connect a small funnel to the outlet of the washed and dried chromatographic column, fill the prepared filler into the column in batches, and tap the column wall continuously until it is filled to 1.5cm 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 constantly tap the column wall to make it evenly and tightly filled. After filling, plug a small ball of glass wool at the inlet and press it appropriately to prevent the column filler from moving. 4.3.4.3 Aging of the chromatographic columnwww.bzxz.net
Connect the inlet end of the chromatographic column to the vaporization chamber, do not connect the outlet end 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 (N2) 30 Hydrogen 40
Air 400
Injection volume (pL): 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. A typical gas chromatogram of Isoblastine emulsifiable concentrate is shown in Figure 2. (27)
HG3286—2002
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
1 Solvent; 2-Isocarb 3-dibutyl phthalate Figure 2 Gas chromatogram of Isocarb emulsion
Weigh 0.1 g of Isocarb standard sample (accurate to 0.0002 g), place it in a stoppered glass bottle, add 5 mL of internal standard solution accurately with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh about 0.1 g of sample containing Isocarb (accurate to 0.0002 g), place it in a stoppered glass bottle, add 5 mL of internal standard solution accurately with the same pipette used in 4.3.6.1, and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several injections of standard solution, calculate the repeatability of the relative response value of each injection, and when the relative response value of two adjacent injections of Izaobojing changes less than 1.5%, perform the 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 Izaobojing to the internal standard in the two injections of sample solution and the two injections of standard solution before and after the sample.
The mass fraction of Isoblast in the sample, wi (%), is calculated according to formula (1): rmp
Wherein:
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; the mass of the standard, 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 shall not exceed 1.0%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of moisture
HG3286-2002
It shall be carried out according to the "Karl Fischer" method in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy for determination. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Ethanol: 50% aqueous solution by volume.
Sodium hydroxide standard 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 the sample (accurate to 0.002g), place it 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 the end point is orange-yellow. Perform a blank determination at the same time.
The acidity of the sample expressed as the mass fraction of sulfuric acid (H2SO4) e2 (%) is calculated according to formula (2): c(V4-V.)X0.049
Wherein:
The actual concentration of the sodium hydroxide standard titration solution, in moles per liter (mol/L); V—the volume of the sodium hydroxide standard titration solution consumed by titrating the sample solution, in milliliters (mL); V. —the volume of the sodium hydroxide standard titration solution consumed by titrating the blank, in milliliters (mL); m
The mass of the sample, in grams (g);
The mass of sulfuric acid equivalent to 1.00mL of the sodium hydroxide standard titration solution [c (NaOH) = 1.000mol/L] expressed in grams.
4.6 Emulsion stability test
Performed in accordance with GB/T1603. The test results show that the sample is qualified if there is no floating oil on the top, no sinking oil on the bottom, and no precipitation. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃ for 1 hour, and the presence of solid and oily matter is recorded. It is then stored at 0℃ for 7 days. The solid precipitate is centrifuged to settle, and its volume is recorded.
4.7.2 Apparatus
Refrigerator: maintained at 0℃±2℃.
Centrifuge tube: 100mL, with scale on the bottom of the tube accurate to 0.05mL. Centrifuge: Matching the centrifuge tube.
4.7.3 Test steps
HG3286—2002
Take 100mL±1.0mL of the sample and add it to the centrifuge tube. Cool it to 0℃±2℃ in the refrigerator. Keep the centrifuge tube and its contents at 0℃±2℃ for 1 hour. Stir it every 15min for 15s each time. Check and record the presence of solid or oily matter. Put the centrifuge tube back into the refrigerator and continue to place it at 0℃±2℃ for 7 days. Then take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge it for 15 minutes (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accuracy 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Thermal storage stability test
4.8.1 Instrument
Thermostatic box (or constant temperature water bath): 54℃±2℃. Ampoule (or stoppered bottle that can still be sealed at 54℃): 50mL. Medical syringe 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of the emulsifiable concentrate sample into a clean bottle (or glass bottle) (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath until it cools, and quickly seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed bottle in a metal container, and then place the metal container in a 54℃±2℃ constant temperature box (or water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle clean and weigh it separately. For samples that have not changed in mass, test the mass fraction of Isoblast and emulsion stability within 24 hours. The content of Isoblast after emulsifiable concentrate should not be less than 95% of the content measured before storage, and the emulsion stability should meet the standard requirements. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method is used for the processing of limit values. 5.1 The marking, labeling and packaging of Isocarb-free EC shall comply with the provisions of GB4838. 5.2 Isocarb-free EC shall be packaged in brown glass bottles with stoppers and caps, with a net content of 500g, 1000g, etc.; the outer packaging shall be in calcium plastic boxes or corrugated paper boxes, with a net content of no more than 15kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB4838. 5.4 The packages shall be stored in a ventilated and dry warehouse. 5.5 During storage and transportation, it shall be strictly prevented from moisture and sunlight, and shall not be mixed with food, seeds, and feed, and shall avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Isocarb-free EC is a low-toxic fungicide. Protective gloves should be worn when using this product. Spray in the direction of the wind to prevent inhalation through 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 immediately. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Isoblastine EC is two years from the date of production. All indicators should meet the standard requirements when leaving the factory. During the warranty period, the mass fraction of Isoblastine in 40% and 50% Isoblastine EC should not be less than 39.0% and 48.5%, and other indicators should meet the standard requirements. (30)0002g), place it in a stoppered glass bottle, accurately add 5mL of internal standard solution with a pipette, 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, accurately add 5mL of internal standard solution with the same pipette used in 4.3.6.1, 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 when the relative response value of Irvine Blast Net 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 Isofenac to the internal standard in the two sample solutions and the two standard solutions before and after the sample.
The mass fraction of Isofenac in the sample, wi (%), is calculated according to formula (1): rmp
Wherein:
The average value of the peak area ratio of Isofenac to the internal standard in the standard solution; the average value of the peak area ratio of Isofenac to the internal standard in the sample solution; the mass of the standard sample, in grams (g);
The mass of the sample, in grams (g);
P—the mass fraction of Isofenac in the standard sample, expressed in %. 4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. Take their arithmetic mean as the determination result. 4.4 Determination of moisture
HG3286-2002
Carry out according to the "Karl Fischer" method in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy for determination. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Ethanol: 50% aqueous solution by volume.
Sodium hydroxide standard 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 the sample (accurate to 0.002g), place it 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 the end point is orange-yellow. Perform a blank determination at the same time.
The acidity of the sample expressed as the mass fraction of sulfuric acid (H2SO4) e2 (%) is calculated according to formula (2): c(V4-V.)X0.049
Wherein:
The actual concentration of the sodium hydroxide standard titration solution, in moles per liter (mol/L); V—the volume of the sodium hydroxide standard titration solution consumed by titrating the sample solution, in milliliters (mL); V. —the volume of the sodium hydroxide standard titration solution consumed by titrating the blank, in milliliters (mL); m
The mass of the sample, in grams (g);
The mass of sulfuric acid equivalent to 1.00mL of the sodium hydroxide standard titration solution [c (NaOH) = 1.000mol/L] expressed in grams.
4.6 Emulsion stability test
Performed in accordance with GB/T1603. The test results show that the sample is qualified if there is no floating oil on the top, no sinking oil on the bottom, and no precipitation. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃ for 1 hour, and the presence of solid and oily matter is recorded. It is then stored at 0℃ for 7 days. The solid precipitate is centrifuged to settle, and its volume is recorded.
4.7.2 Apparatus
Refrigerator: maintained at 0℃±2℃.
Centrifuge tube: 100mL, with scale on the bottom of the tube accurate to 0.05mL. Centrifuge: Matching the centrifuge tube.
4.7.3 Test steps
HG3286—2002
Take 100mL±1.0mL of the sample and add it to the centrifuge tube. Cool it to 0℃±2℃ in the refrigerator. Keep the centrifuge tube and its contents at 0℃±2℃ for 1 hour. Stir it every 15min for 15s each time. Check and record the presence of solid or oily matter. Put the centrifuge tube back into the refrigerator and continue to place it at 0℃±2℃ for 7 days. Then take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge it for 15 minutes (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accuracy 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Thermal storage stability test
4.8.1 Instrument
Thermostatic box (or constant temperature water bath): 54℃±2℃. Ampoule (or stoppered bottle that can still be sealed at 54℃): 50mL. Medical syringe 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of the emulsifiable concentrate sample into a clean bottle (or glass bottle) (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath until it cools, and quickly seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed bottle in a metal container, and then place the metal container in a 54℃±2℃ constant temperature box (or water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle clean and weigh it separately. For samples that have not changed in mass, test the mass fraction of Isoblast and emulsion stability within 24 hours. The content of Isoblast after emulsifiable concentrate should not be less than 95% of the content measured before storage, and the emulsion stability should meet the standard requirements. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method is used for the processing of limit values. 5.1 The marking, labeling and packaging of Isocarb-free EC shall comply with the provisions of GB4838. 5.2 Isocarb-free EC shall be packaged in brown glass bottles with stoppers and caps, with a net content of 500g, 1000g, etc.; the outer packaging shall be in calcium plastic boxes or corrugated paper boxes, with a net content of no more than 15kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB4838. 5.4 The packages shall be stored in a ventilated and dry warehouse. 5.5 During storage and transportation, it shall be strictly prevented from moisture and sunlight, and shall not be mixed with food, seeds, and feed, and shall avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Isocarb-free EC is a low-toxic fungicide. Protective gloves should be worn when using this product. Spray in the direction of the wind to prevent inhalation through 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 immediately. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Isoblastine EC is two years from the date of production. All indicators should meet the standard requirements when leaving the factory. During the warranty period, the mass fraction of Isoblastine in 40% and 50% Isoblastine EC should not be less than 39.0% and 48.5%, and other indicators should meet the standard requirements. (30)0002g), place it in a stoppered glass bottle, accurately add 5mL of internal standard solution with a pipette, 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, accurately add 5mL of internal standard solution with the same pipette used in 4.3.6.1, 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 when the relative response value of Irvine Blast Net between 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 Isofenac to the internal standard in the two sample solutions and the two standard solutions before and after the sample.
The mass fraction of Isofenac in the sample, wi (%), is calculated according to formula (1): rmp
Wherein:
The average value of the peak area ratio of Isofenac to the internal standard in the standard solution; the average value of the peak area ratio of Isofenac to the internal standard in the sample solution; the mass of the standard sample, in grams (g);
The mass of the sample, in grams (g);
P—the mass fraction of Isofenac in the standard sample, expressed in %. 4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. Take their arithmetic mean as the determination result. 4.4 Determination of moisture
HG3286-2002
Carry out according to the "Karl Fischer" method in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy for determination. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Ethanol: 50% aqueous solution by volume.
Sodium hydroxide standard 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 the sample (accurate to 0.002g), place it 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 it turns orange-yellow, which is the end point. Perform a blank determination at the same time.
The acidity of the sample expressed as the mass fraction of sulfuric acid (H2SO4) e2 (%) is calculated according to formula (2): c(V4-V.)X0.049
Wherein:
The actual concentration of the sodium hydroxide standard titration solution, in moles per liter (mol/L); V—the volume of the sodium hydroxide standard titration solution consumed by titrating the sample solution, in milliliters (mL); V. —the volume of the sodium hydroxide standard titration solution consumed by titrating the blank, in milliliters (mL); m
The mass of the sample, in grams (g);
The mass of sulfuric acid equivalent to 1.00mL of the sodium hydroxide standard titration solution [c (NaOH) = 1.000mol/L] expressed in grams.
4.6 Emulsion stability test
Performed in accordance with GB/T1603. The test results show that the sample is qualified if there is no floating oil on the top, no sinking oil on the bottom, and no precipitation. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃ for 1 hour, and the presence of solid and oily matter is recorded. It is then stored at 0℃ for 7 days. The solid precipitate is centrifuged to settle, and its volume is recorded.
4.7.2 Apparatus
Refrigerator: maintained at 0℃±2℃.
Centrifuge tube: 100mL, with scale on the bottom of the tube accurate to 0.05mL. Centrifuge: Matching the centrifuge tube.
4.7.3 Test steps
HG3286—2002
Take 100mL±1.0mL of the sample and add it to the centrifuge tube. Cool it to 0℃±2℃ in the refrigerator. Keep the centrifuge tube and its contents at 0℃±2℃ for 1 hour. Stir it every 15min for 15s each time. Check and record the presence of solid or oily matter. Put the centrifuge tube back into the refrigerator and continue to place it at 0℃±2℃ for 7 days. Then take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge it for 15 minutes (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accuracy 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Thermal storage stability test
4.8.1 Instrument
Thermostatic box (or constant temperature water bath): 54℃±2℃. Ampoule (or stoppered bottle that can still be sealed at 54℃): 50mL. Medical syringe 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of the emulsifiable concentrate sample into a clean bottle (or glass bottle) (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath until it cools, and quickly seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed bottle in a metal container, and then place the metal container in a 54℃±2℃ constant temperature box (or water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle clean and weigh it separately. For samples that have not changed in mass, test the mass fraction of Isoblast and emulsion stability within 24 hours. The content of Isoblast after emulsifiable concentrate should not be less than 95% of the content measured before storage, and the emulsion stability should meet the standard requirements. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method is used for the processing of limit values. 5.1 The marking, labeling and packaging of Isocarb-free EC shall comply with the provisions of GB4838. 5.2 Isocarb-free EC shall be packaged in brown glass bottles with stoppers and caps, with a net content of 500g, 1000g, etc.; the outer packaging shall be in calcium plastic boxes or corrugated paper boxes, with a net content of no more than 15kg per box. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB4838. 5.4 The packages shall be stored in a ventilated and dry warehouse. 5.5 During storage and transportation, it shall be strictly prevented from moisture and sunlight, and shall not be mixed with food, seeds, and feed, and shall avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Isocarb-free EC is a low-toxic fungicide. Protective gloves should be worn when using this product. Spraying should be done in the direction of the wind to prevent inhalation through 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 immediately. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Isoblastine EC is two years from the date of production. All indicators should meet the standard requirements when leaving the factory. During the warranty period, the mass fraction of Isoblastine in 40% and 50% Isoblastine EC should not be less than 39.0% and 48.5%, and other indicators should meet the standard requirements. (30)2 Determination steps
Weigh 1g of the sample (accurate to 0.002g), place it 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 it turns orange-yellow, which is the end point. Perform a blank determination at the same time.
The acidity e2 (%) of the sample expressed as the mass fraction of sulfuric acid (H2SO4) is calculated according to formula (2): c(V4-V4)X0.049
Where:
The actual concentration of the sodium hydroxide standard titration solution, in moles per liter (mol/L); V—the volume of the sodium hydroxide standard titration solution consumed in titrating the sample solution, in milliliters (mL); V.一Titrate blank, the volume of sodium hydroxide standard titration solution consumed, in milliliters (mL); m
Sample mass, in grams (g);
The mass of sulfuric acid in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c (NaOH) = 1.000mol/L.
4.6 Emulsion stability test
Carry out in accordance with GB/T1603. Test results, no floating oil on the top, no sinking oil and precipitation below are qualified. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃ for 1h, and the presence of solid and oily precipitation is recorded. Continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instrument
Refrigerator: maintain 0℃±2℃.
Centrifuge tube: 100mL, with scale on the bottom of the tube accurate to 0.05mL. Centrifuge: Matching with centrifuge tube.
4.7.3 Test steps
HG3286—2002
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0℃±2℃ in the refrigerator, keep the centrifuge tube and its contents at 0℃±2℃ for 1h, stir it every 15min, and each time for 15s, check and record whether there is solid or oily precipitation. Put the centrifuge tube back into the refrigerator and continue to place it at 0℃±2℃ for 7d, then take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge it for 15min (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Thermal storage stability test
4.8.1 Apparatus
Thermostatic box (or thermostatic water bath): 54℃±2℃. Ampoule (or bottle with a stopper that can still be sealed at 54℃): 50mL. Medical syringe 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of the emulsifiable concentrate sample into a clean ampoule (or glass bottle) (avoid the sample from contacting the bottleneck), place the ampoule in an ice-salt bath until it is cooled, and quickly seal it with a high-temperature flame (to avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed ones in a metal container, and then place the metal container in a thermostatic box (or water bath) at 54℃±2℃ for 14 days. Take out and cool to room temperature, wipe the outside of the container and weigh them separately. For samples with unchanged mass, test the mass fraction of Isoblast and emulsion stability within 24 hours. The content of Isoblast emulsion after storage should not be less than 95% of the content measured before storage, and the emulsion stability should meet the standard requirements. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of Isoblast emulsion shall comply with the provisions of GB4838. 5.2 Isoblast emulsion shall be packaged in brown glass bottles with stoppers and caps, with a net content of 500g, 1000g, etc.; the outer packaging shall be calcium plastic boxes or corrugated boxes, and the net content of each box shall not exceed 15kg. 5.3 According to user requirements or ordering agreements, other forms of packaging may be used, but they must comply with the provisions of GB4838. 5.4 Packages should be stored in ventilated, dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Isocarb is a low-toxic fungicide. Wear protective gloves when using this product. Spray in the direction of the wind to prevent inhalation through 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, seek medical treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Isocarb EC is two years from the date of production. All indicators should meet the standard requirements when leaving the factory. During the warranty period, the mass fraction of Isocarb in 40% and 50% Isocarb EC should not be less than 39.0% and 48.5%, and other indicators should meet the standard requirements. (30)2 Determination steps
Weigh 1g of the sample (accurate to 0.002g), place it 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 it turns orange-yellow, which is the end point. Perform a blank determination at the same time.
The acidity e2 (%) of the sample expressed as the mass fraction of sulfuric acid (H2SO4) is calculated according to formula (2): c(V4-V4)X0.049
Where:
The actual concentration of the sodium hydroxide standard titration solution, in moles per liter (mol/L); V—the volume of the sodium hydroxide standard titration solution consumed in titrating the sample solution, in milliliters (mL); V.一Titrate blank, the volume of sodium hydroxide standard titration solution consumed, in milliliters (mL); m
Sample mass, in grams (g);
The mass of sulfuric acid in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c (NaOH) = 1.000mol/L.
4.6 Emulsion stability test
Carry out in accordance with GB/T1603. Test results, no floating oil on the top, no sinking oil and precipitation below are qualified. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃ for 1h, and the presence of solid and oily precipitation is recorded. Continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instrument
Refrigerator: maintain 0℃±2℃.
Centrifuge tube: 100mL, with scale on the bottom of the tube accurate to 0.05mL. Centrifuge: Matching with centrifuge tube.
4.7.3 Test steps
HG3286—2002
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0℃±2℃ in the refrigerator, keep the centrifuge tube and its contents at 0℃±2℃ for 1h, stir it every 15min, and each time for 15s, check and record whether there is solid or oily precipitation. Put the centrifuge tube back into the refrigerator and continue to place it at 0℃±2℃ for 7d, then take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge it for 15min (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Thermal storage stability test
4.8.1 Apparatus
Thermostatic box (or thermostatic water bath): 54℃±2℃. Ampoule (or bottle with a stopper that can still be sealed at 54℃): 50mL. Medical syringe 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of the emulsifiable concentrate sample into a clean ampoule (or glass bottle) (avoid the sample from contacting the bottleneck), place the ampoule in an ice-salt bath until it is cooled, and quickly seal it with a high-temperature flame (to avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed ones in a metal container, and then place the metal container in a thermostatic box (or water bath) at 54℃±2℃ for 14 days. Take out and cool to room temperature, wipe the outside of the container and weigh them separately. For samples with unchanged mass, test the mass fraction of Isoblast and emulsion stability within 24 hours. The content of Isoblast emulsion after storage should not be less than 95% of the content measured before storage, and the emulsion stability should meet the standard requirements. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of Isoblast emulsion shall comply with the provisions of GB4838. 5.2 Isoblast emulsion shall be packaged in brown glass bottles with stoppers and caps, with a net content of 500g, 1000g, etc.; the outer packaging shall be calcium plastic boxes or corrugated boxes, and the net content of each box shall not exceed 15kg. 5.3 According to user requirements or ordering agreements, other forms of packaging may be used, but they must comply with the provisions of GB4838. 5.4 Packages should be stored in ventilated, dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Isocarb is a low-toxic fungicide. Wear protective gloves when using this product. Spray in the direction of the wind to prevent inhalation through 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, seek medical treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Isocarb EC is two years from the date of production. All indicators should meet the standard requirements when leaving the factory. During the warranty period, the mass fraction of Isocarb in 40% and 50% Isocarb EC should not be less than 39.0% and 48.5%, and other indicators should meet the standard requirements. (30)4 Packages should be stored in ventilated, dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Isocarb is a low-toxic fungicide. Wear protective gloves when using this product. Spray in the direction of the wind to prevent inhalation through 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, seek medical treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Isocarb EC is two years from the date of production. All indicators should meet the standard requirements when leaving the factory. During the warranty period, the mass fraction of Isocarb in 40% and 50% Isocarb EC should not be less than 39.0% and 48.5%, and other indicators should meet the standard requirements. (30)4 Packages should be stored in a ventilated, dry warehouse. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Isocarb is a low-toxic fungicide. Wear protective gloves when using this product. Spray in the direction of the wind to prevent inhalation through 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, seek medical treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Isocarb EC is two years from the date of production. All indicators should meet the standard requirements when leaving the factory. During the warranty period, the mass fraction of Isocarb in 40% and 50% Isocarb EC should not be less than 39.0% and 48.5%, and other indicators should meet the standard requirements. (30)
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