Some standard content:
ICS65.100
Registration No.: 10930—2002
Chemical Industry Standard of the People's Republic of China
HG33052002
Replaces HG3305-1990
Isoprothiolane Emulsifiable Concentrates
Isoprothiolane Emulsifiable Concentrates2002-09-28 Issued
Implemented on 2003-06-01
Isoprothiolane Emulsifiable Concentrates Issued on 2002-09-28
Isoprothiolane Emulsifiable Concentrates Issued on 2003-06-01 Issued by the State Economic and Trade Commission of the People's Republic of China Foreword
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. This standard replaces the mandatory chemical industry standard HG3305-1990 "Isoprothiolane Emulsifiable Concentrates". The main differences between this standard and HG3305--1990 are: 1. The foreword is added.
HG3305—2002
- The mass fraction of rice blasting agent was changed from 30.0± to greater than or equal to 30.0% and 40.0± to greater than or equal to 40.0% respectively; the acidity was changed from less than or equal to 0.3% to less than or equal to 0.2%. - The method for determining low temperature stability was changed from 0℃±2℃ storage for 1h to 0℃±2℃ storage for 7d, and the precipitate was required to be no more than 0.3mL.
- The analytical conditions of the capillary gas chromatography method for the mass fraction of rice blasting agent were 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: Shenyang Chemical Research Institute. The participating drafting units of this standard: 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 Technical Committee for Standardization of Pesticides for interpretation. I
Isoprothiolane EC
Other names, structural formulas and basic physicochemical parameters of the active ingredient of this product, isoprothiolane, are as follows: ISO common name: Isoprothiolane
CIPAC digital code: 456
Chemical name: 1,3-dithiolane-2-ylidenemalonic acid diisopropyl ester Structural formula:
-CHCH）
-CH(CHs）
Empirical formula: C12H1aO,S2
Relative molecular mass, 290.4 (according to the 1997 National International relative atomic mass) Biological activity: Bactericidal
Melting point: 50℃~54.5℃
Boiling point: 167℃~169℃/66.5Pa
HG3305—2002
Solubility (g/L, 20℃): 0.048 in water, easily soluble in organic solvents such as benzene, alcohol, acetone, etc. 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 rice blast emulsifiable concentrate. This standard applies to rice blast emulsifiable concentrate prepared by dissolving rice blast emulsifiable concentrate that meets the standard with an emulsifier 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/T1600 Determination of moisture content in pesticides
GB/T1603 Determination of stability of pesticide emulsions GB/T1604 Acceptance rules for commercial pesticides
GB/T1605 Sampling methods for commercial pesticides
8 Packaging of pesticide emulsions
GB4838
3 Requirements
3.1 Appearance: It should be a stable homogeneous liquid without visible suspended matter and precipitation. 3.2 The control indicators of rice cancer emulsion should meet the requirements of Table 1. (67)
HG3305--2002
Mass fraction of rice blast, %
Water, %
Acidity (in HSO,), %
Emulsion stability (diluted 200 times)
Low temperature stability
Hot storage stability"
Control item indicators of rice blast emulsion
Low temperature stability and hot storage stability tests shall be conducted at least once every three months. 4 Test methods
4.1 Sampling
The method of "Sampling of liquid preparations" in GB/T1605 shall be followed. The sampling packages shall be determined by the random number table method, and the final sampling volume shall be not less than 250mL.
4.2 Identification test
Gas chromatography method ：This identification test can be carried out simultaneously with the determination of the mass fraction of rice cancer. 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 rice cancer in the standard solution should be within 1.5%. When there are doubts about the identification of the active ingredient using the above method, other effective methods can be used for identification. 4.3 Determination of the mass fraction of rice cancer
4.3.1 Method summary
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 chromatography 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||t t||Trifluoromethane.
Standard sample of rice blast: known mass fraction greater than or equal to 99.0%. n-Docosane: must not contain impurities that interfere with the chromatographic analysis. Stationary phase: SE-30.
Carrier: ChromosorbWAWDMCS, 180μm~25oμm (or other carriers with equivalent performance). Internal standard solution: weigh about 2.4g of n-docosane in a 1000mL volumetric flask, dissolve and dilute to the scale with chloroform, and shake the spoon. 4.3.3 Instruments
Gas chromatograph: hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1m×3mm(id) glass column (or stainless steel column). Column filling: 5%SE-30/Chromoso rbWAWDMCS (180μm~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 the 7 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 2h, take it out and place it in a desiccator for use. 4.3.4.2 Filling of chromatographic column
Connect a small funnel to the outlet of the washed and dried chromatographic column, and fill the prepared filler into the column in batches, while constantly tapping the column wall 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 constantly tap the column wall to make it evenly and tightly filled. After filling, also plug a small ball of glass wool at the inlet end and press it appropriately to keep the column filler from moving. 4.3.4.3 Aging of chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, do not connect the detector at the outlet end, pass the carrier gas (Nz) at a flow rate of 20 mL/min, raise the temperature to 250℃ 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 (N2) 35 Hydrogen 40
Air 300
Injection volume (pL): 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 emulsifiable concentrate is shown in Figure 1. (69)
HG33052002
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
1-Solvent; 2-Pyrochlore; 3-Internal standard (n-docosane) Figure 1 Gas chromatogram of pyrochlore emulsifiable concentrate
Weigh 0.1g of pyrochlore standard sample (accurate to 0.0002g), place it in a stoppered glass bottle, accurately add 20mL of internal standard solution with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh 0.1g of sample containing pyrochlore (accurate to 0.0002g), place it in a stoppered glass bottle, accurately add 20mL of internal standard solution with the same pipette as in 4.3.6.1, and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the instrument baseline is stable, inject several needles of standard solution continuously, 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%, measure 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 of rice blasting agent (%) is calculated according to formula (1): te,-m;P
Wherein:
-the average value of the peak area ratio of rice blasting agent to internal standard substance in standard solution; r
-the average value of the peak area ratio of rice blasting agent to internal standard substance in sample solution; ml--the mass of standard sample, in grams (g); (70)
mz--the mass of sample, in grams (g)P--the mass fraction of rice blasting agent in standard sample, expressed in %. HG3305-2002
Also, according to the provisions of GB/T4946 "Terms of Gas Chromatography", the correction factor is calculated first, and then the effective body mass fraction in the sample is calculated.
4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. 4.4 Determination of moisture
4.4.1 Determination method
According to the "Karl Fischer method" in GB/T1600, it is allowed to use a moisture meter with equivalent accuracy. 4.4.2 Allowable difference
The relative deviation of two parallel determination results should not be greater than ± 25%. Take the arithmetic mean as the determination result. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Standard sodium hydroxide titration solution: c(NaOH)=0.02mol/L. 95% ethanol.
Methyl bromide Phenol 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 to mix. 4.5.2 Determination steps
Weigh 3g~4g of sample (accurate to 0.0002g), place 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. At the same time, perform a blank determination. The acidity of the sample expressed as the mass fraction of sulfuric acid (HSO) w2 (%) is calculated according to formula (2): c(Vi-V.)X0. 049×100
Where:
c—actual concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L); Vi—volume of sodium hydroxide standard titration solution consumed by titrating sample solution, in milliliters (mL) V. - volume of sodium hydroxide standard titration solution consumed by titrating blank solution, in milliliters (mL) m-——mass of sample, in grams (g): (2)bzxZ.net
0.049--with 1.00mL sodium hydroxide standard titration solution Lc (NaOH) = 1.000mol/LI is the mass of sulfuric acid expressed in grams.
4.5.3 Allowable difference
The relative deviation of two parallel determination results should not be greater than ±25%. Take the arithmetic mean as the determination result. 4.6 Determination of emulsion stability
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the surface and no precipitation on the bottom. 4.7 Low temperature stability test
4.7.1 Method summary|| tt||Keep the sample at 0℃ for 1h, record whether there is solid and oily precipitation, continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instruments
Refrigerator: maintain 0℃±2℃
Centrifuge tube: 100mL, the scale on the bottom of the tube is accurate to 0.05mLCentrifuge: matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0 in the refrigerator ℃±2℃, keep the centrifuge tube and its contents at (71)
HG3305-—2002
0℃±2℃ for 1 hour, stir every 15 minutes, each time for 15 seconds, 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 7 days. Take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge 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 (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Hot Storage Stability Test
4.8.1 Instrument
Constant Temperature Box (or Constant Temperature Water Bath): 54℃±2℃. An (or a stoppered glass bottle that can still be sealed at 54℃). Medical syringe: 50mL.
4.8.2 Test steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid the solvent from volatilizing). Seal at least 3 bottles and weigh them separately. Place the sealed bottles in a metal container, and then place the metal container in a constant temperature box (or constant temperature water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with unchanged mass, measure the mass fraction of rice blast and emulsion stability within 24 hours. The mass fraction of rice blast after storage should not be less than 97% of the mass fraction measured before storage, and the emulsion stability should still meet the standard requirements. 4.9 Inspection and acceptance of products
Should 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, packaging, purchase and transportation of Daokailing EC shall comply with the provisions of GB4838. 5.2 Daokailing EC shall be packaged in clean and dry steel drums with a net content of 200kg per drum. It shall be packaged in glass bottles or polyester bottles, and the net content of each bottle and box shall not be less than the value indicated on the label. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Daokailing EC packages shall be stored in ventilated and dry warehouses. 5.5 During transportation, strictly 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: This product is a low-toxic preparation that can penetrate through the skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash it immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of the rice cancer emulsion is two years from the date of production. (72)
A.1 Method Summary
Appendix A
(Informative Appendix)
Analysis conditions of rice cancer capillary gas chromatography HG3305-2002
The sample is dissolved in trifluoromethane, and n-docosane is used as the internal standard. The gas chromatography separation and determination are carried out on the HP-1701 column using a hydrogen flame ionization detector.
A.2 Gas chromatography operating conditions
Gas chromatograph: equipped with a hydrogen flame ionization detector. Chromatographic column: 30m×0.32mm(id) glass column, coated with HP-1701, liquid film thickness: 0.25μm or other capillary columns that can meet the requirements of separation degree.
Column temperature: 220℃, vaporization temperature: 260℃; detector temperature: 260℃. Carrier gas flow rate (nitrogen): 2mL/min: hydrogen flow rate: 30mL/min. Air flow rate: 300mL/min.
Split ratio: 40:1.
Injection volume: 1.0μL.
Retention time: about 7.8min for rice blast, about 3.8min for n-docosane. The above operating conditions are typical operating parameters. According to the characteristics of different instruments and chromatographic columns, the given operating parameters can be appropriately adjusted to obtain the best effect. The capillary gas chromatogram of rice blast emulsifiable concentrate is shown in Figure A.1. 2
1-Internal standard (n-docosane); 2-Rice blast Figure A.1 Capillary gas chromatogram of rice blast emulsifiable concentrate (73)1 Preparation of standard solution
1-Solvent; 2-Pyrochlore; 3-Internal standard (n-docosane) Figure 1 Gas chromatogram of Pyrochlore emulsifiable concentrate
Weigh 0.1g of Pyrochlore standard sample (accurate to 0.0002g), place it in a stoppered glass bottle, accurately add 20mL of internal standard solution with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh 0.1g of sample containing Pyrochlore (accurate to 0.0002g), place it in a stoppered glass bottle, accurately add 20mL of internal standard solution with the same pipette as in 4.3.6.1, and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the instrument baseline is stable, inject several needles of standard solution continuously, 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%, measure 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 of rice blasting agent (%) is calculated according to formula (1): te,-m;P
Wherein:
-the average value of the peak area ratio of rice blasting agent to internal standard substance in standard solution; r
-the average value of the peak area ratio of rice blasting agent to internal standard substance in sample solution; ml--the mass of standard sample, in grams (g); (70)
mz--the mass of sample, in grams (g)P--the mass fraction of rice blasting agent in standard sample, expressed in %. HG3305-2002
Also, according to the provisions of GB/T4946 "Terms of Gas Chromatography", the correction factor is calculated first, and then the effective body mass fraction in the sample is calculated.
4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. 4.4 Determination of moisture
4.4.1 Determination method
According to the "Karl Fischer method" in GB/T1600, it is allowed to use a moisture meter with equivalent accuracy. 4.4.2 Allowable difference
The relative deviation of two parallel determination results should not be greater than ± 25%. Take the arithmetic mean as the determination result. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Standard sodium hydroxide titration solution: c(NaOH)=0.02mol/L. 95% ethanol.
Methyl bromide Phenol 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 to mix. 4.5.2 Determination steps
Weigh 3g~4g of sample (accurate to 0.0002g), place 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. At the same time, perform a blank determination. The acidity of the sample expressed as the mass fraction of sulfuric acid (HSO) w2 (%) is calculated according to formula (2): c(Vi-V.)X0. 049×100
Where:
c—actual concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L); Vi—volume of sodium hydroxide standard titration solution consumed by titrating sample solution, in milliliters (mL) V. - volume of sodium hydroxide standard titration solution consumed by titrating blank solution, in milliliters (mL) m-——mass of sample, in grams (g): (2)
0.049--with 1.00mL sodium hydroxide standard titration solution Lc (NaOH) = 1.000mol/LI is the mass of sulfuric acid expressed in grams.
4.5.3 Allowable difference
The relative deviation of two parallel determination results should not be greater than ±25%. Take the arithmetic mean as the determination result. 4.6 Determination of emulsion stability
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the surface and no precipitation on the bottom. 4.7 Low temperature stability test
4.7.1 Method summary|| tt||Keep the sample at 0℃ for 1h, record whether there is solid and oily precipitation, continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instruments
Refrigerator: maintain 0℃±2℃
Centrifuge tube: 100mL, the scale on the bottom of the tube is accurate to 0.05mLCentrifuge: matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0 in the refrigerator ℃±2℃, keep the centrifuge tube and its contents at (71)
HG3305-—2002
0℃±2℃ for 1 hour, stir every 15 minutes, each time for 15 seconds, 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 7 days. Take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge 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 (accurate to 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℃. An (or a stoppered glass bottle that can still be sealed at 54℃). Medical syringe: 50mL.
4.8.2 Test steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid the solvent from volatilizing). Seal at least 3 bottles and weigh them separately. Place the sealed bottles in a metal container, and then place the metal container in a constant temperature box (or constant temperature water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with unchanged mass, measure the mass fraction of rice blast and emulsion stability within 24 hours. The mass fraction of rice blast after storage should not be less than 97% of the mass fraction measured before storage, and the emulsion stability should still meet the standard requirements. 4.9 Inspection and acceptance of products
Should 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, packaging, purchase and transportation of Daokailing EC shall comply with the provisions of GB4838. 5.2 Daokailing EC shall be packaged in clean and dry steel drums with a net content of 200kg per drum. It shall be packaged in glass bottles or polyester bottles, and the net content of each bottle and box shall not be less than the value indicated on the label. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Daokailing EC packages shall be stored in ventilated and dry warehouses. 5.5 During transportation, strictly 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: This product is a low-toxic preparation that can penetrate through the skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash it immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of the rice cancer emulsion is two years from the date of production. (72)
A.1 Method Summary
Appendix A
(Informative Appendix)
Analysis conditions of rice cancer capillary gas chromatography HG3305-2002
The sample is dissolved in trifluoromethane, and n-docosane is used as the internal standard. The gas chromatography separation and determination are carried out on the HP-1701 column using a hydrogen flame ionization detector.
A.2 Gas chromatography operating conditions
Gas chromatograph: equipped with a hydrogen flame ionization detector. Chromatographic column: 30m×0.32mm(id) glass column, coated with HP-1701, liquid film thickness: 0.25μm or other capillary columns that can meet the requirements of separation degree.
Column temperature: 220℃, vaporization temperature: 260℃; detector temperature: 260℃. Carrier gas flow rate (nitrogen): 2mL/min: hydrogen flow rate: 30mL/min. Air flow rate: 300mL/min.
Split ratio: 40:1.
Injection volume: 1.0μL.
Retention time: about 7.8min for rice blast, about 3.8min for n-docosane. The above operating conditions are typical operating parameters. According to the characteristics of different instruments and chromatographic columns, the given operating parameters can be appropriately adjusted to obtain the best effect. The capillary gas chromatogram of rice blast emulsifiable concentrate is shown in Figure A.1. 2
1-Internal standard (n-docosane); 2-Rice blast Figure A.1 Capillary gas chromatogram of rice blast emulsifiable concentrate (73)1 Preparation of standard solution
1-Solvent; 2-Pyrochlore; 3-Internal standard (n-docosane) Figure 1 Gas chromatogram of Pyrochlore emulsifiable concentrate
Weigh 0.1g of Pyrochlore standard sample (accurate to 0.0002g), place it in a stoppered glass bottle, accurately add 20mL of internal standard solution with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh 0.1g of sample containing Pyrochlore (accurate to 0.0002g), place it in a stoppered glass bottle, accurately add 20mL of internal standard solution with the same pipette as in 4.3.6.1, and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the instrument baseline is stable, inject several needles of standard solution continuously, 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%, measure 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 of rice blasting agent (%) is calculated according to formula (1): te,-m;P
Wherein:
-the average value of the peak area ratio of rice blasting agent to internal standard substance in standard solution; r
-the average value of the peak area ratio of rice blasting agent to internal standard substance in sample solution; ml--the mass of standard sample, in grams (g); (70)
mz--the mass of sample, in grams (g)P--the mass fraction of rice blasting agent in standard sample, expressed in %. HG3305-2002
Also, according to the provisions of GB/T4946 "Terms of Gas Chromatography", the correction factor is calculated first, and then the effective body mass fraction in the sample is calculated.
4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. 4.4 Determination of moisture
4.4.1 Determination method
According to the "Karl Fischer method" in GB/T1600, it is allowed to use a moisture meter with equivalent accuracy. 4.4.2 Allowable difference
The relative deviation of two parallel determination results should not be greater than ± 25%. Take the arithmetic mean as the determination result. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Standard sodium hydroxide titration solution: c(NaOH)=0.02mol/L. 95% ethanol.
Methyl bromide Phenol 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 to mix. 4.5.2 Determination steps
Weigh 3g~4g of sample (accurate to 0.0002g), place 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. At the same time, perform a blank determination. The acidity of the sample expressed as the mass fraction of sulfuric acid (HSO) w2 (%) is calculated according to formula (2): c(Vi-V.)X0. 049×100
Where:
c—actual concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L); Vi—volume of sodium hydroxide standard titration solution consumed by titrating sample solution, in milliliters (mL) V. - volume of sodium hydroxide standard titration solution consumed by titrating blank solution, in milliliters (mL) m-——mass of sample, in grams (g): (2)
0.049--with 1.00mL sodium hydroxide standard titration solution Lc (NaOH) = 1.000mol/LI is the mass of sulfuric acid expressed in grams.
4.5.3 Allowable difference
The relative deviation of two parallel determination results should not be greater than ±25%. Take the arithmetic mean as the determination result. 4.6 Determination of emulsion stability
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the surface and no precipitation on the bottom. 4.7 Low temperature stability test
4.7.1 Method summary|| tt||Keep the sample at 0℃ for 1h, record whether there is solid and oily precipitation, continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instruments
Refrigerator: maintain 0℃±2℃
Centrifuge tube: 100mL, the scale on the bottom of the tube is accurate to 0.05mLCentrifuge: matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0 in the refrigerator ℃±2℃, keep the centrifuge tube and its contents at (71)
HG3305-—2002
0℃±2℃ for 1 hour, stir every 15 minutes, each time for 15 seconds, 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 7 days. Take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge 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 (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Hot Storage Stability Test
4.8.1 Instrument
Constant Temperature Box (or Constant Temperature Water Bath): 54℃±2℃. An (or a stoppered glass bottle that can still be sealed at 54℃). Medical syringe: 50mL.
4.8.2 Test steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid the solvent from volatilizing). Seal at least 3 bottles and weigh them separately. Place the sealed bottles in a metal container, and then place the metal container in a constant temperature box (or constant temperature water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with unchanged mass, measure the mass fraction of rice blast and emulsion stability within 24 hours. The mass fraction of rice blast after storage should not be less than 97% of the mass fraction measured before storage, and the emulsion stability should still meet the standard requirements. 4.9 Inspection and acceptance of products
Should 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, packaging, purchase and transportation of Daokailing EC shall comply with the provisions of GB4838. 5.2 Daokailing EC shall be packaged in clean and dry steel drums with a net content of 200kg per drum. It shall be packaged in glass bottles or polyester bottles, and the net content of each bottle and box shall not be less than the value indicated on the label. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Daokailing EC packages shall be stored in ventilated and dry warehouses. 5.5 During transportation, strictly 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: This product is a low-toxic preparation that can penetrate through the skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash it immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of the rice cancer emulsion is two years from the date of production. (72)
A.1 Method Summary
Appendix A
(Informative Appendix)
Analysis conditions of rice cancer capillary gas chromatography HG3305-2002
The sample is dissolved in trifluoromethane, and n-docosane is used as the internal standard. The gas chromatography separation and determination are carried out on the HP-1701 column using a hydrogen flame ionization detector.
A.2 Gas chromatography operating conditions
Gas chromatograph: equipped with a hydrogen flame ionization detector. Chromatographic column: 30m×0.32mm(id) glass column, coated with HP-1701, liquid film thickness: 0.25μm or other capillary columns that can meet the requirements of separation degree.
Column temperature: 220℃, vaporization temperature: 260℃; detector temperature: 260℃. Carrier gas flow rate (nitrogen): 2mL/min: hydrogen flow rate: 30mL/min. Air flow rate: 300mL/min.
Split ratio: 40:1.
Injection volume: 1.0μL.
Retention time: about 7.8min for rice blast, about 3.8min for n-docosane. The above operating conditions are typical operating parameters. According to the characteristics of different instruments and chromatographic columns, the given operating parameters can be appropriately adjusted to obtain the best effect. The capillary gas chromatogram of rice blast emulsifiable concentrate is shown in Figure A.1. 2
1-Internal standard (n-docosane); 2-Rice blast Figure A.1 Capillary gas chromatogram of rice blast emulsifiable concentrate (73)1g (accurate to 0.0002g), put it in a glass bottle with a stopper, add 20mL of internal standard solution accurately with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh 0.1g of sample containing rice blasting agent (accurate to 0.0002g), put it in a glass bottle with a stopper, use the same pipette as in 4.3.6.1 to accurately add 20mL of internal standard solution, and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the baseline of the instrument 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%, determine 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 rice blasting agent to the internal standard substance in the two needles of sample solution and the two needles of standard solution before and after the sample. The mass fraction of rice blasting agent (%) is calculated according to formula (1): te,-m;P
Wherein:
-the average value of the peak area ratio of rice blasting agent to internal standard substance in standard solution; r
-the average value of the peak area ratio of rice blasting agent to internal standard substance in sample solution; ml--the mass of standard sample, in grams (g); (70)
mz--the mass of sample, in grams (g)P--the mass fraction of rice blasting agent in standard sample, expressed in %. HG3305-2002
Also, according to the provisions of GB/T4946 "Terms of Gas Chromatography", the correction factor is calculated first, and then the effective body mass fraction in the sample is calculated.
4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. 4.4 Determination of moisture
4.4.1 Determination method
According to the "Karl Fischer method" in GB/T1600, it is allowed to use a moisture meter with equivalent accuracy. 4.4.2 Allowable difference
The relative deviation of two parallel determination results should not be greater than ± 25%. Take the arithmetic mean as the determination result. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Standard sodium hydroxide titration solution: c(NaOH)=0.02mol/L. 95% ethanol.
Methyl bromide Phenol 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 to mix. 4.5.2 Determination steps
Weigh 3g~4g of sample (accurate to 0.0002g), place 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. At the same time, perform a blank determination. The acidity of the sample expressed as the mass fraction of sulfuric acid (HSO) w2 (%) is calculated according to formula (2): c(Vi-V.)X0. 049×100
Where:
c—actual concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L); Vi—volume of sodium hydroxide standard titration solution consumed by titrating sample solution, in milliliters (mL) V. - volume of sodium hydroxide standard titration solution consumed by titrating blank solution, in milliliters (mL) m-——mass of sample, in grams (g): (2)
0.049--with 1.00mL sodium hydroxide standard titration solution Lc (NaOH) = 1.000mol/LI is the mass of sulfuric acid expressed in grams.
4.5.3 Allowable difference
The relative deviation of two parallel determination results should not be greater than ±25%. Take the arithmetic mean as the determination result. 4.6 Determination of emulsion stability
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the surface and no precipitation on the bottom. 4.7 Low temperature stability test
4.7.1 Method summary|| tt||Keep the sample at 0℃ for 1h, record whether there is solid and oily precipitation, continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instruments
Refrigerator: maintain 0℃±2℃
Centrifuge tube: 100mL, the scale on the bottom of the tube is accurate to 0.05mLCentrifuge: matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0 in the refrigerator ℃±2℃, keep the centrifuge tube and its contents at (71)
HG3305-—2002
0℃±2℃ for 1 hour, stir every 15 minutes, each time for 15 seconds, 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 7 days. Take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge 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 (accurate to 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℃. An (or a stoppered glass bottle that can still be sealed at 54℃). Medical syringe: 50mL.
4.8.2 Test steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid the solvent from volatilizing). Seal at least 3 bottles and weigh them separately. Place the sealed bottles in a metal container, and then place the metal container in a constant temperature box (or constant temperature water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with unchanged mass, measure the mass fraction of rice blast and emulsion stability within 24 hours. The mass fraction of rice blast after storage should not be less than 97% of the mass fraction measured before storage, and the emulsion stability should still meet the standard requirements. 4.9 Inspection and acceptance of products
Should 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, packaging, purchase and transportation of Daokailing EC shall comply with the provisions of GB4838. 5.2 Daokailing EC shall be packaged in clean and dry steel drums with a net content of 200kg per drum. It shall be packaged in glass bottles or polyester bottles, and the net content of each bottle and box shall not be less than the value indicated on the label. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Daokailing EC packages shall be stored in ventilated and dry warehouses. 5.5 During transportation, strictly 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: This product is a low-toxic preparation that can penetrate through the skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash it immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of the rice cancer emulsion is two years from the date of production. (72)
A.1 Method Summary
Appendix A
(Informative Appendix)
Analysis conditions of rice cancer capillary gas chromatography HG3305-2002
The sample is dissolved in trifluoromethane, and n-docosane is used as the internal standard. The gas chromatography separation and determination are carried out on the HP-1701 column using a hydrogen flame ionization detector.
A.2 Gas chromatography operating conditions
Gas chromatograph: equipped with a hydrogen flame ionization detector. Chromatographic column: 30m×0.32mm(id) glass column, coated with HP-1701, liquid film thickness: 0.25μm or other capillary columns that can meet the requirements of separation degree.
Column temperature: 220℃, vaporization temperature: 260℃; detector temperature: 260℃. Carrier gas flow rate (nitrogen): 2mL/min: hydrogen flow rate: 30mL/min. Air flow rate: 300mL/min.
Split ratio: 40:1.
Injection volume: 1.0μL.
Retention time: about 7.8min for rice blast, about 3.8min for n-docosane. The above operating conditions are typical operating parameters. According to the characteristics of different instruments and chromatographic columns, the given operating parameters can be appropriately adjusted to obtain the best effect. The capillary gas chromatogram of rice blast emulsifiable concentrate is shown in Figure A.1. 2
1-Internal standard (n-docosane); 2-Rice blast Figure A.1 Capillary gas chromatogram of rice blast emulsifiable concentrate (73)1g (accurate to 0.0002g), put it in a glass bottle with a stopper, add 20mL of internal standard solution accurately with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh 0.1g of sample containing rice blasting agent (accurate to 0.0002g), put it in a glass bottle with a stopper, use the same pipette as in 4.3.6.1 to accurately add 20mL of internal standard solution, and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the baseline of the instrument 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%, determine 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 rice blasting agent to the internal standard substance in the two needles of sample solution and the two needles of standard solution before and after the sample. The mass fraction of rice blasting agent (%) is calculated according to formula (1): te,-m;P
Wherein:
-the average value of the peak area ratio of rice blasting agent to internal standard substance in standard solution; r
-the average value of the peak area ratio of rice blasting agent to internal standard substance in sample solution; ml--the mass of standard sample, in grams (g); (70)
mz--the mass of sample, in grams (g)P--the mass fraction of rice blasting agent in standard sample, expressed in %. HG3305-2002
Also, according to the provisions of GB/T4946 "Terms of Gas Chromatography", the correction factor is calculated first, and then the effective body mass fraction in the sample is calculated.
4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. 4.4 Determination of moisture
4.4.1 Determination method
According to the "Karl Fischer method" in GB/T1600, it is allowed to use a moisture meter with equivalent accuracy. 4.4.2 Allowable difference
The relative deviation of two parallel determination results should not be greater than ± 25%. Take the arithmetic mean as the determination result. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Standard sodium hydroxide titration solution: c(NaOH)=0.02mol/L. 95% ethanol.
Methyl bromide Phenol 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 to mix. 4.5.2 Determination steps
Weigh 3g~4g of sample (accurate to 0.0002g), place 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. At the same time, perform a blank determination. The acidity of the sample expressed as the mass fraction of sulfuric acid (HSO) w2 (%) is calculated according to formula (2): c(Vi-V.)X0. 049×100
Where:
c—actual concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L); Vi—volume of sodium hydroxide standard titration solution consumed in titration of sample solution, in milliliters (mL) V. - volume of sodium hydroxide standard titration solution consumed in titration of blank solution, in milliliters (mL) m-——mass of sample, in grams (g): (2)
0.049--with 1.00mL sodium hydroxide standard titration solution Lc (NaOH) = 1.000mol/LI is the mass of sulfuric acid expressed in grams.
4.5.3 Allowable difference
The relative deviation of two parallel determination results should not be greater than ±25%. Take the arithmetic mean as the determination result. 4.6 Determination of emulsion stability
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the surface and no precipitation on the bottom. 4.7 Low temperature stability test
4.7.1 Method summary|| tt||Keep the sample at 0℃ for 1h, record whether there is solid and oily precipitation, continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instruments
Refrigerator: maintain 0℃±2℃
Centrifuge tube: 100mL, the scale on the bottom of the tube is accurate to 0.05mLCentrifuge: matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0 in the refrigerator. ℃±2℃, keep the centrifuge tube and its contents at (71)
HG3305-—2002
0℃±2℃ for 1 hour, stir every 15 minutes, each time for 15 seconds, 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 7 days. Take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge 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 (accurate to 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℃. An (or a stoppered glass bottle that can still be sealed at 54℃). Medical syringe: 50mL.
4.8.2 Test steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid the solvent from volatilizing). Seal at least 3 bottles and weigh them separately. Place the sealed bottles in a metal container, and then place the metal container in a constant temperature box (or constant temperature water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with unchanged mass, measure the mass fraction of rice blast and emulsion stability within 24 hours. The mass fraction of rice blast after storage should not be less than 97% of the mass fraction measured before storage, and the emulsion stability should still meet the standard requirements. 4.9 Inspection and acceptance of products
Should 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, packaging, purchase and transportation of Daokailing EC shall comply with the provisions of GB4838. 5.2 Daokailing EC shall be packaged in clean and dry steel drums with a net content of 200kg per drum. It shall be packaged in glass bottles or polyester bottles, and the net content of each bottle and box shall not be less than the value indicated on the label. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Daokailing EC packages shall be stored in ventilated and dry warehouses. 5.5 During transportation, strictly 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: This product is a low-toxic preparation that can penetrate through the skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash it immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of the rice cancer emulsion is two years from the date of production. (72)
A.1 Method Summary
Appendix A
(Informative Appendix)
Analysis conditions of rice cancer capillary gas chromatography HG3305-2002
The sample is dissolved in trifluoromethane, and n-docosane is used as the internal standard. The gas chromatography separation and determination are carried out on the HP-1701 column using a hydrogen flame ionization detector.
A.2 Gas chromatography operating conditions
Gas chromatograph: equipped with a hydrogen flame ionization detector. Chromatographic column: 30m×0.32mm(id) glass column, coated with HP-1701, liquid film thickness: 0.25μm or other capillary columns that can meet the requirements of separation degree.
Column temperature: 220℃, vaporization temperature: 260℃; detector temperature: 260℃. Carrier gas flow rate (nitrogen): 2mL/min: hydrogen flow rate: 30mL/min. Air flow rate: 300mL/min.
Split ratio: 40:1.
Injection volume: 1.0μL.
Retention time: about 7.8min for rice blast, about 3.8min for n-docosane. The above operating conditions are typical operating parameters. According to the characteristics of different instruments and chromatographic columns, the given operating parameters can be appropriately adjusted to obtain the best effect. The capillary gas chromatogram of rice blast emulsifiable concentrate is shown in Figure A.1. 2
1-Internal standard (n-docosane); 2-Rice blast Figure A.1 Capillary gas chromatogram of rice blast emulsifiable concentrate (73)1 Accurately add 20mL of internal standard solution with the same pipette and shake to hook. 4.3.6.3 Determination
Under the above operating conditions, after the baseline of the instrument 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%, measure 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 of rice blasting agent (%) is calculated according to formula (1): te,-m;P
Wherein:
-the average value of the peak area ratio of rice blasting agent to internal standard substance in standard solution; r
-the average value of the peak area ratio of rice blasting agent to internal standard substance in sample solution; ml--the mass of standard sample, in grams (g); (70)
mz--the mass of sample, in grams (g)P--the mass fraction of rice blasting agent in standard sample, expressed in %. HG3305-2002
Also, according to the provisions of GB/T4946 "Terms of Gas Chromatography", the correction factor is calculated first, and then the effective body mass fraction in the sample is calculated.
4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%. 4.4 Determination of moisture
4.4.1 Determination method
According to the "Karl Fischer method" in GB/T1600, it is allowed to use a moisture meter with equivalent accuracy. 4.4.2 Allowable difference
The relative deviation of two parallel determination results should not be greater than ± 25%. Take the arithmetic mean as the determination result. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Standard sodium hydroxide titration solution: c(NaOH)=0.02mol/L. 95% ethanol.
Methyl bromide Phenol 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 to mix. 4.5.2 Determination steps
Weigh 3g~4g of sample (accurate to 0.0002g), place 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 end point is grass green. At the same time, perform a blank determination. The acidity of the sample expressed as the mass fraction of sulfuric acid (HSO) w2 (%) is calculated according to formula (2): c(Vi-V.)X0. 049×100
Where:
c—actual concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L); Vi—volume of sodium hydroxide standard titration solution consumed in titration of sample solution, in milliliters (mL) V. - volume of sodium hydroxide standard titration solution consumed in titration of blank solution, in milliliters (mL) m-——mass of sample, in grams (g): (2)
0.049--with 1.00mL sodium hydroxide standard titration solution Lc (NaOH) = 1.000mol/LI is the mass of sulfuric acid expressed in grams.
4.5.3 Allowable difference
The relative deviation of two parallel determination results should not be greater than ±25%. Take the arithmetic mean as the determination result. 4.6 Determination of emulsion stability
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the surface and no precipitation on the bottom. 4.7 Low temperature stability test
4.7.1 Method summary|| tt||Keep the sample at 0℃ for 1h, record whether there is solid and oily precipitation, continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.7.2 Instruments
Refrigerator: maintain 0℃±2℃
Centrifuge tube: 100mL, the scale on the bottom of the tube is accurate to 0.05mLCentrifuge: matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of sample and add it to the centrifuge tube, cool it to 0 in the refrigerator. ℃±2℃, keep the centrifuge tube and its contents at (71)
HG3305-—2002
0℃±2℃ for 1 hour, stir every 15 minutes, each time for 15 seconds, 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 7 days. Take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3 hours, and centrifuge 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 (accurate to 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℃. An (or a stoppered glass bottle that can still be sealed at 54℃). Medical syringe: 50mL.
4.8.2 Test steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid the solvent from volatilizing). Seal at least 3 bottles and weigh them separately. Place the sealed bottles in a metal container, and then place the metal container in a constant temperature box (or constant temperature water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with unchanged mass, measure the mass fraction of rice blast and emulsion stability within 24 hours. The mass fraction of rice blast after storage should not be less than 97% of the mass fraction measured before storage, and the emulsion stability should still meet the standard requirements. 4.9 Inspection and acceptance of products
Should 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, packaging, purchase and transportation of Daokailing EC shall comply with the provisions of GB4838. 5.2 Daokailing EC shall be packaged in clean and dry steel drums with a net content of 200kg per drum. It shall be packaged in glass bottles or polyester bottles, and the net content of each bottle and box shall not be less than the value indicated on the label. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions of GB4838. 5.4 Daokailing EC packages shall be stored in ventilated and dry warehouses. 5.5 During transportation, strictly 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: This product is a low-toxic preparation that can penetrate through the skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash it immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of the rice cancer emulsion is two years from the date of production. (72)
A.1 Method Summary
Appendix A
(Informative Appendix)
Analysis conditions of rice cancer capillary gas chromatography HG3305-2002
The sample is dissolved in trifluoromethane, and n-docosane is used as the internal standard. The gas chromatography separation and determination are carried out on the HP-1701 column using a hydrogen flame ionization detector.
A.2 Gas chromatography operating conditions
Gas chromatograph: equipped with a hydrogen flame ionization detector. Chromatographic column: 30m×0.32mm(id) glass column, coated with HP-1701, liquid film thickness: 0.25μm or other capillary columns that can meet the requirements of separation degree.
Column temperature: 220℃, vaporization temperature: 260℃; detector temperature: 260℃. Carrier gas flow rate (nitrogen): 2mL/min: hydrogen flow rate: 30mL/min. Air flow rate: 300mL/min.
Split ratio: 40:1. |
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