Some standard content:
ICS65.100
Registration No.: 10932—2002
Chemical Industry Standard of the People's Republic of China
HG3702--2002
Trifluralin Emulsifiable Concentrates
Trifluralin Emulsifiable ConcentratesPublished on 2002-09-28
Implemented on 2003-06-01
Published by the State Economic and Trade Commission of the People's Republic of Chinawww.bzxz.net
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. 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 (CSBTC/TC133). The responsible drafting unit of this standard is Shenyang Chemical Research Institute. The participating drafting unit of this standard is Dongyang Dongnong Chemical Co., Ltd. The main drafters of this standard are Zhang Pilong, Lou Shaowei, Xu Guoxin, and Wu Hao. The Secretariat of the National Pesticide Standardization Technical Committee is entrusted with the interpretation of this standard. HG3702-—2002
Trifluralin EC
Other names, structural formulas and basic physicochemical parameters of the active ingredient trifluralin of this product are as follows: ISO common name: Trifluralin
CIPAC digital code: 183
Chemical name: N,N-dipropyl-4-trifluoromethyl-2,6-dinitroaniline Structural formula:
Empirical formula: ChraHiF.NO
NOCH.CHCHs
CH2CHaCH
Relative molecular mass: 335.3 (according to the 1997 international relative atomic mass) Biological activity: Herbicidal
Vapor pressure (25℃).1.4×10-+Pa
Relative density (22℃): 1. 36
Flash point (℃): 151 (closed cup)
Melting point (℃): 48.5~49
Boiling point (℃.24Pa): 9697
HG37022002
Solubility (g/L25℃): Water 1.84×10-4 (pH5), 2.21×10-* (pH7), 1.88×10-* (pH9), acetone 400, xylene 580, chloroform, acetonitrile, toluene, ethyl acetate 1000, methanol 33~40, hexane 50~60Stability: Stable below 52℃, stable in aqueous medium with pH=3~9 (52℃), decomposes under ultraviolet light in the range of 1
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of fluralin emulsifiable concentrate. This standard applies to trifluralin emulsifiable concentrate prepared by dissolving trifluralin technical and emulsifier in suitable solvent. 2 Normative references
The clauses in the following documents become clauses of this standard through reference in this standard. For all dated references, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties who reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For all undated references, the latest versions are applicable to this standard. GB/T1600 Determination of moisture content in pesticides
GB/T1601 Determination of pH value in pesticides
GB/T1603 Determination of stability of pesticide emulsionsGB/T1604
GB/T1605
Acceptance rules for commercial pesticides
Sampling methods for commercial pesticides
GB/T4472—1984 General rules for determination of density and relative density of chemical productsGB4838 Packaging of pesticide emulsions
3 Requirements
3.1 Appearance: It should be a stable homogeneous orange-yellow liquid with no visible suspended matter and precipitation. 3.2 The control indicators of trifluralin emulsion should meet the requirements of Table 1. (11D)
HG3702—2002
Mass fraction of trifluralin", %
or mass concentration (20℃), g/100ml
Water content, %
PH value range
Emulsion stability (diluted 200 times)
Low temperature stability
Hot storage stability
Table 1 Control item indicators of trifluralin emulsifiable concentrate
aWhen there is a dispute over the quality of trifluralin, the mass fraction calculation result shall prevail. 6 Low temperature stability and thermal stability test Under normal production conditions, the test shall be conducted at least once every three months. 4 Test method
4.1 Sampling
It shall be carried out in accordance with the "Liquid Preparation Sampling" method in GB/T1605. The sampling packages shall be determined by the random number table method, and the most The final sampling volume should be no 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 fluralin. Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak in the sample solution and the retention time of the fluralin chromatographic peak in the standard solution should be within 1.5%. 4.2.2 Infrared spectroscopy: There should be no obvious difference in the infrared spectrum of the effective component separated from the sample and the standard sample in the wavenumber range of 4000cm-1 to 400cm-. The infrared spectrum of the fluralin standard sample is shown in Figure 1.4000
Infrared spectrum of the fluralin standard sample
4.3 Determination of the mass fraction of fluralin
4.3.1 Method summary
HG3702—20 02
The sample is dissolved in acetone, and diisobutyl phthalate is used as the internal standard. A glass column filled with 5% DC-200 and a hydrogen flame ionization detector are used for gas chromatography separation and internal standard method quantification. 4.3.2 Reagents and solutions
Acetone.
Fluralin standard sample: known mass fraction greater than or equal to 99.0%. Internal standard: diisobutyl phthalate, which should be free of impurities that interfere with the analysis. Stationary phase: DC-200.
Carrier: ChromosorbW/AWDMCS (180μm～250μm). Internal standard solution: weigh 0.8g of diisobutyl phthalate, place it in a 250mL volumetric flask, add appropriate amount of acetone to dissolve it, dilute to the scale, and shake to hook.
4.3.3 Instruments
Gas Phase chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1.5mX3.2mm(id) glass column. Column filling: DC-200 coated on Chromosorb W/AWDMCS (180μm～250um), stationary liquid: (stationary liquid + carrier) = 5:100.
4.3.4 Preparation of chromatographic column
4.3.4.1 Coating of stationary liquid
Accurately weigh 0.5gDC-200 stationary liquid into a 250mL beaker, add an appropriate amount (slightly larger than the volume of the carrier) of acetone to completely dissolve it, pour in 9.5g of the carrier, shake gently to mix evenly and evaporate the solvent to nearly dry, then put the beaker in an oven at 80℃ to dry for 2h, take it out and put it in a desiccator to cool to room temperature.
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 0.5cm 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 filled evenly and tightly. After filling, also plug a small ball of glass wool at the inlet end and press it appropriately to keep the filler in the column 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 outlet end to the detector for the time being, pass the carrier gas at a flow rate of 15mL/min, raise the temperature to 230℃ in stages, and age at this temperature for 24h. 4.3.5 Gas Chromatography Operating Conditions
Temperature (°C): Column chamber 174, Vaporization chamber 205, Detector chamber 275. Gas flow rate (mL/min): Carrier gas (Nz) 50, Hydrogen 35, Air 350. Injection volume (μL): 1.0.
Retention time (min): Trifluralin 5.7, Internal standard 11.4. 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 results. The gas chromatogram of flufluralin emulsifiable concentrate is shown in Figure 2. 3
HG3702-2002
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
1—Solvent: 2—Flufluralin; 3 Internal standard
Figure 2 Gas chromatogram of flufluralin emulsifiable concentrate
Weigh 0.05 g of flufluralin standard sample (accurate to 0.0002g), put it in a stoppered glass bottle, add 10mL of internal standard solution accurately with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh a sample containing about 0.05g of fluralin (accurate to 0.0002g), put it in a stoppered glass bottle, and use the same pipette used in 4.3.6.1 to accurately add 10mL of internal standard solution, and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the relative response value of each needle, and when the relative response value of two adjacent needles changes by less than 1%, measure in the order of standard solution, sample solution, sample solution, and standard solution.
4.3.6.4 Determination of density
Perform according to 2.3 "Determination of density of liquids" in GB/T4472-1984. 4.3.7 Calculation
Average the peak area ratios of trifluralin to the internal standard in the two sample solutions and the two standard solutions before and after the sample. The mass fraction ui (%) of trifluralin is calculated according to formula (1), and the mass concentration P of trifluralin expressed in g/100mL is calculated according to formula (2):TemP
Where:
Is the average value of the peak area ratio of trifluralin to the internal standard in the standard solution; I is the average value of the peak area ratio of trifluralin to the internal standard in the sample solution; I is the mass of trifluralin standard sample, in grams (g); (114)
m2—mass of the sample, in grams (g); P—mass fraction of trifluralin in the standard sample, expressed in %; 0 is the density of trifluralin emulsifiable concentrate (20℃), in grams per milliliter (g/mL). 4.3.8 Allowable difference
The difference between two parallel determination results should not be greater than 1.0%. The arithmetic mean is taken as the determination result. 4.4 Determination of moisture
HG3702-2002
According to the "Chemical Titration (Karl Fischer Method)" in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy. 4.5 Determination of pH value
According to GB/T1601.
4.6 Emulsion stability test
The sample is diluted 200 times and then carried out according to GB/T1603. The test results show that there is no floating oil on the top, no sinking oil and precipitation on the bottom, which is qualified. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃±2℃ for 1h, and the precipitation of solid and oily substances is recorded. Continue to store at 0℃±2℃ for 7d, centrifuge, settle the solid precipitate, and record its volume.
4.7.2 Instruments
Refrigerator: maintain 0℃±2℃.
Centrifuge tube: 100mL, the scale accuracy of the tube bottom is to 0.05mL. Centrifuge, matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL 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 every 15min, each time for 15s, check and record whether there is any solid or oily matter precipitated. Put the centrifuge tube back into the refrigerator and continue to place it at 0℃±2℃ for 7d. After 7d, take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge 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 Hot storage stability test
4.8.1 Instrument
Constant temperature 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 emulsion 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 cools, and quickly seal it with a high-temperature flame (to avoid solvent evaporation), seal the two bottles, and weigh them separately. Place the sealed ampoule in a metal container, and then place the metal container in a constant temperature box (or water bath) for 14d. Take it out and cool to room temperature, After wiping the outside of the container clean, weigh them separately. For samples that have not changed in mass, test the mass fraction of fluramide and the stability of the emulsion within 24 hours. The test results should meet the requirements of 3.2.
4.9 Inspection and acceptance of products
Inspection and acceptance of products should meet the requirements of GB/T1604. The rounded value comparison method should be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of fluramide emulsifiable concentrate should meet the requirements of GB4838. 5.2 Fluramide emulsifiable concentrate should be packaged in brown glass bottles or polyester bottles with inner plugs and outer caps. The net content of each bottle is 100g, 450g, 500g, etc. The outer packaging should be made of calcium plastic boxes or corrugated paper boxes. The net content of each box should not exceed 10kg (115)
HG 3702—2002
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 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, and other materials, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin EC is low-toxic in nature. Wear protective gloves when using this product. Spray in the direction of the wind to prevent inhalation through the mouth and nose; if the skin or exposed parts of the body come into contact with this product, wash it with soap and water in time; if poisoning occurs, seek medical treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Fluoralin EC is two years from the date of production.0mL sample is added to the centrifuge tube, cooled to 0℃±2℃ in the refrigerator, and the centrifuge tube and its contents are kept at 0℃±2℃ for 1h. Stir once every 15min for 15s each time, and 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. After 7d, take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge 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 Instrument
Thermostatic box (or constant temperature water bath): 54℃±2℃. An (or a 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 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 (avoid solvent volatilization). Seal the two bottles and weigh them separately. Place the sealed ampoule in a metal container, and then place the metal container in a constant temperature box (or water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the ampoule and weigh it separately. For samples that have not changed in mass, test the mass fraction of trifluralin and the stability of the emulsion within 24 hours. The test results should meet the requirements of 3.2.
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 Fluoralin EC shall comply with the provisions of GB4838. 5.2 Fluoralin EC shall be packaged in brown glass bottles or polyester bottles with inner plugs and outer caps. The net content of each bottle is 100g, 450g, 500g, etc. The outer packaging shall be in calcium plastic boxes or corrugated paper boxes. The net content of each box shall not exceed 10kg (115)
HG 3702—2002
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, strictly prevent moisture and sunlight, do not mix with food, seeds, and other materials, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin EC is low-toxic in nature. Wear protective gloves when using this product. When spraying, it should be done in the direction of the wind to prevent inhalation through the mouth and nose; if the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time; if poisoning occurs, seek medical treatment in time. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of trifluralin emulsifiable concentrate is two years from the date of production.0mL sample is added to the centrifuge tube, cooled to 0℃±2℃ in the refrigerator, and the centrifuge tube and its contents are kept at 0℃±2℃ for 1h. Stir once every 15min for 15s each time, and 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. After 7d, take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge 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 Instrument
Thermostatic box (or constant temperature water bath): 54℃±2℃. An (or a 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 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 (avoid solvent volatilization). Seal the two bottles and weigh them separately. Place the sealed ampoule in a metal container, and then place the metal container in a constant temperature box (or water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the ampoule and weigh it separately. For samples that have not changed in mass, test the mass fraction of trifluralin and the stability of the emulsion within 24 hours. The test results should meet the requirements of 3.2.
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 Fluoralin EC shall comply with the provisions of GB4838. 5.2 Fluoralin EC shall be packaged in brown glass bottles or polyester bottles with inner plugs and outer caps. The net content of each bottle is 100g, 450g, 500g, etc. The outer packaging shall be in calcium plastic boxes or corrugated paper boxes. The net content of each box shall not exceed 10kg (115)
HG 3702—2002
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, strictly prevent moisture and sunlight, do not mix with food, seeds, and other materials, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin EC is low-toxic in nature. Wear protective gloves when using this product. When spraying, do it in the direction of the wind to prevent inhalation through the mouth and nose; if the skin or exposed parts of the body come into contact with this product, wash it with soap and water immediately; if poisoning occurs, consult a doctor immediately. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of trifluralin EC is two years from the date of production.
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