Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2320—92
Butyl Ester Emulsifiable Concentrate
2,4-D
Published on June 1, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1993
Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
Ester Emulsifiable Concentrate
HG2320—92
This standard specifies the technical conditions, test methods, inspection rules, and marking, packaging, transportation and storage requirements for 2,4-D butyl ester emulsifiable concentrate. This standard applies to 2,4-D butyl ester emulsifiable concentrate prepared from 2,4-D butyl ester technical with suitable emulsifiers and solvents. Active ingredient: 2,4-D-butyl ester
Chemical name: 2,4-dichlorophenoxyacetic acid n-butyl ester Structural formula:
Molecular formula: C12Hi/C2Os
CHCOOC,Hg
Relative molecular mass: 277.15 (according to the international relative atomic mass in 1989). Reference standards
GB1600
GB1603
GB1604
GB1605
GB4838
Technical requirements
Method for determining moisture content in pesticides
Method for determining stability of pesticide emulsions
Pesticide acceptance rules
Commercial pesticide sampling method
Emulsifiable concentrate pesticide packaging
3.1 Appearance: Brown oily single-phase liquid, without visible suspended matter and sediment. 3.2 2,4-D butyl ester emulsifiable concentrate shall also meet the following index requirements: Item
2,4-D butyl ester content, % (m/m)
Total ester content, % (m/m)
Free phenol (calculated as 2,4-dichlorophenol), % (m/m) Free acid (calculated as 2,4-D acid), % (m/m) Moisture, % (m/m)
Emulsion stability (diluted 200 times)
Low temperature stability\)
Hot storage stability2)
Note: 1) and 2) shall be inspected at least once every six months. Approved by the Ministry of Chemical Industry of the People’s Republic of China on June 1, 1992. Implementation on January 1, 1993. 4 Test method. 4.1 Determination of 2,4-D butyl ester content. 4.1.1 Summary of method. The sample was dissolved in chloroform and separated and determined on a mixed column of tetrachlorophthalic acid glycol polyester and Apizolide LChromosorb W-AWDMCS 180~250um, taking diisobutyl phthalate as the internal standard. 4.1.2 Reagents and solutions
Chloroform (GB682);
2,4-D butyl ester standard: known content; Diisobutyl phthalate: internal standard, identified by this method as having no interfering impurities; Tetrachlorophthalic acid glycol polyester: gas chromatography stationary phase; Apizone L: gas chromatography stationary phase;
Chromosorb W-AWDMCS: 180~250μm (60~80 mesh), carrier for gas chromatography; Internal standard solution: weigh 3.5g of diisobutyl phthalate, place it in a 100mL volumetric flask, add chloroform to dissolve, dilute to the scale, and shake well.
4.1.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector; chromatographic column: 2m long, 3mm inner diameter stainless steel column, filled with 1.7% tetrachlorophthalic acid ethylene glycol polyester and 0.3% Apizolide L/Chromosorb W-AWDMCS180~250um filler; recorder or gas chromatography data processor; micro-injector: 10uL.
4.1.4 Operation steps
4.1.4.1 Coating of stationary liquid
Accurately weigh 0.100g of tetrachlorophthalic acid glycol polyester and 0.020g of Apizoline L stationary liquid into a 250mL beaker, add an appropriate amount (about 25mL) of chloroform to completely dissolve it, add a certain amount of carrier (about 6g) according to the pre-prepared ratio, gently shake to mix evenly and evaporate the solvent to near dryness, then place the beaker in an oven at 110℃ for 1h, take it out and place it in a desiccator. 4.1.4.2 Filling of chromatographic column
Connect a funnel to the inlet end of the column, plug the outlet end with gauze, and connect it to the vacuum pump with a rubber tube. Turn on the vacuum pump, add the column filler from the funnel in batches, tap the tube wall continuously, so that the filler fills the chromatographic column evenly and tightly, and plug the two ends of the column with silanized glass wool.
4.1.4.3 Aging of the chromatographic column
Connect the inlet of the chromatographic column to the vaporizer, and do not connect the outlet to the detector for the time being. Aging at least 48h at a column temperature of 210℃ with a carrier flow rate of 20mL/min.
4.1.5 Chromatographic operating conditions
Temperature:
Column chamber 170℃;
Vaporizer chamber 260℃;
Detection chamber 260℃.
Gas flow rate:
Carrier (N2) 20mL/min;
Air 320mL/min;
Hydrogen 32mL/min.
Injection volume: 0.6uL.
Retention time:
2,4-D butyl ester about 11min;
Internal standard about 6.7min.
HG2320—92
Gas chromatogram of 2,4-D butyl ester
1—Solvent; 2, 3, 4, 5—Unknown impurities, 6—N-butyl monochlorophenoxyacetate; 7—Internal standard, 8—Isobutyl 24-dichlorophenoxyacetate; 9—24-D butyl ester; 10—N-butyl trichlorophenoxyacetate The above gas chromatography conditions are typical operating parameters. Analysts can make appropriate adjustments to the operating conditions according to the characteristics of the instrument to obtain the best results.
4.1.6 Determination steps
4.1.6.1 Preparation of standard solution
Weigh 0.1g (accurate to 0.0002g) of 2,4-D butyl ester standard sample and place it in a 5mL ground-mouth glass bottle. Use a pipette to accurately add 2mL of internal standard solution and shake well.
4.1.6.2 Preparation of sample solution
Weigh an emulsion sample containing about 0.1g of 2,4-D butyl ester (accurate to 0.0002g), place it in a 5mL glass bottle with a ground stopper, accurately add 2mL of internal standard solution with a pipette, and shake well. 4.1.6.3 Sample determination
Under the selected conditions, after the instrument is stable, use a microinjector to inject and analyze in the following order: standard solution, sample solution, sample solution, standard solution. The relative deviation of the peak area ratio of 2,4-D butyl ester to the internal standard in the two sample solutions and the two standard solutions before and after the sample should not be greater than 1.5%, otherwise the injection needs to be repeated. 4.1.6.4 Calculation
Calculate the average value of the peak area ratio of 2,4-D butyl ester to the internal standard in the two sample solutions and the two standard solutions before and after the sample. The mass percentage of 2,4-D butyl ester is calculated according to formula (1): 21-im2
Wherein: 1 is the average value of the peak area ratio of 2,4-D butyl ester to the internal standard in the sample solution; T2 is the average value of the peak area ratio of 2,4-D butyl ester to the internal standard in the standard solution; m1 is the mass of the sample, g;
(1)
m2 is the mass of the standard, g;
% is the mass percentage of the standard. 4.1.6.5 Allowable error
HG2320-92
The difference between the results of two parallel determinations shall not be greater than 1.5%. 4.2 Determination of total esters
4.2.1 Method summary
Use the normalized result of the corrected 2,4-D butyl ester peak area to calculate the ratio of total esters to 2,4-D butyl ester, and then multiply it by the 2,4-D butyl ester content to obtain the total ester content.
4.2.2 Operation steps
Same as in 4.1.
4.2.3 Calculation
According to the chromatogram obtained for each injection in 4.1.6.3, calculate the peak areas of corrected monochlorophenoxyacetic acid n-butyl ester, 2,4-D butyl ester, 2,4-dichlorophenoxyacetic acid isobutyl ester, and trichlorophenoxyacetic acid n-butyl ester, and the mass percentage of total esters a2 is calculated according to formula (2): 2
Wherein: a1——
-2,4-D butyl ester content;
fiA,+A2+A+f2A
Relative correction factor of butyl monochlorophenoxyacetate to 2,4-butyl ester, (1.143); f2—Relative correction factor of butyl trichlorophenoxyacetate to 2,4-butyl ester, (0.890); A1——Peak area of butyl monochlorophenoxyacetate; A2——Peak area of 2,4-butyl ester;
As——2,The peak area of 4-dichlorophenoxyacetic acid isobutyl ester; A
The peak area of trichlorophenoxyacetic acid n-butyl ester. Note: The total ester result is the average of the two injection calculation results. 4.3 Determination of free acid and free phenol
4.3.1 Method summary
The sample is dissolved in ethanol, first with methyl red as indicator, and titrated with 0.01mol/sodium hydroxide standard titration solution until yellow, at which time the free acid in the solution is completely neutralized, then add phenol as an indicator, and continue to titrate with 0.1mol/sodium hydroxide standard titration solution until the free phenol is completely neutralized.
4.3.2 Reagents and solutions
Absolute ethanol (GB678);
Standard sodium hydroxide titration solution: ci(NaOH)=0.01mol/L, c2(NaOH)=0.1mol/L, prepared and calibrated according to GB601; Methyl red indicator: 1g methyl red ethanol solution; Phenolphthalein indicator: 10g/L phenolyl ethanol solution. 4.3.3 Analysis steps
Weigh 1g (accurate to 0.0002g) of 2,4-D butyl ester emulsifiable concentrate sample into a 250mL conical flask, add 50mL of absolute ethanol to dissolve, and shake. Add 3 drops of methyl red solution and titrate with 0.01mol/L sodium hydroxide standard titration solution until the solution turns yellow. Note the volume of sodium hydroxide standard titration solution consumed (V). Add 3 drops of phenol solution and titrate with 0.1mol/L sodium hydroxide standard titration solution until the solution turns red. The end point is when the color does not fade within half a minute. Note the volume of sodium hydroxide standard titration solution consumed (V). Perform a blank experiment with the same steps. 4.3.4 Calculate the acidity mass percentage3 according to formula (3): _C(V,-V)X0.221bzxz.net
wherein—
actual concentration of sodium hydroxide standard titration solution, mol/L; (3)
HG2320-92
Vi—volume of sodium hydroxide standard titration solution consumed in titrating the free acid, mL; V'i——volume of sodium hydroxide standard titration solution consumed in titrating the blank, mL; mmass of the sample, g;
0.221——mass of 2,4-dihydrochloric acid equivalent to 1.00mL of sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L], expressed in grams.
The mass percentage of free phenol a4 is calculated according to formula (4): #4=)×0.163×100
Wherein: C2——actual concentration of sodium hydroxide standard titration solution, mol/L; V2——volume of sodium hydroxide standard titration solution consumed for titration of free phenol, mL; V'z——volume of sodium hydroxide standard titration solution consumed for titration of blank, mL; m—mass of sample, g;
0.163——mass of 2,4-dichlorophenol equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0H)=1.000mol/] in grams.
4.4 Determination of moisture
Determine according to the Karl Fischer method in GB1600. 4.5 Emulsion stability test
Take 0.5mL sample and determine according to GB1603. No floating oil on the top and no precipitation (or sinking oil) on the bottom is qualified. 4.6 Low temperature stability test
Measure about 100mL of sample into a 150mL beaker, put it into a refrigerator or ice water bath at 0±1℃, leave it for 1h, stir it from time to time, and observe whether there is solid or oily precipitation in the cup. If there is no, it is qualified. 4.7 Hot storage stability test
4.7.1 Apparatus
Constant temperature box or constant temperature water bath;
An: 50mL, long neck;
Syringe: 50mL.
4.7.2 Operating conditions
Use a syringe to inject about 20mL of sample into a clean annular (avoid the sample contacting the neck of the annular), cool the annular in an ice bath, and seal it with a gas lamp. Put the sealed annular in a metal container, and then put the container into a constant temperature box at 54±2℃ (or put the annular in a constant temperature water bath) and store it for 14d. After being taken out of the thermostat (or constant temperature water bath), all inspection items should be completed within 24 hours. After hot storage, all indicators still meet the standard requirements.
5 Inspection rules
5.12,4-D butyl ester emulsifiable concentrate products should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer should ensure that the 2,4-D butyl ester emulsifiable concentrate shipped out of the factory meets the requirements of this standard, and each batch of 2,4-D butyl ester emulsifiable concentrate shipped out of the factory should be accompanied by a quality certificate. 5.2 The batch size of each batch of 2,4-D butyl ester emulsifiable concentrate products should not exceed the capacity of the packaging storage tank. 5.3 The sampling method shall be carried out in accordance with GB1605.
5.4 The user has the right to verify whether the received 2,4-D butyl ester emulsifiable concentrate meets the requirements of this standard in accordance with the various provisions in the product standard. 5.5 If any index does not meet the standard in the test results, samples should be taken from twice the number of packages for re-testing. If only one index does not meet the requirements, the whole batch of products will be unqualified. 5.6 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation or the legal inspection agency can conduct arbitration analysis in accordance with the inspection methods specified in this standard.
Marking, packaging, transportation and purchase and storage
HG2320-92
6.12,4-D butyl ester emulsifiable concentrate shall be marked and packaged in accordance with the relevant provisions of GB4838. 6.22,4-D butyl ester emulsifiable concentrate shall be packaged in clean and dry glass bottles, with a net weight of 0.5kg or 1.0kg per bottle, covered with straw covers or foam air cushions, and tightly arranged in cartons or calcium plastic boxes, with a net weight of no more than 20kg per box. Other forms of packaging can also be used according to user requirements. All containers for packaging 2,4-D butyl ester emulsifiable concentrate must be dedicated and shall not contain other pesticides. 6.3 During storage and transportation, strictly prevent moisture and sunlight, maintain good ventilation, do not mix with food, seeds, feed, avoid contact with skin, and prevent inhalation through the mouth.
6.4 The validity period is 2 years from the date of manufacture, and all indicators are guaranteed to meet the standard requirements within 2 years. Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard was drafted and technically coordinated by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry, and the 9719 Factory of the Chinese People's Liberation Army participated in the drafting. The main drafters of this standard are Jiang Minyi, Yuan Chunfeng, Li Xiujie, Wang Xuecheng, Mei Baogui, Zhang Zhenhua, and Zhang Daidi.163×100
Wherein: C2——actual concentration of sodium hydroxide standard titration solution, mol/L; V2——volume of sodium hydroxide standard titration solution consumed for titration of free phenol, mL; V'z——volume of sodium hydroxide standard titration solution consumed for titration of blank, mL; m—mass of sample, g;
0.163——mass of 2,4-dichlorophenol equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0H)=1.000mol/] in grams.
4.4 Determination of moisture
Determine according to the Karl Fischer method in GB1600. 4.5 Emulsion stability test
Take 0.5mL sample and determine according to GB1603. No floating oil on the top and no precipitation (or sinking oil) on the bottom is qualified. 4.6 Low temperature stability test
Measure about 100mL of sample into a 150mL beaker, put it into a refrigerator or ice water bath at 0±1℃, leave it for 1h, stir it from time to time, and observe whether there is solid or oily precipitation in the cup. If there is no, it is qualified. 4.7 Hot storage stability test
4.7.1 Apparatus
Constant temperature box or constant temperature water bath;
An: 50mL, long neck;
Syringe: 50mL.
4.7.2 Operating conditions
Use a syringe to inject about 20mL of sample into a clean annular (avoid the sample contacting the neck of the annular), cool the annular in an ice bath, and seal it with a gas lamp. Put the sealed annular in a metal container, and then put the container into a constant temperature box at 54±2℃ (or put the annular in a constant temperature water bath) and store it for 14d. After being taken out of the thermostat (or constant temperature water bath), all inspection items should be completed within 24 hours. After hot storage, all indicators still meet the standard requirements.
5 Inspection rules
5.12,4-D butyl ester emulsifiable concentrate products should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer should ensure that the 2,4-D butyl ester emulsifiable concentrate shipped out of the factory meets the requirements of this standard, and each batch of 2,4-D butyl ester emulsifiable concentrate shipped out of the factory should be accompanied by a quality certificate. 5.2 The batch size of each batch of 2,4-D butyl ester emulsifiable concentrate products should not exceed the capacity of the packaging storage tank. 5.3 The sampling method shall be carried out in accordance with GB1605.
5.4 The user has the right to verify whether the received 2,4-D butyl ester emulsifiable concentrate meets the requirements of this standard in accordance with the various provisions in the product standard. 5.5 If any index does not meet the standard in the test results, samples should be taken from twice the number of packages for re-testing. If only one index does not meet the requirements, the whole batch of products will be unqualified. 5.6 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation or the legal inspection agency can conduct arbitration analysis in accordance with the inspection methods specified in this standard.
Marking, packaging, transportation and purchase and storage
HG2320-92
6.12,4-D butyl ester emulsifiable concentrate shall be marked and packaged in accordance with the relevant provisions of GB4838. 6.22,4-D butyl ester emulsifiable concentrate shall be packaged in clean and dry glass bottles, with a net weight of 0.5kg or 1.0kg per bottle, covered with straw covers or foam air cushions, and tightly arranged in cartons or calcium plastic boxes, with a net weight of no more than 20kg per box. Other forms of packaging can also be used according to user requirements. All containers for packaging 2,4-D butyl ester emulsifiable concentrate must be dedicated and shall not contain other pesticides. 6.3 During storage and transportation, strictly prevent moisture and sunlight, maintain good ventilation, do not mix with food, seeds, feed, avoid contact with skin, and prevent inhalation through the mouth.
6.4 The validity period is 2 years from the date of manufacture, and all indicators are guaranteed to meet the standard requirements within 2 years. Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard was drafted and technically coordinated by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry, and the 9719 Factory of the Chinese People's Liberation Army participated in the drafting. The main drafters of this standard are Jiang Minyi, Yuan Chunfeng, Li Xiujie, Wang Xuecheng, Mei Baogui, Zhang Zhenhua, and Zhang Daidi.163×100
Wherein: C2——actual concentration of sodium hydroxide standard titration solution, mol/L; V2——volume of sodium hydroxide standard titration solution consumed for titration of free phenol, mL; V'z——volume of sodium hydroxide standard titration solution consumed for titration of blank, mL; m—mass of sample, g;
0.163——mass of 2,4-dichlorophenol equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0H)=1.000mol/], expressed in grams.
4.4 Determination of moisture
Determine according to the Karl Fischer method in GB1600. 4.5 Emulsion stability test
Take 0.5mL sample and determine according to GB1603. No floating oil on the top and no precipitation (or sinking oil) on the bottom is qualified. 4.6 Low temperature stability test
Measure about 100mL of sample into a 150mL beaker, put it in a refrigerator or ice water bath at 0±1℃, leave it for 1h, stir it from time to time, and observe whether there is solid or oily precipitation in the cup. If there is no, it is qualified. 4.7 Hot storage stability test
4.7.1 Apparatus
Constant temperature box or constant temperature water bath;
An: 50mL, long neck;
Syringe: 50mL.
4.7.2 Operating conditions
Use a syringe to inject about 20mL of sample into a clean annular (avoid the sample contacting the neck of the annular), cool the annular in an ice bath, and seal it with a gas lamp. Put the sealed annular in a metal container, and then put the container in a constant temperature box at 54±2℃ (or put the annular in a constant temperature water bath) and store it for 14d. After being taken out of the thermostat (or thermostatic water bath), all inspection items should be completed within 24 hours. After hot storage, all indicators still meet the standard requirements.
5 Inspection rules
5.12,4-D butyl ester emulsifiable concentrate products should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer should ensure that the 2,4-D butyl ester emulsifiable concentrate shipped out of the factory meets the requirements of this standard, and each batch of 2,4-D butyl ester emulsifiable concentrate shipped out of the factory should be accompanied by a quality certificate. 5.2 The batch size of each batch of 2,4-D butyl ester emulsifiable concentrate products should not exceed the capacity of the packaging storage tank. 5.3 The sampling method shall be carried out in accordance with GB1605.
5.4 The user has the right to verify whether the 2,4-D butyl ester emulsifiable concentrate received meets the requirements of this standard in accordance with the various provisions in the product standard. 5.5 If any index does not meet the standard in the test results, samples should be taken from twice the number of packages for re-verification. If only one index does not meet the requirements in the re-verification results, the entire batch of products will be unqualified. 5.6 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation or the statutory inspection agency can conduct arbitration analysis in accordance with the inspection methods specified in this standard.
Marking, packaging, transportation and purchase and storage
HG2320-92
6.12,4-D butyl ester emulsifiable concentrate marking and packaging shall comply with the relevant provisions of GB4838. 6.22,4-D butyl ester emulsifiable concentrate shall be packaged in clean and dry glass bottles, with a net weight of 0.5kg or 1.0kg per bottle, covered with straw covers or foam air cushions, and tightly arranged in cartons or calcium plastic boxes, with a net weight of no more than 20kg per box. Other forms of packaging can also be used according to user requirements. All containers for packaging 2,4-D butyl ester emulsifiable concentrate must be dedicated and must not contain other pesticides. 6.3 During storage and transportation, strictly prevent moisture and sunlight, maintain good ventilation, do not mix with food, seeds, feed, avoid contact with skin, and prevent inhalation through the mouth.
6.4 The validity period is 2 years from the date of manufacture, and all indicators are guaranteed to meet the standard requirements within 2 years. Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard was drafted and technically coordinated by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry, and the 9719 Factory of the Chinese People's Liberation Army participated in the drafting. The main drafters of this standard are Jiang Minyi, Yuan Chunfeng, Li Xiujie, Wang Xuecheng, Mei Baogui, Zhang Zhenhua, and Zhang Daidi.
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