Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2465.2-93
Published on July 5, 1993
Acetochlor EC
Implemented on January 1, 1994
Ministry of Chemical Industry of the People's Republic of China
Chemical Industry Standard of the People's Republic of China
Acetochlor
Subject Content and Scope of Application
HG2465.2-93
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage of acetochlor EC. This standard applies to EC prepared by dissolving acetochlor technical and emulsifier in a suitable solvent. Active ingredient: Acetochlor
Chemical name: 2I-ethyl-6'-methyl-N-(ethoxymethyl)-2-chloroacetanilide ISo Common name: Acetochlor
Structural formula:
Empirical formula: C1H20CINO2
CH20C2H6
COCH,CI
Relative molecular mass: 267.77 (according to the international relative atomic mass in 1989) Biological properties: Herbicide
Cited standard
GB/T1600|| tt||GB/T1601
GB/T1603
GB1604
GB1605
GB4838
3 Technical requirements
Method for determination of moisture content of pesticides
Method for determination of hydrogen ion concentration of pesticides
Method for determination of stability of pesticide emulsions
Pesticide acceptance rules
Sampling method for commercial pesticides
Emulsifiable concentrate pesticide packaging
3.1 Appearance: Brown or purple homogeneous transparent liquid, without visible suspended matter and precipitation. 3.2 Acetochlor emulsifiable concentrate shall meet the following requirements: Item
Acetochlor content, %
Water, %
pH range
Emulsion stability (diluted 200 times)
Low temperature stability\
Thermal stability\bzxZ.net
Note: 1) Test at least once a quarter.
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 199350% emulsifiable concentrate
40% emulsifiable concentrate
Implemented on January 1, 1994
4Test method
HG2465.2—93
Unless otherwise specified, the reagents used in this standard are analytically pure reagents, and water shall meet the third-grade water specifications in GB6682. 4.1 Determination of Acetochlor
4.1.1 Identification Test
This identification test can be carried out simultaneously with the determination of the content of acetochlor. If the relative difference between the retention time of the main (chromatographic) peak of the sample solution and the retention time of the standard solution acetochlor is within 1.5%, it can be confirmed that the active ingredient of the sample is acetochlor. If there is any doubt about the identification using the above method, at least another method should be used for identification. 4.1.2 Determination of Acetochlor Content
4.1.2.1 Method Summary
The sample is dissolved in chloroform, di-n-pentyl phthalate is used as the internal standard, and a stainless steel column filled with 5% SE-30/Chromosorb W-HP and a hydrogen flame ionization detector are used to separate and determine acetochlor by gas chromatography. 4.1.2.2 Reagents and solutions
Acetochlor standard: known content ≥ 98% (m/m); internal standard: di-n-pentyl phthalate, should not contain impurities that interfere with analysis; stationary liquid SE-30;
Carrier: ChromosorbW-HP150180μm (80~100 mesh); internal standard solution: 8g di-n-pentyl phthalate trichloromethane solution. Store in a refrigerator and use only after returning to room temperature. 4.1.2.3 Instruments
Gas chromatograph: with flame ionization detector; chromatographic data processor;
Chromatographic column: 2m×3mm (id) stainless steel column; column filling: 5%SE-30/ChromosorbW-HP (150~180μm); micro-injector: 10uL.
4.1.2.4 Preparation of chromatographic column
a. Coating of stationary liquid
Weigh about 0.5g SE-30 in a 200mL beaker, add a little chloroform, stir with a glass rod to completely dissolve SE-30, then add an appropriate amount of chloroform (the solvent should just immerse the carrier), and stir. Pour the weighed 10g carrier into the above beaker at a time, place the beaker in a 60℃ water bath, and gently shake the beaker from time to time to keep it in a uniform state. When the solvent evaporates to near dryness, place the beaker in a 100℃ oven and dry for 1h.
b. Filling of chromatographic column
Connect a funnel to the inlet end of the clean and dry chromatographic column, wrap a clean gauze at the outlet end, and connect it to the vacuum pump with a clean rubber tube. Turn on the vacuum pump and pour the filler in batches from the funnel while tapping the column wall continuously to fill the column tightly and evenly. Then plug a small ball of glass wool at each end of the column and press it properly to prevent the filler from moving. c. Aging of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, and do not connect the outlet end to the detector for the time being. Raise the temperature to 250℃ in stages at a carrier gas flow rate of about 20mL/min, and age at this temperature for at least 24h. After cooling down, connect the outlet end of the column to the detector. 4.1.2.5 Gas chromatography operating conditions
Column chamber: 215℃;
Vaporization chamber: 280℃;
Detection chamber: 280℃;
Gas flow rate
Carrier gas: (N2) 40mL/min;
Hydrogen: 40mL/min;
Air: 400mL/min;
Injection volume
1.0μL.
Relative retention value
Acetochlor: 1.00 (about 6min);
Internal standard: 2.00.
HG2465.2—93
Gas chromatogram of acetochlor emulsifiable concentrate
1—acetochlor; 2—internal standard
The above operating conditions are typical operating parameters. According to the characteristics of the instrument, the given operating parameters can be appropriately adjusted to obtain the best results. 4.1.2.6 Determination steps
a. Preparation of standard solution
Weigh about 0.09g of standard sample containing acetochlor (accurate to 0.0001g), place it in a 25mL stoppered volumetric flask, use a pipette to accurately transfer 10mL of internal standard solution, and shake well.
b. Preparation of sample solution
Weigh about 0.09g of sample containing acetochlor (accurate to 0.0001g), place it in a 25mL stoppered volumetric flask, use a pipette to accurately transfer 10mL of internal standard solution, and shake well.
c. Determination
HG2465.2—93
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the relative response value of each needle, and when the relative response value of two adjacent needles changes less than 1.2%, perform gas chromatography analysis in the following order: a. Standard solution; b. Sample solution; c. Sample solution; d. Standard solution. 4.1.2.7 Calculation
Average the ratios of the measured ad and bc acetochlor peak areas to the internal standard peak area. The mass percentage of acetochlor X1 is calculated according to formula (1):
Wherein: 1--the average value of the peak area ratio of acetochlor to the internal standard in the standard solution; 2--the average value of the peak area ratio of acetochlor to the internal standard in the test solution; m1--the mass of the standard, g;
m2--the mass of the test sample, g;
w--the purity of the standard, (%, m/m).
4.1.2.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.0%, and the average value shall be taken as the reported result. 4.2 Determination of moisture
Carry out according to the Karl Fischer method in GB/T1600. 4.3 Determination of pH value
Carry out according to the pH meter method in GB/T1601.
4.4 Emulsion stability test
Carry out according to GB/T1603. No floating oil on the top and no precipitation on the bottom is qualified. 4.5 Low temperature stability test
Put 50mL of the sample in a 100mL beaker, cool it to 0±1℃ by appropriate methods, and keep it at this temperature for 1h, stirring it slowly with a glass rod from time to time. No solid or oily matter is precipitated, it is qualified. 4.6 Thermal stability test
4.6.1 Instrument
Constant temperature box (or constant temperature water bath): 54±2℃; long neck bottle, or glass bottle with stopper that can be sealed at 54℃. Medical syringe: 50mL.
4.6.2 Test steps
Use a syringe to inject 30mL of the emulsion sample into a clean anshao (or glass bottle) (avoid the sample from contacting the bottleneck), place the anshao in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (to avoid solvent volatilization). Seal at least 2 bottles and weigh them separately. Put the sealed anshao into a metal container first, and then put the metal container into a 54±2℃ constant temperature box (or water bath) for 14 days. Take out and weigh them separately. If the weight of the sample does not change, inspect the specified items within 24 hours. If it meets the requirements of various indicators, it is qualified. 5 Inspection rules
5.1 Sampling method
Carry out the sampling method for emulsions and liquid states in GB1605. The sampling package is determined by random method, and the final sampling volume should be not less than 250mL.
5.2 Acceptance rules
Acceptance shall be carried out in accordance with GB1604 standards.
6 Marking, packaging, transportation and storage
6.1 The packaging and marking of acetochlor emulsifiable concentrate shall comply with the relevant provisions of GB4838. 4
HG 2465.293
6.2 Acetochlor emulsifiable concentrate shall be packed in clean, dry brown glass bottles with inner and outer covers, with a net weight of 0.5kg per bottle, and straw or corrugated paper as a liner, and tightly arranged in calcium plastic paper boxes, with a net weight of no more than 12kg per box. Other forms of packaging may also be used according to user requirements. 6.3 During storage and transportation, it shall be strictly prevented from moisture and sunlight, and shall not be mixed with food, seeds, and feed, and shall be avoided from contact with skin and eyes, and from inhalation through the mouth and nose. 6.4 Packages shall be stored in ventilated, dry (low temperature) indoor warehouses. The stacking method shall comply with the principles of safety and convenient handling. 6.5 Warranty period: Under the specified storage conditions, the warranty period of acetochlor emulsifiable concentrate shall be at least 2 years from the date of production. During the warranty period, the content of active ingredients and emulsion stability indicators still meet the requirements of this standard. 5
HG2465.2—93
Appendix A
Gas chromatography determination method for acetochlor content
(Supplement)
The following two methods can be used for production control analysis. Method
AI1 Method Summary
The sample is dissolved in acetone, di-n-pentyl phthalate is used as the internal standard, and a 2m stainless steel chromatographic column and a thermal conductivity cell detector are used as the filling material to separate and determine acetochlor by gas chromatography. Preparation of AI2 standard and sample solutions
a. Internal standard solution
50g di-n-pentyl phthalate acetone solution, standard and sample solutions
Weigh the standard and sample containing about 0.10g of sethoxydim (accurate to 0.0001g) respectively, place them in two stoppered small glass bottles, add 2mL of internal standard solution to each vial using a pipette and shake well.
AI3 Chromatographic operating conditions
Column chamber 220℃;
Vaporization chamber: 280℃;
Detector chamber: 250℃;
Carrier gas (H2) flow rate: 40mL/min;
Bridge flow: 170mA;
Injection volume: 4uL:
Retention time: acetochlor about 1min;
Di-n-pentyl phthalate about 3.5min. Method 1
AI1 Method Summary
The sample was dissolved in xylene, hexachlorobenzene was used as the internal standard, and a 2m stainless steel chromatographic column filled with 10% SE-30/101 silanized carrier (180250um) and a thermal conductivity cell detector were used to separate and determine acetochlor by gas chromatography (peak height quantitative method). AI2 Preparation of standard and sample solutions
a Internal standard solution
16g/hexachlorobenzene xylene solution;
Standard and sample solutions
Weigh the standard and sample containing about 0.10g of acetochlor (accurate to 0.0001g) respectively, place them in two small glass bottles with stoppers, add 5mL of internal standard solution to each with a pipette, and shake well.
AI3 Chromatographic operating conditions
Column chamber: 200℃
Vaporization chamber: 300℃;
Detector chamber, 250℃;
Carrier gas (H2) flow rate: 60mL/min;
Bridge flow: 150mA;
Injection volume: 4μL;
Retention time: hexachlorobenzene about 5min;
acetochlor about 8min.
Additional Notes:
HG2465.2—93
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry, and Kunshan Chemical Plant participated in the drafting. The main drafters of this standard are Wang Yufan, Zhang Xuebing, Gu Shunxing, Yuan Weijian, Fan Rong, Pang Guangming, and Yu Yaliang. 70001g), placed in two stoppered glass bottles, add 5mL of internal standard solution to each vial with a pipette, and shake well.
AI3 Chromatographic operating conditions
Column chamber: 200℃
Vaporization chamber: 300℃;
Detector chamber, 250℃;
Carrier gas (H2) flow rate: 60mL/min;
Bridge flow: 150mA;
Injection volume: 4μL;
Retention time: hexachlorobenzene about 5min;
Acetochlor about 8min.
Additional instructions:
HG2465.2—93
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 is under the technical jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and Kunshan Chemical Plant participated in the drafting. The main drafters of this standard are Wang Yufan, Zhang Xuebing, Gu Shunxing, Yuan Weijian, Fan Rong, Pang Guangming and Yu Yaliang.0001g), placed in two stoppered glass bottles, add 5mL of internal standard solution to each vial with a pipette, and shake well.
AI3 Chromatographic operating conditions
Column chamber: 200℃
Vaporization chamber: 300℃;
Detector chamber, 250℃;
Carrier gas (H2) flow rate: 60mL/min;
Bridge flow: 150mA;
Injection volume: 4μL;
Retention time: hexachlorobenzene about 5min;
Acetochlor about 8min.
Additional instructions:
HG2465.2—93
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 is under the technical jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and Kunshan Chemical Plant participated in the drafting. The main drafters of this standard are Wang Yufan, Zhang Xuebing, Gu Shunxing, Yuan Weijian, Fan Rong, Pang Guangming and Yu Yaliang.
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