Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2465.1-93
Published on July 5, 1993
Acetochlor Technical
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
HG2465.1-93
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage of acetochlor technical. This standard applies to acetochlor technical synthesized by acylation and condensation process with 2,6-methyl-ethylaniline, chloroacetic acid and trioxymethylene as the main raw materials, and shall be free of foreign impurities.
Active ingredient: Acetochlor
Chemical name: 2I-ethyl-6-methyl-N-(ethoxymethyl)-2-chloroacetanilide ISoGeneric name: Acetochlor
Structural formula:
Empirical formula: CiuH20CINO2
CH2—0—C,Hs
COCH,CI
Relative molecular mass: 267.77 (according to the international relative atomic mass in 1989)Biological properties: Herbicide
2 Reference standard
GB 601 Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents GB/T1600 Method for determination of moisture content in pesticides
GB1604 Rules for acceptance of pesticides
5 Sampling method for commercial pesticides
GB1605
GB3796 General rules for pesticide packaging
3 Technical requirements
3.1 Appearance: Brown or purple homogeneous transparent liquid, without visible foreign matter. 3.2 The technical material of acetochlor shall meet the following requirements:%
Acetochlor content
Acidity (in HSO)
Superior quality
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 1993
Qualified quality
Implemented on January 1, 1994
4 Test method
HG 2465.1—93
Unless otherwise specified, the reagents used in this standard are analytically pure reagents, and the 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 acetochlor content. 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/Chromsorb 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 dissolve SE-30 completely, 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. Wait until the solvent evaporates and is almost dry. 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 from the funnel in batches while tapping the column wall continuously to fill the column evenly and tightly. 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
Relative retention value
Acetochlor: 1.00 (about 6min);
Internal standard: 2.00.
HG2465.1-93
Gas chromatogram of acetochlor technical
1—acetochlor; 2—internal standard
The above operating conditions are typical operating parameters. The given operating parameters can be appropriately adjusted according to the characteristics of the instrument to obtain the best effect. 4.1.2.6 Determination steps
a. Preparation of standard solution
Weigh about 0.09g of standard sample (accurate to 0.0001g) containing acetochlor, place it in a 25mL volumetric flask with a stopper, accurately transfer 10mL of internal standard solution with a pipette, 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 volumetric flask with a stopper, accurately transfer 10mL of internal standard solution with a pipette, and shake well.
c. Determination
HG2465.1—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. a. Standard solution; b. Sample solution; c. Sample solution; d. Standard solution. 4.1.2.7 Calculation
Average the measured ratios of the peak areas of acetochlor to the internal standard in a, d and b, c. The mass percentage of acetochlor X1 is calculated according to formula (1):
wherein, a is the average value of the peak area ratio of acetochlor to the internal standard in the standard solution; 2 is the average value of the peak area ratio of acetochlor to the internal standard in the sample solution; m1 is the mass of the standard,;
m2 is the mass of the sample, g;
is the purity of the standard, (%, m/m).
4.1.2.8 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.5%. The average value shall be taken as the reported result. 4.2 Determination of moisture
Determine according to the Karl Fischer method in GB/T1600 4.3 Determination of acidity
4.3.1 Reagents and solutions
Sodium hydroxide (GB629);
Glacial acetic acid (GB676);
Acetone (GB686) redistilled;
Standard sodium hydroxide titrant: c(NaOH)=0.02mol/L, (1)
Buffer solution: Mix 100mL120g/L acetic acid solution and 100mL40g/L sodium hydroxide solution, and dilute 1000mL with water. 4.3.2 Instruments
pH meter: accurate to 0.1, pH meter must have temperature compensation or temperature correction chart; electromagnetic stirring;
Glass electrode: soak in distilled water for 24h before use; saturated calomel electrode.
4.3.3 Analysis steps
4.3.3.1 Using the above-mentioned electrode and pH meter, measure the pH value of a mixture of 50 mL redistilled acetone and 5 mL buffer solution at 20°C.
4.3.3.2 Weigh 10 g of sample (accurate to 0.0.1g) is placed in a 100mL beaker, dissolved in 50mL redistilled acetone, and 5mL of water is added and mixed. Under the same conditions as above, the pH value of the acetone-buffer solution mixture at 20℃ is titrated with sodium hydroxide standard titration solution, which is the end point.
4.3.4 Calculation
The acidity X2 of acetochlor expressed as a mass percentage is calculated according to formula (2): cV×0. 049×100
Wherein: V-the volume of the standard sodium hydroxide solution consumed by the titration sample, mL;-the actual concentration of the standard sodium hydroxide solution, mol/L; m-bzxZ.net
-the mass of the sample, g;
0.049-the mass of sulfuric acid in grams equivalent to 1.00mL of the standard sodium hydroxide solution [c(NaOH)=1.000mol/L) 4
Inspection rules
5.1 Sampling method
HG2465.1-93
According to the sampling method for emulsions and liquids in GB1605. The sampling package shall be determined by random method; the final sampling volume shall not be less than 250mL.
5.2 Acceptance rules
Acceptance shall be carried out in accordance with GB1604.
Marking, packaging, transportation and purchase and storage
6.1 The packaging and marking of acetochlor technical shall comply with the relevant provisions of GB3796 and shall be trademarked. 6.2 During storage and transportation, it shall be strictly prevented from moisture and sunlight, and shall not be mixed with food, seeds, and feed, and shall avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 6.3 Packages shall be stored in ventilated, dry (low temperature) indoor warehouses. The stacking method shall comply with the principles of safety and convenient handling. 6.4 Warranty period: Under the specified storage conditions, the warranty period of acetochlor technical shall be at least 1 year from the date of production. During the warranty period, all indicators shall meet the requirements of this standard.
HG2465.1—93
Appendix A
Gas chromatography determination method for sethoxydim
(Supplement)
A1 The following two methods can be used for production control analysis A1.1 Method I:
A1.1.1 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 filled with 5% sE-30/Chromosorb WAWDMCS (180~250um) and a thermal conductivity cell detector are used to separate and determine sethoxydim by gas chromatography. A1.1.2 Preparation of 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 0.10% of acetochlor respectively (accurate to 0.0001g), place them in two stoppered small glass bottles, add 2mL of internal standard solution to each vial using a pipette, and shake well.
A1.1.3 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. A1.2 Method I:
A1.2.1 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 (180-250um) and a thermal conductivity cell detector were used to separate and determine acetochlor by gas chromatography (peak height quantitative method). A1.2.2 Preparation of standard and sample solutions
a. Internal standard solution
16g hexachlorobenzene xylene solution
b. Standard and sample solutions
Weigh about 0.10g of standard and sample (accurate to 0.0001g) respectively, place them in two small glass bottles with stoppers, and add 5mL of internal standard solution to each vial with a pipette and shake well.
A1.2.3 Chromatographic operating conditions
Column chamber: 200℃;
Vaporization chamber: 300℃;
Detector chamber: 250℃;
Carrier gas (H2) flow rate 60mL/min;
Bridge flow: 150mA;
Injection volume: 4uL;
Retention time: about 5min for hexachlorobenzene; about 8min for acetochlor. 6
Additional Notes:
HG2465.1—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 jurisdiction 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. 73 Chromatographic operating conditions
Column chamber: 200℃;
Vaporization chamber: 300℃;
Detector chamber: 250℃;
Carrier gas (H2) flow rate 60mL/min;
Bridge flow: 150mA;
Injection volume: 4uL;
Retention time: hexachlorobenzene about 5min; acetochlor about 8min. 6
Additional instructions:
HG2465.1—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 technically managed by 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. 73 Chromatographic operating conditions
Column chamber: 200℃;
Vaporization chamber: 300℃;
Detector chamber: 250℃;
Carrier gas (H2) flow rate 60mL/min;
Bridge flow: 150mA;
Injection volume: 4uL;
Retention time: hexachlorobenzene about 5min; acetochlor about 8min. 6
Additional instructions:
HG2465.1—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 technically managed by 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. 7
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