Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2214—91
50% fenvalerate EC
Published on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
Chemical Industry Standard of the People's Republic of China
50% fenvalerate EC
Subject Content and Scope of Application
HG2214—91
This standard specifies the technical requirements, inspection methods, inspection rules and marking, packaging, transportation and storage of 50% fenvalerate EC. This standard applies to 50% fenvalerate EC composed of fenvalerate technical, emulsifier and solvent. Active ingredient: fenvalerate
Chemical name; S-(4-chloro) N,N-diethylthiocarbamate. Structural formula:
Molecular formula: C1HNOSCI
Relative molecular mass: 257.78 (according to the international relative atomic mass in 1987) Cited standards
GB1600
GB1601
GB1603
GB1604
GB1605
GB4838
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: Pale yellow or brownish yellow homogeneous liquid. 3.250% fenvalerate emulsifiable concentrate shall meet the following index requirements: Item
fenvalerate content, %(m/m)
Water content, %(m/m)
Emulsion stability (diluted 200 times)
Hot storage stability
Cold storage stability
Note: 1) and 2) are type inspection items.
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991 N
Implemented on July 1, 1992
4 Test method
4.1 Determination of chlorpyrifos content
4.1.1 Summary of method
HG2214-91
The sample was dissolved in anhydrous ethanol, di(2-ethylhexyl) succinate was used as the internal standard, and chlorpyrifos was separated and quantified using a chromatographic column filled with 5% DEGA/chromosorbW·AW-DMCS and a hydrogen flame ionization detector. 4.1.2 Reagents and solutions
Trichloromethane (GB682); analytical grade;
Absolute ethanol (GB678); analytical grade;
Granumidil standard: known content;
Diisooctyl succinate (or dipropylene phthalate): internal standard (no impurities interfering with the analysis); Diethylene glycol adipate (DEGA): chromatographic stationary liquid (imported, maximum operating temperature 210°C). ChromosorbW·AW-DMCS, 150~180μm (80~100 mesh) chromatographic carrier; Internal standard solution: weigh 8g of diisooctyl succinate (accurate to 0.0002g) and place it in a 100mL volumetric flask, dilute to the mark with anhydrous ethanol and shake well.
4.1.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector; Chromatographic column: 1m long, 4mm inner diameter stainless steel column, filled with 5% DEGA/chromosorbW·AW-DMCS, 150~180μm (80~100 mesh) filler;
Micro syringe: 10uL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
a. Coating of stationary liquid: Weigh 1.00g of diethylene glycol adipate and place it in a 200mL beaker, add 60mL of chloroform to dissolve it, and slowly pour 20g of dry chromosorbW·AW-DMCS150~180um (80~100 mesh) carrier into it to completely immerse the carrier. Place the beaker in a fume hood and slowly evaporate the solvent under an infrared lamp until it is dry (the beaker should be tapped and rotated frequently to ensure that it is evenly coated). Then move it to a 90~100℃ oven and dry it for 30 minutes.
b. Filling of the chromatographic column: Connect a small funnel to the inlet of the cleaned and dried stainless steel column, fill the outlet with an appropriate amount of glass wool and wrap it with gauze, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, slowly pour the filler from the funnel, and tap the column wall continuously to make the filler fill the chromatographic column evenly and tightly. Remove the chromatographic column, plug the glass wool at the inlet, and press it appropriately to keep the filler from moving. c. Aging of the chromatographic column: Connect the inlet of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the outlet to the detector for the time being. Raise the temperature to 190℃ in stages at a nitrogen flow rate of about 10mL/min, and age it at this temperature for 24 hours. After cooling down, connect the outlet of the column to the detector.
4.1.4.2 Gas chromatography operating conditions
Temperature:
Column chamber 180℃;
Vaporization chamber 250℃;
Detection chamber 250℃.
Gas flow rate:
Carrier gas (N2) 60mL/min;
Hydrogen 45mL/min;
Air 500mL/min.
Injection volume:
0.6~0.8uL.
Retention time:
HG2214—-91
About 11.5min for fenvalerate, about 9.5min for o-fenvalerate; about 6.0min for internal standard diisooctyl succinate (about 6.5min for dipropylene phthalate). Gas chromatogram of fenvalerate emulsifiable concentrate
1-internal standard; 2-orthofenvalerate; 3-fenvalerate The above chromatographic conditions are typical conditions of SP-501 gas chromatograph. Appropriate adjustments can be made for different types of instruments to obtain the best results. 4.1.4.3 Preparation of standard solution
Weigh 0.13g of fenvalerate standard (accurate to 0.0002g) and place it in a sample bottle. Use a 1mL pipette to accurately add 1mL of internal standard solution and shake it thoroughly.
4.1.4.4 Preparation of sample solution:
Weigh 0.28g of fenvalerate emulsifiable concentrate (accurate to 0.0002g) and place it in a sample bottle. Use a 1mL pipette to accurately add 1mL of internal standard solution and shake it thoroughly.
4.1.4.5 Determination
After the instrument is stable, inject several needles of standard solution until the peak height ratio of two adjacent needles does not change by more than 1.5%, and then perform the analysis in the following order:
a. Standard solution;
b. Sample solution;
c. Sample solution;
Standard solution.
Use a micro syringe to inject 0.6-0.8uL each time. On the chromatograms of the two needles of sample solution and the two needles of standard solution before and after the sample, the difference between the peak height ratio of Hexachloran 3
HG2214-91
and the internal standard divided by the average value should not be more than 1.5%, otherwise, the injection needs to be repeated. 4.1.5 Calculation
Average the obtained peak height ratios of a, d and b, c, respectively, and calculate the mass percentage of fenpyrocarb X1 according to formula (1): 2·mi·w
-the average value of the peak height ratios of fenpyrocarb and internal standard on the chromatogram of the standard solution;
-the average value of the peak height ratios of fenpyrocarb and internal standard on the chromatogram of the sample solution; m1-the mass of fenpyrocarb standard, g;
m2-the mass of fenpyrocarb sample, g;
-the mass percentage of fenpyrocarb standard.
4.1.6 Allowable difference
The difference between the results of two parallel determinations should not be greater than 1.0%. 4.2 Determination of moisture
According to the Karl Fischer method in GB1600bzxZ.net
4.3 pH determination
According to the pH meter method in GB1601 Pesticide hydrogen ion concentration determination method. 4.4 Emulsion stability determination
Take 0.5mL of sample and carry out the determination according to GB1603 pesticide emulsion stability determination method, with a dilution factor of 200 times. 4.5 Thermal storage stability
4.5.1 Instrument
4.5.1.1 Constant temperature box: temperature control accuracy is 54±2℃4.5.1.2 Ampoule: capacity is about 20mL, long neck. 4.5.2 Determination
Take 10mL of sample and inject it into a clean ampoule, seal it with a blowtorch, and store it in a constant temperature box at 54±2℃ for two weeks. After taking it out, cool it to room temperature, shake it well and set it aside. Take an appropriate amount of the same sample as the pre-storage sample, and measure the content of fenvalerate before and after hot storage, and calculate the fenvalerate decomposition rate according to formula (2): decomposition rate fenvalerate content before hot storage minus fenvalerate content after hot storage 100%. The fenvalerate content before hot storage
The fenvalerate decomposition rate after hot storage should not be greater than 3%. 4.6 Cold storage stability
4.6.1 Instruments
Refrigerator: Temperature control accuracy is 0±1℃
4.6.2 Determination
.......(2)
Take 100mL of sample into a 100mL stoppered measuring cylinder and store it in a refrigerator at 0±1℃ for 1h. Stir it every 15min. If there is no precipitate or stratification, it is qualified. The sample is stored in a refrigerator at 0±1℃ for one week. The appearance of the emulsion is still homogeneous. 5 Acceptance rules
5.1 Follow GB1604.
5.2 Sampling method:
Follow GB1605.
5.3 Hot storage stability and low temperature stability are type inspection items. The inspection cycle is half a year. 6 Marking, packaging, transportation and purchase and storage
6.1 Packaging and marking shall be carried out in accordance with the provisions of GB4838 for packaging of emulsifiable pesticides. 4
HG 2214—91
During storage and transportation, strictly prevent sun and rain, maintain good ventilation, and stay away from fire sources. The railway transportation code is 61040. It is forbidden to mix with food, seeds6.2
and feed during storage and transportation. Avoid contact with skin and prevent inhalation through the mouth and nose. 6.3 Under normal storage conditions, the warranty period of this product is two years. After years, the content of chlorpyrifos shall not be less than 48% within two 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 is under the jurisdiction of the Pesticide Standardization Office of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Hunan Chemical Industry Research Institute, and Zhuzhou Chemical Plant participated in the drafting. The main drafters of this standard are Hong Lizhen, Xiang Yuanying, Yang Fangbin, Tang Xinkai, and Wei Guizhen. 5
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