Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2199—91
Isocarbophos emulsifiable concentrate
Issued on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
W Chemical Industry Standard of the People's Republic of China
Isocarbophos emulsifiable concentrate
Subject content and scope of application
HG2199—91
This standard specifies the technical requirements, test methods, inspection rules, and packaging, marking, transportation and storage of isocarbophos emulsifiable concentrate. This standard applies to isocarbophos emulsifiable concentrate prepared from isocarbophos technical with suitable emulsifiers and solvents. Active ingredient: Azophos
Chemical name: 0-methyl-0-(o-isopropoxycarbonylphenyl)thiophosphoramide Structural formula:
COOCH(CH3)2
Molecular formula: CuH16NO,PS
Relative molecular mass: 289.3 (1987 international relative atomic mass) 2 Reference standard
GB1600
GB1603
GB1604
GB1605www.bzxz.net
GB3796
GB4838
3 Technical requirements
Method for determination of moisture content in pesticides
Method for determination of stability of pesticide emulsions
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
Emulsifiable concentrate pesticide packaging
3.1 Appearance: Bright yellow or dark brown, slightly viscous, transparent, oily liquid. 3.2 Carbofuran emulsifiable concentrate shall meet the following requirements: %(m/m)
Active ingredient content
Acidity (measured in HSO.)
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991>
Implementation on July 1, 1992
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Heat stability)
Low temperature stability)
Note: 1) It is a type inspection item, and the inspection period is half a year. 4 Test method
4.1 Determination of carbofuran content
4.1.1 Summary of method
HG2199-91
%(m/m）
The sample was dissolved in ethyl acetate and determined by gas chromatography on a 5% OV-3 packed column using di-n-butyl sebacate as the internal standard and a hydrogen flame ionization detector.
4.1.2 Reagents and solutions
4.1.2.1 Ethyl acetate (HG3-1226); 4.1.2.2 Azophos standard: known content; 4.1.2.3
Di-n-butyl sebacate: must not contain impurities that interfere with the chromatographic analysis; Stationary phase: 0V-3;
Carrier: 101 silanized white carrier (180~250um); 4.1.2.5
Dimethyldichlorosilane ：For chromatography
4.1.2.7 Internal standard solution: weigh 5g (accurate to 0.0001g) of di-n-butyl sebacate in a 250mL volumetric flask, dissolve and dilute to the mark with ethyl acetate, and mix;
4.1.2.8 Standard sample solution: weigh about 0.2g (accurate to 0.0001g) of carbofuran standard in a 10mL volumetric flask, use a pipette to accurately add 5mL of internal standard solution, dissolve and dilute to the mark with ethyl acetate, and mix. 4.1.3 Instruments
4.1.3.1 Gas chromatograph: with hydrogen flame ionization detector; 4.1.3.2 Chromatographic column: 1m×3mm glass column (or stainless steel column), filled with 5% 0V-3/101 silanized white support (180~250um);
4.1.3.3 Recorder: 5mV (or data processor); 4.1.3.4 Micro-injector: 5uL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
4.1.4.1.1 Coating of stationary liquid: Weigh 0.5g 0V-3 stationary liquid, put it in a 200mL beaker, add about 30mL chloroform, stir with a glass rod to completely dissolve 0V-3. Then add 10.0g of 101 silanized white support, shake the beaker gently by hand to make the support completely immersed in the solution, place the beaker under an infrared lamp to heat, shake the beaker while heating, until the solvent evaporates and is almost dry, then place it in a 120℃ oven to dry for 2 hours, take it out and put it in a desiccator for use.
4.1.4.1.2 Silanization treatment of glass column (or stainless steel column) and glass lining of vaporization chamber: inject 5% silanization reagent (DMCS) toluene solution into an empty, clean, dry glass column and lining, soak for 15 minutes, release the silanization reagent toluene solution, wash the column and lining with toluene, methanol and distilled water in turn, and finally wash with acetone, and dry it in a 110℃ oven for 2 hours. 4.1.4.1.3 Filling of chromatographic column: connect a small funnel to the inlet end of the silanized and dried glass column (or stainless steel column), wrap the outlet end with gauze, and connect it to the vacuum pump with a rubber tube. Turn on the vacuum pump and add the column filler from the funnel in batches while tapping the column wall continuously to fill the column evenly and tightly. Remove the column and plug both ends of the column with an appropriate amount of silanized glass wool. 2
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4.1.4.1.4 Aging of the column: Connect the inlet end of the column to the vaporization chamber, and temporarily do not connect the outlet end to the detector. Raise the temperature to 260°C in stages at a carrier gas flow rate of about 15mL/min, and age at this temperature for at least 24h. After cooling, connect the outlet end of the column to the detector. 4.1.4.2 Chromatographic operating conditions
Temperature:
Column chamber 210℃;
Vaporization 270℃,
Gas flow rate:
Carrier gas (N2)
60mL/min,
45mL/min;
Hydrogen (H2)
Air 450mL/min;
Attenuation:
16×102 (data processor 4×10)
Paper speed:
2.5mm/min (data processor 2mm/min)Injection volume:
Retention time:
About 6.1min for isothiocarb, and about 9.5min for internal standard. Gas chromatogram of chlorpyrifos emulsifiable concentrate
1 chlorpyrifos monohydrate; 2 di-n-butyl sebacate 3
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The above chromatographic operating conditions are typical conditions for GC-7A gas chromatograph. Appropriate adjustments can be made for different types of instruments to obtain the best results.
4.1.4.3 Preparation of sample solution
Weigh about 0.2g of chlorpyrifos emulsifiable concentrate sample (accurate to 0.0001g) in a 10mL volumetric flask, accurately add 5mL of internal standard solution with a pipette, dilute to the mark with ethyl acetate, and mix well. 4.1.4.4 Determination
After the instrument is stable, repeatedly inject 0.6uL of isothiocarb standard solution until the ratio of the response values of two adjacent needles (ratio of isothiocarb peak area/internal standard peak area) is basically stable (its change is within 2.5%), and then analyze in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution,
d. Standard solution.
4.1.4.5 Calculation:
Average the response values of a, d and b, c, and calculate the mass percentage of chlorpyrifos in the sample X1 according to formula (1): X
.mi·u
Where: 1-average value of the response value ratio of chlorpyrifos to the internal standard in the standard solution: 12-average value of the response value ratio of chlorpyrifos to the internal standard in the sample solution, m1-weighing amount of chlorpyrifos standard sample, gm2
weighing amount of chlorpyrifos sample, g
mass percentage of chlorpyrifos standard sample. 4.1.5 Allowable difference
The difference between the results of the second determination should not exceed 1.5%. 4.2 Determination of water content
Determine according to the Karl Fischer method in the GB1600 method for determining water content in pesticides. 4.3 Acidity determination
4.3.1 Reagents and solutions
4.3.1.1 Sodium hydroxide (GB629): standard titration solution c(NaOH) = 0.02 mol/L4.3.1.2 Anhydrous ethanol (GB678)
4.3.1.3 0.1% bromophenol blue indicator solution: weigh 0.100 g bromophenol blue, dissolve it in ethanol, and dilute it to 100 mL with ethanol. 4.3.2 Operation steps
Weigh 2~3 g sample (accurate to 0.001g) was placed in a 150mL conical flask, 20mL of anhydrous ethanol was added, 3 drops of bromophenol blue indicator solution were titrated with sodium hydroxide standard titration solution until the blue color was reached, which was the end point. At the same time, a blank determination was performed. 4.3.3 Calculation
The acidity X2 of carbofuran emulsifiable concentrate expressed in mass percentage shall be calculated according to formula (2): X2=g(V1-V2)×0. 049×100
Wherein: c——actual concentration of sodium hydroxide standard titration solution, mol/L; V1——volume of sodium hydroxide standard titration solution consumed when titrating the sample, mL, 4
(2)
W.HG2199—91
V2——volume of sodium hydroxide standard titration solution consumed when titrating the blank, mL, m——sample weight, g,
0.049——mass of sulfuric acid equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L), expressed in grams.
4.4 Determination of emulsion stability
According to the GB1603 pesticide emulsion stability determination method, the dilution ratio is 500 times. The constant temperature water bath temperature is controlled at 30±1℃. 4.5 Thermal storage stability test
4.5.1 Instrument
4.5.1.1 Oven or water bath: temperature control accuracy is 54±2℃; 4.5.1.2 Ampoule: capacity is about 50mL, long neck. 4.5.2 Determination
Pour about 30mL of sample into a clean ampoule, seal it with a gas lamp, place it in a 54±2℃ oven or water bath, and store it for 14 days. The relative decomposition rate of the active ingredient of the sample after thermal storage is no more than 10% compared with that before thermal storage. 4.6 Low temperature stability test
4.6.1 Instrument
Ice water bath or refrigerator: control the temperature to 0±1℃4.6.2 Operation steps
Take about 50mL of sample in a 100mL beaker, put it in a refrigerator or ice water bath, keep the temperature at 0±1℃, and place it for 1h. During the placement period, stir it once every 15min, and stir for 0.5min each time. Then observe whether there is solid or oily matter precipitated in the cup. If not, it is qualified. 5 Inspection rules
5.1 Carry out in accordance with GB1604 pesticide acceptance rules. Within the two-year warranty period, the mass percentage of isocarbophos shall not be less than 90% of the marked content.
5.2 Carry out in accordance with GB1605 regulations
5.3 The performance of this product is equivalent to the 40% isocarbophos emulsifiable concentrate analyzed by the original chemical method. 6 Packaging, marking, transportation and storage
6.1 The packaging and marking of carbofuran emulsifiable concentrate shall comply with the relevant provisions of GB3796 and GB4838. 6.2 During transportation and storage, carbofuran emulsifiable concentrate must be kept dry, ventilated, and protected from moisture and sunlight, and must not be mixed with food, seeds, feed, etc.
Additional instructions:
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 Qingdao Second Pesticide Factory. The main drafters of this standard are Chen Jianli, Xu Zhenhuan, Sun Siping, and Zhang Qizhong. 5
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