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Chemical Industry Standard of the People's Republic of China
HG/T2218.4—91
Miehailing Aerosol Type E
Published 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
Miehailing Aerosol Type E
Subject Content and Scope of Application
HG/T2218.4—91
This standard specifies the technical requirements, test methods, inspection rules, and requirements for marking, packaging, transportation and storage of Miehailing Aerosol Type E.
This standard applies to Miehailing Aerosol Type E processed from cypermethrin, cypermethrin, suitable solvents and propellants.
1.1 Active ingredient 1: Cypermethrin
Chemical name: α-cyano-3-phenoxybenzyl (R·S)-2-(4-chlorophenyl)-3-methylbutyrate Structural formula:
CH(CHs)2
Molecular formula: C25H22CINO3
Relative molecular mass: 419.9 (according to the international relative atomic mass in 1987) 1.2 Active ingredient 2 Cypermethrin||t t||Chemical name: α-cyano-3-phenoxybenzyl (IR·S)-3-(2,2-dichlorovinyl) 2,2-dimethylcyclopropanecarboxylate Structural formula:
Molecular formula: C22H1gNOgCl2
CH=CCl2
Relative molecular mass: 416.3 (according to the international relative atomic mass in 1987) 2 Technical requirements
2.1 Appearance: colorless or light yellow transparent liquid. 2.2 Miehailing Aerosol Type E shall also meet the following index requirements: Index
Cypermethrin content 8/L (25℃）
Cypermethrin content g/L (25℃)
Acidity (as HC1): g/L
Atomization rate, % (m/m）
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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Product pressure MPa, (55℃)
Note 1) See 4.2.
3 Test method
3.1 Determination of cypermethrin and fenvalerate content 3.1.1 Pretreatment of test sample
HG/T2218.4—91
600±6
Take a can of sample and place it in a fume hood. Chisel two small holes with a diameter of about 0.2mm on the top of the can (you can hear the sound of propellant overflowing but no liquid splashing), let the propellant evaporate slowly, then make the holes larger and pour out the liquid for inspection. 3.1.2 Reagents and solutions
Fixed liquid: SE-30, 0V-101;
Carrier: Chromosorb W/AW-DMCS (150~180um); b.
Cypermethrin standard: known content;
Cypermethrin standard: known content;
Dicaprylyl phthalate: analytical grade;
Jet fuel or reagent benzene;
Cypermethrin standard solution: weigh 0.18 cypermethrin standard g (accurate to 0.2 mg) and placed in a 25 mL volumetric flask, diluted to scale with aviation kerosene or reagent benzene;
h. Cypermethrin standard solution: weigh 0.23 g (accurate to 0.2 mg) of cypermethrin standard and place in a 25 mL volumetric flask, diluted to scale with aviation kerosene or reagent benzene;
Dicetyl phthalate internal standard solution: weigh 1.2 g (accurate to 0.2 mg) of dicetyl phthalate and place in a 100 mL volumetric flask, diluted to scale with aviation kerosene or reagent benzene. 3.1.3 Instruments
a. Gas chromatograph: with hydrogen flame ionization detector; chromatographic column: 4% SE-30, 4% oV-101 coated on 150~180μm ChromosorbW/AW-DMCS carrier respectively, b.1
then mixed in 1+1 ratio and filled in a stainless steel column with a length of 2m and a diameter of 4mm; recorder (5mV) or data processor;
micro syringe: 1uL.
3.1.4 Operation steps
3.1.4.1 Chromatographic operation conditions (taking 102G chromatograph as an example) a.
Temperature: column 260℃, detection chamber 270℃, vaporization chamber 290℃; gas flow: carrier gas (N2) 20mL/min, hydrogen 40mL/min, air 500mL/min; sensitivity: 1000;
Attenuation: 1/4;
Paper speed: 5mm/min;
fRetention time: cypermethrin 4.3min, fenvalerate 5.7min, internal standard 8.85min (see figure). 3.1.4.2 Preparation of standard solution: Accurately pipette 2mL each of cypermethrin standard solution, fenvalerate standard solution and didecyl phthalate internal standard solution, place in a 10mL volumetric flask, dilute to scale with aviation kerosene or reagent benzene, shake well for later use. 3.1.4.3 Preparation of sample solution: Accurately pipette 2mL of didecyl phthalate internal standard solution into a 10mL volumetric flask, dilute to the mark with the sample treated in 3.1.1, and shake for later use. 2
3.1.4.4 Determination
HG/T2218.4—91
After the instrument is stable, first repeatedly inject 0.6uL of standard solution, and measure the response ratio each time (peak height or peak area of cypermethrin/didecyl phthalate, peak height or peak area of fenvalerate/didecyl phthalate), until the response ratio changes within 1.0% for two consecutive times. Then inject the sample solution twice and measure its average response ratio R, then inject the standard solution, and measure the average response ratio R1 of the standard solution before and after the injection of the sample solution.
3.1.4.5 Calculation
The cypermethrin content X, (g/L) is calculated according to formula (1): Xi = Rm·P,
P×1000=R·mPX125
Wherein: R is the average value of the peak height or peak area ratio of cypermethrin to didecyl phthalate in the sample solution; R1 is the average value of the peak height or peak area ratio of cypermethrin to didecyl phthalate in the standard solution; m
8 is the mass of cypermethrin in the standard solution, mL;
P is the percentage of cypermethrin standard. The cypermethrin content (g/L) X2 is calculated according to formula (2): X2-
R'.m'·PIX125
-the average value of the peak height or peak area ratio of cypermethrin to didecyl phthalate in the sample solution; where .R!
R1-the average value of the peak height or peak area ratio of cypermethrin to didecyl phthalate in the standard solution; m-the mass of cypermethrin in the standard solution, g; PI-the percentage content of cypermethrin standard. The deviation of the parallel determination results of this method should not exceed 0.05g/L. 3.2 Acidity determination
3.2.1 Reagents and solutions
3.2.1.1 Sodium hydroxide (GB629) standard solution: c(NaOH)=0.02mol/L; 3.2.1.2 95% ethanol (GB679);
3.2.1.3 Phenol indicator.
3.2.2 Operation steps
Accurately pipette 25mL of the sample treated in 3.1.1, place it in a 250mL conical flask, add 60mL of neutralized ethanol and 5 drops of phenolphthalein indicator, and titrate with sodium hydroxide standard solution until it turns slightly red. 3.2.3 Calculation
Acidity X: (g/L) Calculate according to formula (3):
Xs=o.VX0.0365X1000
Wherein: c—concentration of sodium hydroxide standard solution, mol/L; volume of sodium hydroxide standard solution consumed by titrating the sample, mL; (3)
0.0365—mass of hydrochloric acid in grams equivalent to 1.00mL sodium hydroxide standard solution [c(NaOH)=1.000mol/L]. 3.3 Determination of atomization rate
Weigh the tinplate can containing the E-type Miehailing Aerosol (accurate to 0.01g), follow the instructions on the can, spray the liquid, weigh the tinplate can and the residual liquid, then open a hole to pour out the residual liquid, and weigh the empty can again. 3
HG/T2218.4—91
Gas chromatogram
1-Jet fuel; 2-Cypermethrin; 3-Cypermethrin; 4-Internal standard atomization rate X (%) is calculated according to formula (4):
-Mass of the tank before spraying, nom;
Wherein: m1-
-Mass of the tank after spraying, nom;
Mass of the empty tank, nom.
3.4 Net capacity determination
Operation steps: Take a can of sample and place it in a fume hood. Cut two small holes with a diameter of about 0.2mm on the top of the can (you can hear the sound of the propellant overflowing but no liquid splashing out), let the propellant evaporate slowly, then make the hole larger, pour the liquid into a 1000mL measuring cylinder, and the liquid volume is the net capacity.
3.5 Determination of product pressure
3.5.1 Instrument
Pressure gauge 0~1.6MPa.
3.5.2 Determination stepswwW.bzxz.Net
Take two can samples, shake them several times and place them in a fume hood, remove the outer cover, gently twist off the plastic safety cover and pull out the nozzle, align the inlet of the pressure gauge with the valve core on the top of the tank, press hard, read the indicated pressure of the two tanks, and the product pressure Xs is calculated according to formula (5): Xp×(55-t)×0.007
Where: p—average value of indicated pressure, MPa; 55——temperature specified in the standard, ℃; t——temperature during measurement, ℃;
0.007——pressure correction factor, MPa/℃. 4 Inspection rules
(5)
4.1 The E-type Miehailing Aerosol shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all indicators of the products shipped meet the standard requirements. Each batch of E-type Miehailing Aerosol shall be accompanied by a quality certificate. 4.2 Atomization rate is a type inspection item and is inspected once a week. 4.3 The quantity of each batch of E-type Miehailing Aerosol shall not exceed the maximum capacity of the preparation kettle. 4.4 Samples shall be taken from 0.2% of the packaging of each batch of products. For small batches, no less than three boxes shall be taken; one can is randomly taken from each packaging box, and approximately equal samples are taken from each can, with a total amount of no less than 0.25L for testing. Random sampling can be used for testing of other items. 4.5 The user has the right to verify whether the received products meet the requirements of this standard in accordance with the provisions of this standard. 4.6 In the test results, if some indicators do not meet the standards, samples should be taken from twice the amount of packaging for re-verification. If only one indicator does not meet the requirements, the whole batch of products will be unqualified. 4.7 When the supply and demand parties have disputes over product quality and cannot resolve them through negotiation, the statutory inspection agency shall conduct arbitration analysis according to the inspection methods specified in this standard.
5 Marking, packaging, transportation and purchase and storage
5.1 Miehailing Aerosol Type E is packaged in tinplate cans with a deformation pressure greater than or equal to 1.2MPa and a burst pressure greater than or equal to 1.4MPa, and is equipped with a plastic cover. The net capacity of each can is 600mL. Every 24 cans of products are tightly arranged in a cardboard box, and the net weight of each box does not exceed 15kg; other forms of packaging can also be used according to user requirements. 5.2 Each box of packaging should be printed with the manufacturer's name, address, product name, specifications, production date, standard number, and drug, fire prevention and other signs, and each box is accompanied by a quality certificate.
5.3 The surface of each can is printed with the product name, manufacturer name, factory address, net capacity, prevention and treatment targets, usage methods, precautions, registration certificate number, production license number, active ingredients, production date, and drug, fire prevention and other signs. 5.4 Storage and transportation shall be carried out in accordance with the "Dangerous Goods Transportation Rules" of the Ministry of Transport; this product shall not be stored or transported together with food, and transportation and loading and unloading shall be handled with care and gentleness, violent impact is strictly prohibited, and it shall not be inverted. 5.5 This product should be stored in a cool, ventilated and dry place, avoid being close to high temperatures, and exposure is strictly prohibited. 5.6 The shelf life of the product is two years under the above storage and transportation conditions. Additional notes:
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 Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Industry Research Institute and Zhongshan Fine Chemical Industry Co., Ltd. The main drafters of this standard are Ye Guo, Wu Zhijian, Yang Shaozong, Pan Changrong, and Wu Bingxiang. 5
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