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Chemical Industry Standard of the People's Republic of China
HG/T2218.2—91
Miehailing Aerosol Type B
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 B
Subject Content and Scope of Application
HG/T2218.2—91
This standard specifies the technical requirements, test methods, inspection rules, and requirements for marking, packaging, transportation and storage of Miehailing Aerosol Type B.
This standard applies to Miehailing Aerosol Type B processed from raw materials such as cis-cypermethrin, piperonyl butoxide, and suitable solvents and propellants.
1.1 Active ingredient 1: cis-cypermethrin
Chemical name: (R, S) α-cyano-3-phenoxybenzyl (1R, 3R)-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate Structural formula:
Molecular formula: C22H1gC12NO3
Relative molecular mass: 416.3 (according to the 1987 international relative atomic mass) 1.2 Effective Ingredient 2 Piperonyl butoxide
Chemical name: Oxidized piperonyl butoxide
Structural formula:
Molecular formula: C1gHsoO6
CHCCI2
CH20C2H,0CH,0C,Hg
Relative molecular mass: 338.45 (according to the international relative atomic mass in 1987) 2 Technical requirements
2.1 Appearance: colorless or light yellow homogeneous liquid. 2.2 Miehailing Aerosol Type B shall also meet the following index requirements:
Cis-cypermethrin content, 8/L (25℃)
Piperonyl ether content/L (25℃)
Acidity (as HC1),/L (25℃)
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991>
Implementation on July 1, 1992
W. Atomization rate, % (m/m)
Net capacity, mL
Product pressure (55℃), MPa
Note: 1) See 4.2.
3 Test method
3.1 Determination of cis-cypermethrin and piperonyl ether content 3.1.1 Pretreatment of samples
HG/T2218.2—91
600±6
Take a can of sample, spray the liquid according to the instructions on the can, collect about 50mL of the sample in a 200mL beaker, and pour the collected sample into a 50mL dropper bottle for testing.
3.1.2 Reagents and solutions
a. Stationary liquid: SE-30, 0V-101;
b. Support: ChromosorbW/AW-DMCS (150~180um); c. Cis-cypermethrin standard: known content; d. Piperonyl butoxide standard: known content;
e.α-Cypermethrin (internal standard): should be free of interfering impurities;f. Aviation kerosene or reagent benzene;
g. Cis-Cypermethrin standard solution: weigh 0.16g of cis-Cypermethrin standard (accurate to 0.2mg), place it in a 25mL volumetric flask, and dilute it to the mark with aviation kerosene or reagent benzene. h. Piperonyl butoxide standard solution: weigh 0.14g of Piperonyl butoxide standard (accurate to 0.2mg), place it in a 10mL volumetric flask, and dilute it to the mark with aviation kerosene or reagent benzene.
i.α-Cypermethrin internal standard solution: weigh 1.2g of α-Cypermethrin (accurate to 0.2mg), place it in a 50mL volumetric flask, and dilute it to the mark with aviation kerosene or reagent benzene.
3.1.3 Instruments
a. Gas chromatograph: with hydrogen flame ionization detector; b. Chromatographic column: 4% SE-30 and 4% oV-101 are coated on 150~180um ChromosorbW/AW-DMCS carriers respectively, then mixed in 1+1 and filled in a stainless steel column with a length of 2m and an inner diameter of 4mm; c. Recorder or microprocessor;
d. Micro syringe: luL.
3.1.4 Operation steps
3.1.4.1 Chromatographic operation conditions (taking 102G chromatograph as an example) a. Temperature: column chamber 253℃, detection chamber 255℃, vaporization chamber 270℃; b. Gas flow rate: carrier gas (Nz) 15mL/min. Hydrogen 40mL/min, air 400mL/min; c. Sensitivity: 1000×1/4;
d. Paper speed: 5mm/min;
e. Retention time: piperonyl butoxide 2.4min, cypermethrin 6.6min, α-cypermethrin 8.5min (see figure). 3.1.4.2 Preparation of standard solution
Accurately pipette 2mL of cis-cypermethrin standard solution, piperonyl butoxide standard solution and α-cypermethrin internal standard solution into a 10mL volumetric flask, and dilute to the mark with aviation kerosene or reagent benzene. 2
3.1.4.3 Preparation of sample solution
HG/T2218.2—91
Accurately pipette 2mL of α-cypermethrin internal standard solution into a 10mL volumetric flask, and dilute to the mark with the sample treated in 3.1.1. 3.1.4.4 Determination
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 cis-cypermethrin and α-cypermethrin, peak height or peak area of piperonyl butoxide/α-cypermethrin) until the response ratio changes within 1.0% for two consecutive times; then inject the sample solution twice and measure the 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 cis-cypermethrin content Xi (g/L) shall be calculated according to formula (1): Xi
R·m·P
R·m·PX125
-the average value of the peak height or peak area ratio of cis-cypermethrin to α-cypermethrin in the sample solution; where. R—
the average value of the peak height or peak area ratio of cis-cypermethrin to α-cypermethrin in the standard solution; the mass of cis-cypermethrin in the standard solution, g; P—the percentage of cis-cypermethrin standard; 8——the volume added to the sample, mL.
The content of piperonyl butoxide (g/L) X2 is calculated according to formula (2): Xz
R·m·PiX125
Wherein: R! is the average value of the peak height or peak area ratio of piperonyl butoxide to α-cypermethrin in the sample solution; R1 is the average value of the peak height or peak area ratio of piperonyl butoxide to α-cypermethrin in the standard solution; ml
is the mass of piperonyl butoxide in the standard solution, g; is the percentage of the piperonyl butoxide standard;
is the volume added to the sample, mL.
The parallel deviation of piperonyl butoxide and cis-cypermethrin in this standard should not be greater than 0.1 g/L. Gas chromatogram
1—piperidinol; 2—unknown substance 3—cis-cypermethrin; 4—α-cypermethrin (1)
W.3.2 Acidity determination
3.2.1 Reagents and solutions
HG/T2218.2—91
a. Sodium hydroxide (GB629) standard solution: c(NaOH)=0.05mol/L; b. 95% ethanol (GB679);
c. Phenolic indicator.
3.2.2 Operation steps
Accurately pipette 10mL of the sample treated in 3.1.1, place it in a 250mL conical flask, add 30mL of neutralized ethanol and 5-7 drops of phenolic 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):
X; = 9VX 0. 0365 X1000
Wherein: c——concentration of sodium hydroxide standard solution, mol/L;-volume of sodium hydroxide standard solution consumed in titrating the sample, mL; V
·(3)
0.0365-mass of hydrochloric acid in grams equivalent to 1.00mL sodium hydroxide standard solution [c(NaOH)=1.000mol/L), 10.0-volume of the sample absorbed, mL.
3.3 Determination of atomization rate
After weighing the iron can containing the Miehailing Aerosol Type B, spray the liquid according to the instructions on the can, weigh the iron can and the residual liquid, then open a hole to pour out the residual liquid, and then weigh the empty can. The atomization rate X (%) is calculated according to formula (4):
-the mass of the tank before spraying, g;
where: m—
-the mass of the tank after spraying,;
-the mass of the empty tank, 8.
3.4 Net capacity determination
mi-m2×100
…(4)
Operation steps: Take a can of sample, place it in a fume hood, drill two small holes with a diameter of about 0.2mm on the top of the can (you can hear a sound but no liquid splashes out), let the propellant evaporate slowly, then make the holes larger, pour the liquid into a 1000mL measuring cylinder, and its volume is the net capacity. 3.5 Product pressure determination
3.5.1 Instrument
Pressure gauge 0~1.6MPa.
3.5.2 Determination steps
Take two cans of sample, shake them several times, place them in a fume hood, remove the outer cover, gently break off the safety cover and pull out the nozzle, align the inlet of the pressure gauge with the valve core of the harmless spirit, press hard, and read the indicated pressure of the two cans. The product pressure X is calculated according to formula (5): www.bzxz.net
X. =p+(55-t)× 0.007
Where: p——average value of indicated pressure, MPa; 55——temperature specified in the standard, ℃; 0.007——pressure correction coefficient, MPa/℃; temperature when measuring pressure, ℃.
4 Inspection rules
4.1 The quality supervision and inspection department of the manufacturer shall inspect the type B of the Miehailing Aerosol. The manufacturer shall ensure that all indicators of the products shipped meet the standard requirements. Each batch of the type B of the Miehailing Aerosol shall be accompanied by a quality certificate. 4.2 Atomization rate is a type inspection item and shall be inspected once a week. 4.3 Each batch of the type B of the Miehailing Aerosol shall not exceed the maximum capacity of the preparation kettle. 4.4 Take samples from 0.2% of the packaging of each batch of products, and the number of small batches shall not be less than three boxes; take one can from each packaging box at random, and take approximately equal test samples from each can, with a total amount of not less than 0.25L, for testing the effective ingredients and acidity; testing of other items requires sampling from the original packaging. 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. Even if only one indicator does not meet the requirements as a result of the re-verification, the entire batch of products will be unqualified. 4.7 When the supply and demand parties have objections to the 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 B is packaged in tinplate cans, the deformation pressure of the can is greater than or equal to 1.2MPa, the bursting pressure is greater than or equal to 1.4MPa, and it 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, factory 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's name, factory address, net capacity, prevention and control 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 must not be stored or transported together with food. Be careful and gentle when transporting and loading and unloading. Severe impact is strictly prohibited, and it cannot be inverted. 5.5 The product should be stored in a cool, ventilated and dry place, avoid high temperature, and strictly prohibit exposure to the sun. 5.6 The shelf life of the product is two years if the above storage and transportation conditions are met. 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, Zhang Xiangxing, and Gao Shaoxia. 5
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