This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage requirements of thiamethoxam wettable powder. This standard applies to wettable powders made from thiamethoxam technical and suitable adjuvants and fillers. HG 2463.2-1993 25% thiamethoxam wettable powder HG2463.2-1993 Standard download decompression password: www.bzxz.net

Chemical Industry Standard of the People's Republic of China
HG2463.2-93
25% Thiaproxil Wettable Powder
Published on 1993-07-05
Ministry of Chemical Industry of the People's Republic of China
Implemented on 1994-01-01
Chemical Industry Standard of the People's Republic of China
25% Thiaproxil Wettable Powder
Subject Content and Scope of Application
HG2463.2-93
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation, and storage requirements for Thiaproxil Wettable Powder. This standard applies to wettable powders made from Thiaproxil technical material and suitable adjuvants and fillers. Active ingredient: Buprofezin
Chemical name: 2-tert-butylimino-3-isopropyl-5-phenyl-3,4,5,6-tetrahydro-2H,1,3,5-thiadiazin-4-oneStructural formula:
Molecular formula: C16H2N:OS
CH(CHs)2
NC(CHs)s
Relative molecular mass: 305.5 (according to the international relative atomic mass in 1989) 2Reference standard
GB/T1600
Determination method of moisture content in pesticides||tt ||GB/T1601
GB/T1604
Method for determination of hydrogen ion concentration of pesticides
Pesticide acceptance rules
Commercial pesticide sampling methods
GB/T1605
GB3796General rules for pesticide packaging
GB/T5451Method for determination of wettability of pesticide wettable powderMethod for determination of fineness of pesticide powder
HG/T2-896
3Technical requirements
3.1Appearance: Loose fine powder with uniform composition and no lumps. 3.225% thiamethoxam wettable powder should meet the following index requirements. Item
Buprofezin content, %
Water content, %
Suspension rate, %
Fineness (particle size <44μm), %
Wetting time, s
PH value range
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 1993
Implementation on January 1, 1994bzxz.net
4 Test method
4.1 Determination of appearance
Visual inspection.
4.2 Determination of thiazolin content
4.2.1 Summary of method
HG2463.2-93
The sample was extracted with chloroform, dicyclohexyl phthalate or tricosane was used as the internal standard, and thiazolin was separated and determined by gas chromatography using a stainless steel column filled with 5% oV-101/GasChromQ and a hydrogen flame ionization detector. 4.2.2 Reagents and solutions
Buprofezin standard: known content, purity required to be not less than 98.0%; internal standard: dicyclohexyl phthalate (or tricosane), must not contain interfering impurity peaks; stationary phase: 0V-101;
Carrier: GasChromQ, particle size 180~250μm (60~80 mesh); Chloroform:
Internal standard solution: weigh 8g of dicyclohexyl phthalate (or 4g of tricosane) in a 250mL volumetric flask, dissolve it with chloroform, dilute to the scale, and shake well.
4.2.3 Instruments
Gas chromatograph: hydrogen flame ionization detector; chromatographic column: 1000mm×3mm (or 800mm×2mm) stainless steel column, filled with 0V-101/GasChromQ column filling material; chromatographic processor (or recorder, 5mV);
Micro-injector: 10μL.
4.2.4 Operation steps
4.2.4.1 Preparation of chromatographic column
Coating of stationary liquid:
Weigh 0.5g 0V-101 and dissolve it in ether. The amount of ether used should be enough to soak the carrier without too much excess. Add 10g GasChromQ while shaking. Gently shake the beaker from time to time to make the coating even. After the solvent evaporates naturally, put it in an oven at 80-100℃ and bake for 1h.
b. Filling of chromatographic column:
Connect a glass funnel to the inlet of the clean and dry chromatographic column, wrap the outlet with a thin layer of cotton (or 2 layers of gauze), connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, slowly add the prepared filler from the funnel, and gently vibrate the chromatographic column. After the filler is tightly and evenly filled, remove the chromatographic column, plug a small ball of glass wool at the outlet and inlet of the column, and press it appropriately. Aging of chromatographic column:
Connect the inlet of the chromatographic column to the vaporization chamber of the gas chromatograph, do not connect the outlet to the detector for the time being, pass the carrier gas at a flow rate of about 20mL/min, raise the temperature to 240℃ in stages, and age it at this temperature for 24h. 4.2.4.2 Gas chromatography operating conditions
Column chamber: 200℃;
Vaporization chamber: 250℃;
Detection chamber: 250℃;
Gas flow rate
Carrier gas (N2): 30mL/min
Hydrogen: 40mL/min;
Air: 400mL/min;
Injection volume: about 0.6μL;
Retention time
Buprofezin: about 5mins
Tricosane: about 8min;
Dicyclohexyl phthalate: about 10min
HG2463.2—93
The above conditions are the operating parameters of 102G chromatograph. According to different instruments, the operating conditions can be appropriately adjusted to obtain the best effect. 1-Buprofezin; 2-Dicyclohexyl phthalate 4.2.4.3 Determination steps
a. Preparation of standard solution
Weigh 0.08 g (accurate to 0.0001 g) of Buprofezin standard sample into a stoppered glass bottle, and add 5 mL of internal standard solution accurately with a pipette and shake well.
Preparation of sample solution
Weigh a sample containing about 0.08 g of Buprofezin (accurate to 0.0001 g) into a stoppered glass bottle, and add 5 mL of internal standard solution accurately with a pipette and shake well.
Under the above conditions, after the instrument is stable, use a microinjector to first inject several needles of standard solution. When the peak height ratio of two adjacent needles changes less than 1.5%, inject and analyze in the following order: a. standard solution, b. sample solution; c. sample solution, d. standard solution. The change of the peak height ratio of thiazide to the internal standard in the two needles of sample solution and the two needles of standard solution before and after the sample should be less than 1.5%, otherwise the injection needs to be repeated. 4.2.4.4 Calculation
Calculate the average value of the peak height ratio of thiazide to the internal standard in the two needles of sample solution b and c and the two needles of standard solution before and after the sample, and calculate the mass percentage content X1 of thiazide according to formula (1).
Wherein: -
The average value of the peak height ratio of thiazide to internal standard in the sample solution; -The average value of the peak height ratio of thiazide to internal standard in the standard solution; -The mass of the sample, g;
The mass of the standard sample, g;
The mass percentage of the standard sample.
4.2.4.5 Allowable difference
The difference between the results of two parallel determinations should not be greater than 0.5% 4.3 Determination of suspension rate
4.3.1 Instruments and reagents
4.3.1.1 250mL stoppered glass cylinder: The distance between the 0 and 250mL scales should be 2021.5cm, and 4~6cm from the bottom of the stopper.
Glass pipette: 30~40cm long, 5mm inner diameter, 2~3mm inner diameter at the tip, bent upward, with the other end connected to the air source; 4.3.1.3 Constant temperature water bath: (30±1)℃; 4.3.1.4 100mL beaker;
4.3.1.5 Standard hard water: 342mg/L hardness in terms of calcium carbonate, prepared according to the standard hard water preparation method in GB5451.
4.3.2 Determination steps
HG2463.2—93
Accurately weigh 1.0g (accurate to 0.0002g) The sample of thiamethoxam wettable powder was slowly placed in a beaker containing 50mL of standard hard water (30℃±1℃). The beaker was shaken by hand in a circular motion for 2min, 120 times per minute, and the beaker was placed in a (30±1)℃ water bath. After 13min, the suspension was quantitatively transferred to a measuring cylinder with (30±1)℃ standard hard water and diluted to 250mL. The stopper was plugged in. The measuring cylinder was turned upside down 30 times at a speed of 1 time every 2s. The measuring cylinder was placed in a water bath with the stopper opened, avoiding direct sunlight and vibration of the water bath. After standing for 30min, 9/10 of the upper layer of the suspension was extracted with a pipette within 10-15s. Be careful when extracting the liquid, do not shake or stir up the sediment in the measuring cylinder, and ensure that the top of the tube is always a few millimeters below the liquid surface. Use a pipette to accurately add 5mL of internal standard solution and 3mL of chloroform to the measuring cylinder, shake and extract, and determine the mass of thiazinone according to 4.2.4.3 of this standard. The mass percentage of suspension rate X2 is calculated according to formula (2): 10×100(ms-m)
Wherein: ms—the mass of thiazinone in the sample weighed in the prepared suspension, g; m4——the mass of thiazinone in 1/10 of the suspension left in the measuring cylinder, g. 4.4 Determination of fineness
According to the wet sieving method in HG/T2-896.
4.5 Determination of moisture content
According to the azeotropic distillation method in GB/T1600. 4.6 Determination of pH value
According to the pH meter method in GB/T1601.
4.7 Determination of wetting time
According to GB/T5451.
5 Inspection rules
5.1 Sampling method: in accordance with the relevant provisions of GB1605. 5.2 Acceptance rules: follow GB1604 standards. 6 Marking, packaging, transportation, storage
6.1 Marking: should comply with the relevant provisions of GB3796, and add trademarks. 111(msm)
6.2 Packaging: Buprofezin wettable powder is packaged in aluminum-plastic composite bags, with a net weight of 25g, 50g, and 100g per bag. The outer packaging is a calcium plastic box or a cardboard box, with a net weight of 10kg per box; it can also be carried out according to user requirements, but it must comply with GB3796 regulations. 6.3 During transportation and storage, it should be handled with care, strictly prevent moisture and sun and rain, maintain good ventilation, and must not be mixed with food, seeds, and feed. 6.4 Under the specified packaging, storage, and transportation conditions, the warranty period of this product is 2 years (from the date of production), and all technical indicators within 2 years must comply with this standard.
Additional Notes:
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 supervision of Shenyang Chemical Research Institute. This standard was drafted by Jiangsu Pesticide Research Institute. The main drafters of this standard are Wang Yunsheng, Hou Yukai and Lin Shu. 4
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