Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2463.1—93
Buprofezin technical
Published on July 5, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1994
Chemical Industry Standard of the People's Republic of China
Buprofezin technical
Subject content and scope of application
HG 2463.1—93
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements of Buprofezin technical. This standard applies to Buprofezin technical prepared by condensation of N-chloromethyl-N-phenyl-carbamoyl chloride and 1-isopropyl-3-tert-butylthiourea.
Active ingredient: Buprofezin
Chemical name; 2-tert-butylimino-3-isopropyl-5-phenyl-3,4,5,6-tetrahydro-2H-1,3,5-thiadiazin-4-one Structural formula:
Molecular formula: C16H23NOS
CH(CHs)2
=NC(CHa)3
Relative molecular mass: 305.5 (according to the international relative atomic mass in 1989) 2 Reference standards
GB/T1604 Pesticide acceptance rules
GB/T1605 Commercial pesticide sampling method
GB3796 General rules for pesticide packaging
3 Technical requirementsWww.bzxZ.net
3.1 Appearance: off-white or light yellow crystalline powder. 3.2 The technical material of thiazide shall meet the following index requirements: Item name
Thiazide content, %
Loss on drying, %
Acidity (in H2SO4) or alkalinity (in NaOH), %4 Test method
4.1 Determination of appearance
Visual inspection.
4.2 Determination of thiazolin content
4.2.1 Summary of method
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 1993 as superior product
First-class product
Qualified product
Implemented on January 1, 1994
HG2463.1-93
The sample was dissolved in 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 impurities that interfere with the analysis; stationary phase: 0V-101;
Carrier: GaschromQ (particle size 180~250μm 60~80 mesh); chloroform;
Internal standard solution: weigh 8g dicyclohexyl phthalate (or 4g 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 5% oV-101/GaschromQ column filler;
Chromatographic processor (or recorder, 5mV); micro-injector: 10μL.
4.2.4 Operation steps
4.2.4.1 Preparation of chromatographic column
a Coating of stationary liquid:
Weigh 0.5g OV-101 and dissolve it in ether. The amount of ether used should be enough to wet the carrier without too much excess. Add 10g GaschromQ while shaking, and gently shake the beaker from time to time to make the coating uniform. After the solvent evaporates naturally, put it in an oven at 80-100℃ 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 respectively, and press it appropriately. c. 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℃;
Air flow rate
Carrier gas (N2): 30mL/min
Hydrogen: 40mL/min;
Air: 400mL/min
Injection volume: about 0.6uL;
Retention time
Buprofezin: about 5min;
Tricosane: about 8min
Dicyclohexyl phthalate: about 10min. 2
HG 2463.1—93
The above conditions are the operating parameters of 102G chromatograph. According to different instruments, the operating conditions can be adjusted appropriately to obtain the best effect. 4.2.4.3 Determination steps
a. Preparation of standard solution
Weigh 0.08g (accurate to 0.0001g) of thiamethoxam standard into a stoppered glass bottle, and add 5mL of internal standard solution accurately with a pipette and shake well.
Preparation of sample solution
Weigh a sample containing approximately 0.08g of thiamethoxam (accurate to 0.0001g) into a stoppered glass bottle, and add 5mL of internal standard solution accurately with a pipette and shake well.
1—Buprofezin; 2—Dicyclohexyl phthalate c. Determination
Under the above conditions, after the instrument is stable, use a microinjector to first inject several needles of standard solution. When the change in the peak height ratio of two adjacent needles is 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 in the peak height ratio of buprofezin 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 thiazinone to the internal standard substance in the two sample solutions b and c and the two standard solutions a and d before and after the sample, respectively. The mass percentage X of thiazinone is calculated according to formula (1): Xi
Where:
the average value of the peak height ratio of thiazinone to the internal standard substance in the sample solution; ↑2—the average value of the peak height ratio of thiazinone to the internal standard substance in the standard solution; the mass of the sample, 8;
—the mass of the standard sample, 8,
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 1.5%. 4.3 Loss on drying
In a (70±2)℃ oven, dry a culture III with a diameter of about 7 cm for 1 hour, take it out, place it in a desiccator and cool it to room temperature, and weigh it. (1)
Take about 5g of sample, crush the lumps in it, spread it into a thin layer in culture III, weigh it accurately (accurate to 0.0001g), place the culture dish in an oven, and dry it at (70±2)℃ for 1.5h. Take out culture III, cool it to room temperature in a desiccator, and weigh it again. The drying loss X2 (%, m/m) is calculated according to formula (2).
Xs=m-(m=-ml)× 100
Where: m2——mass of culture blood and dried sample, g; m——mass of culture blood, g;
mass of sample, g.
4.4 Determination of acidity or alkalinity
4.4.1 Reagents and solutions
(2)
Acetone (GB686);
HG2463.1-93
Sodium hydroxide (GB629) standard titration solution: c(NaOH)=0.02mol/L; hydrochloric acid (GB622) standard titration solution: c(HCI)=0.02mol/L; mixed indicator solution: a mixture of 2mL 0.1% methyl red ethanol solution and 10mL 0.1% bromocresol green ethanol solution. 4.4.2 Determination steps
Weigh 2g of sample (accurate to 0.0002g), place it in a 250mL conical flask, add 50mL acetone, add 5-6 drops of mixed indicator solution, and titrate to the end point with 0.02mol/L sodium hydroxide standard titration solution, and do a blank determination at the same time. If the test solution is alkaline, it needs to be titrated to the endpoint with 0.02 mol/L hydrochloric acid standard titration solution, and a blank determination is also performed. Calculate the acidity Xs or alkalinity X
Xg = c(V -Vo)0 according to formula (3) or formula (4) respectively.049
Wherein: c——actual concentration of sodium hydroxide standard titration solution, mol/L; Vo
——volume of sodium hydroxide standard titration solution consumed in titration of blank, mL; V—volume of sodium hydroxide standard titration solution consumed in titration of sample solution, mL; m-
——sample weight;
（3）
——mass of sulfuric acid expressed in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L].
C (V -V)0. 040 × 100
Wherein: Ci—actual concentration of hydrochloric acid standard titration solution, mol/L; Vo
—volume of hydrochloric acid standard titration solution consumed in titration of blank, mL;—volume of hydrochloric acid standard titration solution consumed in titration of sample, mL;
·(4)
—mass of sodium hydroxide expressed in grams equivalent to 1.00mL hydrochloric acid standard titration solution c(HCI)=1.000mol/L].
5 Inspection rules
5.1 Sampling method: in accordance with the provisions of "raw powder sampling" in GB1605. 5.2 Acceptance rules: in accordance with the provisions of GB1604. 6 Marking, packaging, transportation, storage
6.1 The packaging and marking of thiamethoxam technical shall comply with the relevant provisions of GB3796 and shall be marked with a trademark. 6.2 Buprofezin is packaged in lined plastic bags and plastic woven bags, with each bag weighing 20kg or 30kg (or as required by the user). 6.3 Buprofezin technical must be kept dry and protected from moisture and sunlight during transportation and storage, and must not be mixed with food, seeds, feed, etc.
6.4 Under the packaging, transportation, and storage conditions that comply with this standard, the warranty period of Buprofezin technical (from the date of production) is two years. 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 Shenyang Chemical Industry 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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