Some standard content:
HG3622--1999
The product quality control items and indicators of this standard are formulated based on the quality indicators of similar foreign products and in combination with the enterprise standards of 3% carbofuran granules of various domestic manufacturers. The analytical method of active ingredients is equivalent to the International Pesticide Analysis Cooperation Council (CIPAC) method-high performance liquid chromatography.
Appendix A of this standard is the appendix of the standard.
This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafting unit of this standard: Hunan Chemical Industry Research Institute. Participating drafting units of this standard: Hunan Haili Chemical Co., Ltd. Test Plant, Shandong Huayang Pesticide Chemical Group Co., Ltd., Jiangsu Tongshan Pesticide Factory, Hubei Shalongda Jiangling Pesticide Factory. The main drafters of this standard: Huang Xiangyun, Wu Yanling, Zhou Zhichun, Liu Ziyou, Shao Zhumin, Zheng Jingyu, Peng Jiping. 1205
Chemical Industry Standard of the People's Republic of China
3% Carbofuran Granules
3 %Carbofuran granules
Other names, structural formulas and basic physicochemical parameters of Carbofuran are as follows: ISO common name: Carbofuran
CIPAC digital code: 276
Chemical name: 2,3-Dihydro-2,2-dimethylbenzofuran-7-yl N-methylcarbamate Structural formula:
O--CO--NH-CH:
Empirical formula: C12H1sNO
Relative molecular mass: 221.3 (according to the 1993 international relative atomic mass) Biological activity: Insecticidal
Melting point (℃): 151~152
Vapor pressure (33℃): 2.7MPa
HG 3622—1999
Solubility (g/L, 25℃): 0.7 in water; 150 in acetone, 270 in dimethylformamide; 140 in acetonitrile; 90 in cyclohexanone; 40 in benzene; 40 in ethanol; slightly soluble in petroleum ether and xylene. Stability: Decomposition begins at 180℃, relatively stable in acidic medium, unstable in alkaline medium, and temperature and alkalinity have a greater impact on the hydrolysis rate. 1 Scope
This standard specifies the requirements, test methods, labeling, packaging and storage and transportation of 3% carbofuran granules. This standard applies to granules processed by coating method using carbofuran technical and adjuvants and carriers that meet the standards. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB190-1990 Dangerous Goods Packaging Marking
GB/T1250-1989 Method for indicating and determining limit values GB/T1600-1979 (1989) Method for determining moisture content in pesticides GB/T1601-1993 Method for determining pH value in pesticides GB/T1604-1995 Acceptance rules for commercial pesticides GB/T1605-1979 (1989) Acceptance method for commercial pesticides GB3796-1983 General rules for pesticide packaging
Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999 1206
Implementation on June 1, 2000
3 Requirements
HG 3622--1999
3.1 Appearance: Purple-blue or reddish-brown loose granules, without visible foreign matter. 3.23% carbofuran granules shall meet the requirements of Table 1. Table 13% carbofuran granules control items index items
carbofuran content, %
water, %
particle size (1650~420μm particle size ratio 1 t2.5), % shedding rate, %
pH range
hot storage stability
Note: hot storage stability is sampled once every six months. Test method
4.1 Sampling
The number of packages to be sampled is determined by random number table method, and the final sampling volume shall not be less than 1kg. 4.2 Identification test
This identification test can be carried out simultaneously with the determination of carbofuran content. Under the same high performance liquid chromatography (HPLC) operating conditions, the relative difference between the retention time of a chromatographic peak of the sample solution and the retention time of the chromatographic peak of the standard solution carbofuran should be within 1.5%. 4.3 Determination of carbofuran content
4.3.1 Summary of method
The sample is dissolved in methanol, acetophenone is used as the internal standard, methanol decahydrate is used as the mobile phase, and a stainless steel column filled with C1: bonded stationary phase and a UV detector are used to separate and determine the carbofuran in the sample by high performance liquid chromatography. 4.3.2 Reagents and solutions
Methanol: HPLC grade, filtered through a 0.5 μm pore size filter membrane. Water: twice distilled water, filtered through a 0.5 μm filter membrane. Carbofuran standard sample: known content, greater than or equal to 99.0%. 7-Hydroxyfuranol (2,3-dihydro-2,2-dimethylbenzofuran-7-ol). Internal standard: acetophenone, which should not contain impurities that interfere with the analysis. Internal standard solution: weigh 1000 mg of acetophenone and dilute it to 1000 mL with methanol and shake well. 4.3.3 Instruments and equipment
High performance liquid chromatograph: with variable wavelength UV detector. Chromatographic data processor.
Chromatographic column: 250mm×4.6mm(id) stainless steel column, with Cis bonded stationary phase, 5μm. Guard column: 20mm×4.6mm(id) stainless steel column, with Cie bonded stationary phase, 5μm. Injector: 50μL.
4.3.4 High performance liquid chromatography operating conditions
Mobile phase: methanol + water = 1 + 1 (volume ratio). If there are signs of decomposition on the column, add phosphoric acid (3-5 drops per liter). Flow rate: 1 mL/min.
Column temperature: 40℃.
Detection wavelength: 280nm.
Injection volume: 10μL.
Detector sensitivity: full scale 0.2 absorbance. HG3622--1999
Retention time: about 14 minutes for carbofuran; about 10 minutes for internal standard. 1 Internal standard; 2-carbofuran
Figure 1 High performance liquid chromatogram of carbofuran granules (with internal standard) The above operating parameters are typical (see Figure 1). The given operating parameters can be appropriately adjusted according to the characteristics of the instrument in order to obtain the best effect. 4.3.5 Column optimization
Set the column temperature to 40℃, measure the retention time of carbofuran (preferably between 12 and 15 minutes), and change the composition ratio of the mobile phase if necessary to measure the retention time and separation degree of acetophenone on carbofuran. If acetophenone is not completely separated from carbofuran, reduce the proportion of methanol in the mobile phase. This may result in a retention time of carbofuran greater than 15 minutes on some columns. Determine the retention time of 7-hydroxyfuroxol; if it interferes with carbofuran, re-optimization is required. Increase or decrease the column temperature in 5℃ intervals. Change the mobile phase ratio to keep the separation and retention time of carbofuran and acetophenone unchanged. Pay attention to the retention time and separation of 7-hydroxyfuroxol. When furoxol and other impurities are completely separated from carbofuran, sample analysis can begin.
4.3.6 Determination steps
a) Preparation of standard solution
Weigh about 45 mg (accurate to 0.0001 g) of carbofuran standard and about 45 mg of 7-hydroxyfuroxol in a 100 mL volumetric flask, add 5 mL of methanol and 50 mL of internal standard solution with a pipette, mix well, add deionized water to the scale before determination, shake, degas by ultrasonic, and filter with a filter membrane with a pore size of 0.45 μm.
b) Preparation of sample solution
Weigh about 8g (accurate to 0.0001g) of 3% carbofuran granules into a 50mL volumetric flask, accurately add 25mL of methanol, shake and extract for 15min, let stand for 10min, use a pipette to draw 5mL of sample solution into a 100mL volumetric flask, and then use the same pipette as a) to add 50mL of internal standard solution, mix, add twice-distilled water to the scale before determination, shake, and filter with a filter membrane with a pore size of 0.45μm. c) Determination
Under the above operating conditions, after the instrument baseline is stable, repeat the injection of standard solution, calculate the relative response value of each injection, and when the relative response value of two adjacent injections changes less than 1%, perform determination in the order of standard solution, sample solution, sample solution, and standard solution. 4.3.7 Calculation
Average the ratio of the peak area of carbofuran to the internal standard substance in the two sample solutions and the two standard solutions before and after the sample. The carbofuran content (X) expressed as mass percentage is calculated according to formula (1): 1208
Wherein: r—
HG 3622—1999
Xi = rem;P
The average value of the peak area ratio of carbofuran to the internal standard substance in the standard solution; The average value of the peak area ratio of carbofuran to the internal standard substance in the sample solution; The mass of the carbofuran standard sample, g;
m2——The mass of the sample, g;
P——The mass percentage of carbofuran in the standard sample. 4.3.8 Allowable difference
Take the average value as the reported result. The difference between the results of two parallel determinations should not exceed 0.2%. 4.4 Determination of moisture content
Products with moisture content less than or equal to 1% shall be determined by the Karl-Fischer end-point method in GB/T1600-1979; products with moisture content greater than or equal to 1% shall be determined by the azeotropic method.
4.5 Particle size
The particle size ratio shall be less than or equal to 1:2.5, and the particle size range must be between the specified 1650 and 420 μm (10 to 40 mesh), and the specific particle size range of the product shall be indicated in the product quality project indicators. 4.5.1 Instruments and equipment
Standard sieve group: The aperture is consistent with the selected particle size range. Vibrating screen: Amplitude 36 mm, 243 times/min. Pharmaceutical balance: accuracy 0.1g.Www.bzxZ.net
4.5.2 Determination steps
Stack the standard sieves up and down, place the large particle size sieve on the small particle size sieve, and install a receiving plate under the sieve. At the same time, fix the assembled sieve group on the vibrating sieve machine, accurately weigh 100g (accurate to 0.1g) of 3% carbofuran granules sample, place it in the upper sieve, cover it, start the vibrating sieve machine to vibrate for 10 minutes, collect the small particle size sieve on the weighing. The sieve on the sieve is greater than or equal to 90% and is qualified. 4.5.3 Calculation
The particle size (X,) expressed as mass percentage is calculated according to formula (2): ml×100
Where: m-
-3% carbofuran granules sample mass, 8, - small particle size sieve on the sample mass, m.
4.6 Determination of shedding rate
4.6.1 Instruments and equipment
Standard sieve: The aperture is the same as the small and medium particle size sieve in the “standard sieve group” in 4.5.1. Steel balls: 15 (7.9 mm).
Sieve vibrator: 224 times/min, amplitude 36 mm. 4.6.2 Determination steps
(2)
Accurately weigh 50 g of the sample with measured particle size, put it into the standard sieve containing 15 steel balls, place the sieve on the bottom plate and cover it, move it to the sieve vibrator, fix it and vibrate it for 15 minutes, and accurately weigh the mass of the sample in the receiving plate (accurate to 0.1 g). The shedding rate (X) expressed as a percentage by mass is calculated according to formula (3): Xg = ma×100
Where: m3
The mass of the sample in the receiving pan, g;
The mass of the sample, g.
HG3622-1999
Weigh 10g of the granule sample and measure it according to the pH meter method in GB/T1601-1993\Method for determination of hydrogen ion concentration of pesticides”. 4.8 Thermal storage stability test
4.8.1 Instruments and equipment
Constant temperature box (or constant temperature water bath): (54±2)℃. Glass bottle with a stopper that can still be sealed at 54℃: 50mL. 4.8.2 Test steps
Take about 50g of the granule sample and place it in a glass bottle with a stopper. Store at least 5 bottles, respectively. Weigh, place in a (54 ± 2)℃ constant temperature box, and leave for 14 days. Take out, weigh separately, and test the active ingredient content of the sample with no change in mass within 24 hours, and the content shall not be less than 2.8%. 4.9 Inspection and acceptance of products
Inspection and acceptance of products shall comply with the relevant provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
The marking, labeling and packaging of 5.13% carbofuran granules shall comply with GB3796 and GB190 Dangerous Goods Packaging The relevant provisions of the mark.
5.2 The product is packed in two layers, the inner bag is a plastic bag, and the outer bag is a polypropylene coated woven bag. The bag opening is folded with nylon machine stitching. 5.3 According to user requirements or order agreements, other forms of packaging can be used, but they must comply with the relevant provisions of GB3796. 5.4 The packages should be stored in a ventilated and dry warehouse. The stacking method should meet safety requirements and be careful not to puncture the outer packaging bag. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, and feed, avoid contact with skin and eyes, and prevent Only inhale through the mouth and nose. 5.6 Safety: Carbofuran is a highly toxic carbamate insecticide. It is toxic to people if swallowed or inhaled. It can also penetrate through the skin. Therefore, protective gloves should be worn when using this product. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If poisoning occurs, atropine can be injected intramuscularly for detoxification in mild cases. If necessary, a doctor should be consulted. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of 3% Carbofuran granules is two years from the date of production. During the warranty period, the content of active ingredients should not be less than 2.8%.
HG 3622—1999
Appendix A
(Standard Appendix)
Gas chromatography determination of 3% carbofuran granules This method can be used for production control analysis.
A1 Method Summary
The sample is dissolved in acetone, diethyl phthalate is used as the internal standard, and a glass column filled with 5% OV-101/ChromosorbG AW-DMCS and a hydrogen flame ionization detector are used to perform gas chromatography on the carbofuran in the sample. A2 Reagents and Solutions
Chloroform: analytical grade.
Acetone: analytical grade.
Carbofuran standard: known content, greater than or equal to 99.0%. Internal standard: diethyl phthalate, which should not contain impurities that interfere with the analysis. Stationary liquid: OV-101.
Carrier: ChromosorbGAw-DMCS (250～170 μm). Internal standard solution: weigh about 2 g of diethyl phthalate (accurate to 0.000 2 g) in a 200 mL volumetric flask, dissolve and dilute to the mark with acetone, shake well, and set aside.
A3 Instruments and equipment
Gas chromatograph: with FID detector.
Recorder: full scale 5mV.
Chromatographic column: 1 m×3 mm (id) glass column. Vaporization chamber: column head injection or adding quartz glass cannula. Column filling: OV-101 coated on ChromosorbGAW-DMCS (250～170μm), stationary liquid: (solid liquid + carrier) = 5:100 (mass ratio).
A4 Preparation of chromatographic column
A4.1 Coating of stationary liquid
Weigh 0.5g 0V-101 into a 200mL beaker, add 30mL chloroform to dissolve, mix well, pour 9.5g dry ChromosorbGAW-DMCS carrier into it to make the carrier completely immersed, put the beaker in a fume hood, slowly evaporate the solvent under an infrared lamp (turn the beaker frequently during the desolventizing process and tap it gently to make it evenly coated), then move to a 90~100℃ oven and dry for 30min for use. A4.2 Filling of chromatographic column
Connect a small funnel to the outlet of the washed and dried chromatographic column, fill the prepared filler into the column in batches, and tap the column wall continuously until it is filled to 1.5cm from the column outlet. Move the funnel to the inlet of the chromatographic column, plug a small ball of silanized glass wool at the outlet, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, continue to slowly add the filler, and tap the column wall continuously to make it filled evenly and tightly. After filling, also plug a small ball of glass wool at the inlet end and press it appropriately to keep the column filler from moving. A4.3 Aging of chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, do not connect the detector at the outlet end for the time being, and pass the carrier (N) at a flow rate of 5-10mL/min. Raise the temperature to 180℃ in stages and age at this temperature for at least 6h. A4.4 Gas chromatography operating conditions
HG 3622—1999
Temperature (C): column chamber 154, vaporization chamber 180, detector chamber 180. Gas flow (mL/min): carrier gas (N2) 80, hydrogen 80, air 900. Retention time: about 6.5min for carbofuran, 3.4min for internal standard. ≤2
1--Solvent, 2-Furanol; 3--Internal standard; 4--Carbofuran Figure A1 Gas chromatogram of carbofuran (with internal standard) The above operating parameters are typical (see Figure A1). According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect.
A4.5 Determination steps
a) Preparation of standard solution
Weigh about 0.075g (accurate to 0.0002g) of carbofuran standard, accurately add 5mL of internal standard solution into a 25mL volumetric flask, dilute with acetone, shake and set aside.
b) Preparation of sample solution
Weigh about 5g (accurate to 0.0002g) of 3% carbofuran granules, accurately add 10mL of internal standard solution into a 50mL volumetric flask, shake for 5min, add 15mL of acetone, shake well, let stand and set aside. c) Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the relative response value of each needle, and when the relative response value of two adjacent needles changes less than 1.5%, perform the determination in the order of standard solution, sample solution, sample solution, and standard solution.
A4.6 Calculation
Average the peak height ratios of carbofuran and internal standard in the two sample solutions and the two standard solutions before and after the sample. The carbofuran content (X,) expressed as mass percentage is calculated according to formula (A1): rem,P
Where: ri-
the average value of the peak height ratios of carbofuran and internal standard in the standard solution; the average value of the peak height ratios of carbofuran and internal standard in the sample solution; the mass of the carbofuran standard sample, g;
m2—the mass of the sample, g
Pthe mass percentage of carbofuran in the standard sample. A4.7 Allowable difference
The difference between the results of two parallel measurements should not be greater than 0.2%. 1212
·(A1)
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