Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2215-91
10% Gramocarb Granules
Published on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
Chemical Industry Standard of the People's Republic of China
10% Gramocarb Granules
Subject Content and Scope of Application
HG2215-91
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for 10% Gramocarb Granules.
This standard applies to 10% Gramocarb Granules processed by extrusion granulation adsorption process. Active ingredient: Gramocarb
Chemical name N,N-diethylthiocarbamate p-chloroester. Structural formula:
Molecular formula: C12H16NOSCI
CHS—CO—N(C,H)2
Relative molecular mass: 257.78 (according to the international relative atomic mass in 1987)2
Cited standards
GB1600
GB1601
GB1604
GB1605
GB3796
3 Technical requirements
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3.1 Appearance: Blue-green or gray columnar loose granules. 3.2 10% fenvalerate granules shall also meet the following index requirements: Item
fenvalerate content, % (m/m)
Sieve analysis (the ratio of the sample amount passing through the 2.0mm standard sieve and retained on the 450um standard sieve to the sample amount), % (m/m) Strength, % (m/m)
pH range
Water content, % (m/m)
Disintegration in water (min)
Test method
4.1 Determination of fenvalerate content
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991>
10.0±8: No.|| tt||Implemented on July 1, 1992
4.1.1 Reagents and solutions
Trichloromethane (GB682);
Granumidil standard sample, known content;
HG2215-91
Dipropylene phthalate: internal standard (without impurities interfering with the gas chromatography analysis); Diethylene glycol adipate (DEGA): chromatographic stationary phase; chromosorbW·AW-DMcS, 150~180μm (80~100 mesh), chromatographic carrier; Internal standard solution: 0.3mg/mL trichloromethane solution of dipropylene phthalate. 4.1.2 Instruments
Gas chromatograph: hydrogen flame ionization detector; recorder or electronic digital integrator;
Chromatographic column: 1000mm long, 3mm inner diameter stainless steel column, filled with 5% DEGA/chromosorbW. AW-DMCS150～180um (80100 mesh) filler;
Microinjector: 10uL;
Centrifuge.
4.1.3 Operation steps
4.1.3.1 Preparation of chromatographic column
a. Coating of stationary liquid: Weigh 0.500g of diethylene glycol adipate, place it in a 250mL beaker, add 50mL acetone, and stir to completely dissolve the stationary liquid. Add a certain amount of carrier (about 10) according to the concentration of the stationary liquid to be prepared, so that it is immersed in the stationary liquid. Heat with a steam bath or infrared lamp, and shake the beaker from time to time until the solvent evaporates and is almost dry, then place in a 105℃ oven to dry for 2 hours. b. Filling of the chromatographic column: Connect a small funnel to the inlet of the clean and dried stainless steel column, fill the outlet with an appropriate amount of glass wool and wrap it with gauze, and connect it to the vacuum pump through a hose. Turn on the vacuum pump, add the column filler from the funnel in batches, and tap the column wall continuously to make the filler fill the chromatographic column evenly and tightly. A small ball of glass wool is also plugged at the inlet of the column, and it is properly pressed to keep the filler from moving. c. Aging of the chromatographic column: Connect the inlet of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the outlet to the detector. Raise the temperature to 200℃ in stages at a carrier gas flow rate of about 15mL/min, and age at this temperature for at least 20 hours. After cooling, connect the outlet of the column to the detector. 4.1.3.2 Gas chromatography operating conditions
Temperature:
Column chamber 180±5℃;
Vaporization chamber 240℃;
Detector 280℃.
Gas flow rate:
Carrier gas (N2) 30~40mL/min;
Hydrogen 30mL/min;
Air 300mL/min.
Injection volume:
0.6~1.0uL.
Retention time: (min):
Carbamidocarb 7.29;
2-chloroisomer 6.05;
Dipropylene phthalate 4.12.
HG2215--91
Gas chromatogram of fenvalerate granules
1—Solvent; 4—Dipropylene phthalate; 5—2-chloroisomer; 6fenvalerate 4.1.3.3 Preparation of standard solution
Accurately weigh 0.075 g (accurate to 0.0001 g) of fenvalerate standard sample and place it in a 15 mL stoppered glass bottle. Use a pipette to add 10 mL of internal standard solution and shake well.
4.1.3.4 Preparation of sample solution:
Take about 20g of a representative sample of gramineous granules, grind it in a mortar, accurately weigh 0.75g of the grinded sample, accurate to 0.0001g, and place it in a 10mL centrifuge tube. Use the same pipette as the standard solution to add 10mL of internal standard solution, add a stopper, shake thoroughly for 15min, let stand (or centrifuge), and take the supernatant for analysis. 4.1.3.5 Determination
After the instrument is stable, inject several needles of standard solution until the peak height ratio of two adjacent needles is basically stable, and then inject and analyze in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
The difference between the peak height ratio of fenpyrocarb and the internal standard in the two injections of the sample solution and the two injections of the standard solution before and after the sample, divided by their average value, should not be greater than 1.2%. Otherwise, the injection should be repeated.
4.1.4 Calculation
The peak height ratios of a, d and b, c are averaged respectively, and the mass percentage content of fenpyrocarb X1 is calculated according to formula (1): Xi_\·m..w
Where: \——the average value of the peak height ratio of fenpyrocarb and the internal standard on the chromatogram of the sample solution; *2——the average value of the peak height ratio of fenpyrocarb and the internal standard on the chromatogram of the standard solution; m1——the mass of fenpyrocarb sample, g;
m2——the mass of fenpyrocarb standard, g;
——the percentage content of fenpyrocarb standard, % (m/m). Allowable difference: The difference between the results of two parallel determinations should not be greater than 0.5%. 4.2 Sieving
4.2.1 Instrument
Standard sieve: double-layer sieve with apertures of 2 mm and 450 um, equipped with sieve bottom and sieve cover. (1)
4.2.2 Determination
HG2215--91
Weigh 50 g of sample, accurate to 0.1 g, and put it into a standard sieve with an upper aperture of 2 mm and a lower aperture of 450 um. Vibrate the sieve for 1 min (one back and forth every 2 seconds), and weigh the mass of particles in the 450 um standard sieve. The particle size mass percentage X2 is calculated according to formula (2): Xe
Where: ml——mass of particles in the 450 um standard sieve, g; -mass of sample, g.
4.3 Determination of strength
4.3.1 Apparatus
Flat rotary ball mill: adjustable speed;
m1x100
Material tank: ceramic or iron, inner diameter 100mm, inner depth 100mm; 3 ceramic balls, diameter 30±2mm, mass of each ball 35±3g. 4.3.2 Determination steps
Weigh 100g of the sample that has passed the sieve analysis in 4.2, accurate to 0.1g, put it in the material tank, adjust the speed to 75r/min, ball mill for 15min, take out all the materials (including powder), and pass through a 450um standard sieve again (consistent with the number of sieve analysis and vibration). Weigh the sample under the sieve, and the strength X is calculated according to formula (3):
In the formula, m—sample mass, g;
m1—sample mass under the sieve after ball milling, g.
4.4 pH determination
Measure according to the pH meter method in GB1601, and the sample weight is 10g. 4.5 Determination of moisture
The test is carried out according to the azeotropic distillation method in GB1600. 4.6 Disintegration in water
4.6.1 Apparatus
Cultivation III, inner diameter 100mm
Stopwatch.
4.6.2 Determination
Fill the culture dish with water, put in 10 test pieces, start the stopwatch, and observe the disintegration. If all the test pieces disintegrate within 10 minutes, the test piece is qualified. 5 Acceptance rules
5.1 The sampling method is in accordance with GB1605.
5.2 Acceptance rules: Acceptance is carried out according to the relevant provisions in GB1604. 6 Marking, packaging, transportation and purchase and storage
6.1 The marking and packaging of this product shall comply with the relevant provisions in GB3796. (3)
6.2 10% Grain of Grapefruit Granules shall be packed in polypropylene (or polyvinyl chloride) plastic woven bags lined with polyethylene plastic bags, and the net weight of each bag shall not exceed 25kg.
6.3 During storage and transportation, it shall be strictly protected from moisture and sunlight, and maintained in good ventilation. It shall not be mixed with food, seeds, and feed, and shall avoid contact with the skin and inhalation through the mouth and nose.
6.4 Under normal storage and transportation conditions, the warranty period of this product is 2 years. 4
Additional Notes:
HG2215—91
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 jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard are Hou Yukai, Zhang Yunzhen, Chen Guifa, Xing Hong, and Liu Guoxiu. 5
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