GB 28139-201170% Imidacloprid water dispersible granules (English PDF)

3.1 Composition and appearance

This product shall standard imidacloprid original drug, carriers and adjuvants are made, should be dry, free-flowing, almost no dust, no visible the extraneous matter and hard lumps.

3.2 Technical Specifications

Imidacloprid water dispersible granule should meet the requirements of Table 1.

Table 1 imidacloprid water dispersible granules Item Index Control

Item Index

Imidacloprid content/2.5-2.5 70.0% Moisture /% <= 2.0 pH range 6.0 to 9.0 TABLE 1 (cont.) Item Index Wetting time/s <= 60 Fineness (75µm test sieve) /% >= 98 Suspension rate /% >= 90 Particle size (on the left 100µm test sieve) /% >= 90 Dispersibility /% >= 80 Persistent foaming (amount of foam after 1min)/mL <= 20 Passing a heat storage stability Thermal storage stability test was measured every three months, at least once during a normal production.

Test Method 4

Safety Tips. to use this standard shall have practical experience of laboratory work. This standard does not indicate any safety issues. Make with those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the provisions of relevant state laws and regulations.

4.1 General provisions

This standard reagent in the absence of water and other requirements stated, refer to three predetermined analytical reagents and GB/T 6682-2008 of water. The test results performed by determining 4.3.3 rounding value in comparison 8170-2008 GB/T .

4.2 Sampling

Carried out in GB/T 1605-2001 of "solid preparation sampling" approach. Determining Sample packages with a random number table method; final sample size not less than 600g.

4.3 Identification Test

The present liquid chromatography --- identification test can be conducted simultaneously with the determination of the mass fraction of imidacloprid. Chromatography under the same operating conditions, the test A solution sample peak retention time of the standard solution imidacloprid peak retention time, the relative difference of 1.5% should be or less.

4.4 Determination of the content of Imidacloprid

4.4.1 Method summary

Sample dissolved in mobile phase, methanol and water as mobile phase, used as a filler C18 stainless steel column and UV detector at a wavelength of at 260nm, of the sample imidacloprid RP-HPLC separation and determination, external standard.

4.4.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Imidacloprid Sample. A known mass fraction w>=99.0%.

4.4.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (id) stainless steel column, C18,5µm filler contents (or column with equivalent effect);

Filter. membrane pore size of about 0.45 m;

Microsyringe. 50µL;

Quantitative sampling tube. 5µL;

Ultrasonic cleaning.

4.4.4 HPLC operating conditions

Mobile phase. [Psi] (methanol. water) = 40.60, by membrane filtration, and degassing;

Flow rate. 0.8mL/min;

Column temperature. room temperature (temperature change should be less than 2 deg.] C);

Detection wavelength. 260nm;

Injection Volume. 5µL;

Retention time. imidacloprid about 6.0min.

Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.

A typical aqueous dispersion of 70% by HPLC Imidacloprid granules Figure 1 in FIG.

1 --- imidacloprid.

FIG. 170% imidacloprid water dispersible granules by HPLC FIG.

4.4.5 Determination Step

4.4.5.1 Preparation of standard solution

0.1 g of weighed (accurate to 0.0002g) imidacloprid in Sample 100mL volumetric flask, diluted with methanol to the mark, the ultrasonic oscillation 5min to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, dilute with the mobile phase Release to the mark.

4.4.5.2 Preparation of sample solution

Containing 0.1 g of imidacloprid was weighed (accurate to 0.0002g) sample in 100mL volumetric flask, diluted with methanol to the mark, the ultrasonic vibrator 5min swing dissolve the sample cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, with the mobile phase Diluted to the mark.

4.4.5.3 Determination

Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two adjacent pins relative change in peak area imidacloprid After less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.4.5.4 Computing

The two needle and the sample solution was measured before and after the two doses of the standard sample solution and peak areas were averaged imidacloprid. Imidacloprid sample Mass fraction by formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

--- the imidacloprid sample mass W1 fraction;

A2 --- sample solution, imidacloprid average peak area;

M1 --- imidacloprid standard mass in grams (G);

W --- the mass fraction of the standard imidacloprid;

A1 --- the standard solution, the average peak area imidacloprid;

--- M2 sample mass, in grams (g).

4.4.6 Allows poor

The difference between the results of two replicates imidacloprid content should not exceed 1.0%, and the arithmetic mean value as a measurement result.

4.5 Determination of Moisture

According to GB/T 1600 in the "azeotropic distillation method".

4.6 PH value measured

Carried out in GB/T 1601.

4.7 Determination of the suspension rate

Proceed as GB/T 14825-2006 4.1. Weigh 0.1g of the imidacloprid-containing sample (accurate to 0.0002g), the remaining 1/10 suspensions and the precipitate was transferred to a 100mL volumetric flask, 3 times with methanol 60mL 25mL residue was washed into all 100mL volumetric flask, and shaken at ultrasonic 5min, cooled to room temperature, the volume, shake, filtered, measured by mass 4.4 imidacloprid, namely Operators suspended rate.

4.8 Determination of wetting time

Carried out in GB/T 5451.

4.9 Determination of fineness

According to GB/T 16150 in the "wet sieve method".

Determination of particle size 4.10

4.10.1 Instruments

Standard sieve. aperture (100 m);

Sieve Shaker. amplitude of 25mm, 1400 times/min.

4.10.2 Measuring step

Sample accurately weighed 100g water dispersible granules (accurate to 0.1 g of), placed on a 100µm Standard Sieve, stamped seal, shock promoter sieve shaker Swing 5min, collecting sieve was weighed (to the nearest 0.1g).

4.10.3 Computing

The particle size of the sample according to the formula (2).

w2 = m1m × 100

Where.

--- size w2 of the sample, expressed in%;

the mass m1 --- 100µm sieve material in grams (G);

--- m sample mass, in grams (g).

Determination dispersible 4.11

4.11.1 Method summary

The amount of water in water dispersible granules was added under stirring and mixing to prepare a suspension, after standing for some time, removing a top 9/10 Suspension, and 1/10 bottom drying the precipitate was measured gravimetrically.

4.11.2 Reagents and equipment

Standard hard water. rho (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0, according to GB/T 14825 formulation;

Beaker. 1000mL, inner diameter (102 ± 2) mm;

Electric mixer. with speed control (0 ~ 1000) r/min;

Stainless steel stirring rod (see FIG. 2). with 4 fixed propeller stirring blade stirring bar, the angle between the blades is 45 °;

A rotary vacuum evaporator;

Stopwatch.

In millimeters

FIG 2 stainless stirring rod

4.11.3 Measuring step

At 20 °C ± 1 °C, standard hard water was added to the 900mL beaker, stir bar is fixed in the center of the beaker, stirring the beaker from the blade bar Bottom 15mm, and a stirring blade pitch rotation direction advancing the rod to ensure that the liquid swirls up stir bar, a speed of 300r/min stirring opening Stirrer, the sample 9g water dispersible granules (to the nearest 0.1g) was stirred in water was added, stirring was continued for 1min. Close stirring, so that hydrostatic suspension in the subsurface, and the suspension is possible without stirring, 90mL of water was distilled off remaining suspension using a rotary vacuum evaporator at 60 °C ~ 70 °C Dried to constant weight, weighed (to the nearest 0.1g).

4.11.4 Computing

Dispersion of the sample according to equation (3) is calculated.

w3 = 10

(M-m1)

9m × 100

Where.

W3 --- dispersibility of the sample, expressed in%;

m --- the mass of the sample taken, in grams (G);

After mass M1 --- dried residue, in grams (g).

4.12 Persistent foaming test

4.12.1 Method summary

A predetermined amount of sample is mixed with standard hard water, the foam volume recorded on standing.

4.12.2 Reagent

Standard hard water. rho (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0, according to GB/T 14825 formulated.

4.12.3 Instruments and Appliances

Stoppered graduated cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL scale line to the bottom of the stopper 4cm ~ 6cm);

Industrial balance. a sense of the amount of 0.1g.

4.12.4 Measuring step

Was added 180mL graduated cylinder standard hard water, 1.0g sample was weighed into a measuring cylinder (to the nearest 0.1 g of), was added to the standard hard water from the cylinder 9cm scale line of the bottom plug, the plug cover to the bottom of the cylinder as the center, upside down 30 times (2s). Standing on the bench 1min, foam volume recorded.

4.13 Thermal storage stability test

According to GB/T 19136 of "powder formulation" performed. After the heat storage mass fraction of imidacloprid to be not less than 97% before storage, the suspension was still conform Standards compliance.

4.14 Product inspection and acceptance

Shall comply with the provisions of GB/T 1604's.

5.1 Marking, labeling, packaging

70% water dispersible granule application imidacloprid plastic or aluminum composite aluminum bag, net weight typically 50g, 100g. also may According to user requirements or ordering agreement, other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

70% of the water dispersible granules imidacloprid package airiness, dry place. Storage and transportation to prevent moisture and sun, not with food Thereof, seed, feedstuff, avoid contact with the skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

This formulation is low toxicity. It can penetrate through the skin. When using this product to avoid contact with the skin, application after application with soap and rinse with water.

Poisoning should immediately sent to hospital for symptomatic treatment.

5.4 Warranty Period

Storage conditions at a predetermined, water dispersible to ensure that 70% of Imidacloprid granules, from two years from the production date.

Appendix A

(Informative)

Other names imidacloprid, structural formulas and physicochemical parameters of the basic Other names, structural formulas and physicochemical parameters of the product basic active ingredient imidacloprid is as follows.

ISO common name. Imidacloprid CAS Registry Number. 138261-41-3 CIPAC Numeric Code. 582 Chemical name. 1- (6-chloro-3-pyridylmethyl) -N- nitromethylene-imidazol-2-yl-amine Structure.

Empirical formula. C9H10ClN5O2 Molecular weight. 255.7 Biological activity. insecticide Melting point. 144 °C Vapor pressure (20 °C). 4 × 10-7mPa Solubility (20 °C, g/L). 0.61 water, 0.68 of toluene, 55 dichloromethane, 1.2 isopropanol, n-hexane is less than 0.1 Stability follows. pH of 5 to 11 stable, hard to be hydrolyzed.

1102-