GB 28144-2011Imidacloprid aqueous suspension concentrate (English PDF)

3.1 Composition and appearance

This product shall be made compliant imidacloprid, processing aids and fillers, should be flowable, easy to measure the volume of a liquid suspension, kept Possible release during precipitation, but shake the handle, restitution should be, there should be no lumps.

3.2 Technical Specifications

Imidacloprid suspension shall comply with the requirements of Table 1.

Table 1 Imidacloprid suspension control project indicators

project

index

350g/L 480g/L 600g/L Imidacloprid mass fraction /% Mass concentration or a/(g/L) (20 °C) 31.0 47.0 2.3-2.3 2.0-2.0 1.5-1.5 40.0 35017-17480 24-2460025-25 TABLE 1 (cont.) project index 350g/L 480g/L 600g/L pH range 6.0 to 9.0 Suspension rate /% >= 95 Wet sieve test (Test through 75µm sieve) /% >= 98 Persistent foaming (amount of foam after 1min)/mL <= 25 Pourability /% After pouring the residue <= 4 the residue was washed <= 0.5 Low temperature stability Qualified b B qualified thermal storage stability when a dispute occurs when a mass to mass fraction of arbitration.

Low temperature stability test, the thermal storage stability test was measured every three months, at least once during normal production b.

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 "liquid formulation sampling" approach. Determining Sample packages with a random number table method; final sample size not less than 600mL.

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 of Imidacloprid retention time of the peaks, the relative difference should be less than 1.5%.

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.

Typical HPLC Imidacloprid suspension shown in Figure 1.

1 --- imidacloprid.

FIG FIG 1 HPLC suspending agents Imidacloprid

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, dissolved in methanol and diluted to the mark, ultrasonic 5min shaken to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, with the mobile Phase was diluted 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, dissolved in methanol and diluted to the mark, ultra 5min sonication to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, with Mobile phase and dilute 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) is calculated, according to the concentration of formula (1 ') is calculated.

w1 = A2

· M1 · w

A1 · m2

rho1 =

A2 · m1 · rho · w · 10 A1 · m2 (1') where.

W1 --- imidacloprid sample mass fraction in%;

rho] 1 --- imidacloprid sample concentration, in g/L expressed;

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

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

W --- the mass fraction of imidacloprid standard sample, expressed in%;

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

--- M2 mass of sample, grams (G);

When the density of the sample rho --- 20 °C, units (according to GB/T 4472 measured) grams per milliliter (g/mL).

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. Imidacloprid the measurement results of the concentration should be less than the difference between the two parallel 10g/L, the arithmetic mean as a measurement result.

4.5 PH value measured

Carried out in GB/T 1601.

4.6 Determination of the suspension rate

Perform the GB/T 14825-2006 4.2. 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 flask with 60mL methanol and 25mL three times the residue was washed into a 100mL receiving all Volumetric flask, and shaken at ultrasonic 5min, cooled to room temperature, the volume, shake, filtered, measured by mass 4.4 imidacloprid, suspending calculated Floating rate.

4.7 Wet sieve test

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

4.8 Pourability assay

4.8.1 Method summary

After the sample is placed in a container of the suspension left for a certain time, in accordance with the procedures for the pouring, the measurement sample retained in the container Amount; The vessel was washed with water, and then measuring the amount in the container.

4.8.2 Instruments

With ground-stoppered cylinders. 500mL ± 2mL; cylinder height 39cm, between the upper and the lower scale for distance 25 mL (or for the determination of equivalent pour Down of other containers).

4.8.3 Test Procedure

Good mixing a sufficient amount of sample, wherein the portion promptly placed in the cylinder has been weighed (including a stopper) (accurate to 0.01g), attached to 8/10 at the graduated cylinder, plugged ground-stopper, placed 24h. The tap is opened, rotation of the cylinder 135 ° from the upright position poured 60s, 60s re-inverted, Reweighed and the plug cylinder (accurate to 0.01g).

Equivalent to 80% of the cylinder volume of water (20 °C) was poured into a measuring cylinder, stoppered a ground stopper, after the measuring cylinder upside down 10 times, the above-described tilt operation Pour the contents, and the plug cylinder weighed (accurate to 0.01g).

4.8.4 Computing

The mass fraction and the mass fraction of the residue after pouring a sample of the residue after washing respectively of formula (2) and (3) Calculated.

w2 = m2-m0m1-m0 ×

100 (2)

w3 = m3-m0m1-m0 ×

100 (3)

Where.

Mass fraction w2 of the residue poured --- sample, expressed in%;

The mass fraction of the residue washed W3 --- sample, expressed in%;

--- M2 After pouring, the quality of the cylinder, a ground stopper and the residue, in grams (G);

M0 --- cylinder, the quality of the throwaway gag constant in grams (G);

--- cylinder M1, a ground stopper and the quality of the sample in grams (G);

--- M3 After washing, the quality of the cylinder, a ground stopper and the residue, in grams (g).

4.9 Determination of persistence of foaming

4.9.1 Method summary

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

4.9.2 Reagents

Standard hard water. rho (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0, according to GB/T 14825-2006 formulation.

4.9.3 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.

4.9.4 Determination 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.

4.10 Low temperature stability test

According to GB/T 19137 in the "suspension formulation" for suspension rate and wet sieve test still meet standard requirements for qualified.

4.11 Thermal storage stability test

According to GB/T 19136 "other formulation" for. After the heat storage mass fraction of imidacloprid to be not less than 90% before storage, the suspension was still conform Standards compliance.

4.12 Product inspection and acceptance

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

5.1 Marking, labeling, packaging

Application of Imidacloprid suspension polyester bottle, content is generally net 50g, 100g, 250g, 400g. The user may also request or Ordering Agreement other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

Imidacloprid suspension package airiness, dry place. Storage and transportation, to prevent moisture and sunlight, no food, seed, Feed-mixing, 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

Under the provisions of storage and transportation conditions, imidacloprid suspension of the guarantee period of two years from the date of manufacture.

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.