GB 28143-2011Imidacloprid emulsifiable concentrates (English PDF)

3.1 Composition and appearance

This product should be compliant imidacloprid made of a stable homogeneous liquid, free from visible suspended matter and sediment.

3.2 Technical Specifications

Imidacloprid EC shall comply with the requirements of Table 1.

Table 1 imidacloprid EC Control Project Index

project

index

5% 10% 20%

Imidacloprid mass fraction /% 1.0 to 1.0 20.0 10.0 5.0 0.5-0.5 1.2-1.2 Moisture /% <= 0.5 pH range of 5.0 to 8.0 Emulsion stability (diluted 200 times) Qualified

Table 1 (continued)

project

index

5% 10% 20%

Low temperature stability a qualified Thermal storage stability of a qualified Low temperature stability test, thermal storage stability test was measured at least once every three months during a normal production.

Test Method 4

Safety Tips. Use of this standard shall have practical experience of laboratory personnel work. This standard does not point out all of the safety issues. Make with those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the relevant national regulations.

4.1 General provisions

This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in water. Test results determined in accordance with GB/T 8170-2008 4.3.3 Rounding the value comparison method.

4.2 Sampling

According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determining sample package using a random number table method; the final sample size not less than 200mL.

4.3 Identification Test

Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of imidacloprid. Under the same chromatographic operating conditions, the test the retention time of the sample solution and the standard solution in a chromatographic peak retention time peaks imidacloprid, the relative difference should be less than 1.5%.

4.4 Determination of the mass fraction of imidacloprid

4.4.1 Method summary

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

4.4.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Imidacloprid standard. a known mass fraction w>=99.0%.

4.4.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

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

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

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 not exceed 2 °C);

Detection wavelength. 260nm;

Injection volume. 5µL;

Retention time. about imidacloprid 6.0min.

It said operating parameters are typical, according to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results.

Typical imidacloprid EC HPLC is shown in Figure 1.

1 --- imidacloprid.

Figure 1 Figure imidacloprid EC by HPLC

4.4.5 Measuring step

4.4.5.1 Preparation of standard solution

Weigh 0.1g (accurate to 0.0002g) imidacloprid standard in 100mL flask with methanol to volume, ultrasonic oscillation 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with mobile phase Release to the mark.

4.4.5.2 Preparation of sample solution

Weigh containing imidacloprid 0.1g (accurate to 0.0002g) sample in 100mL flask with methanol to the mark, the ultrasonic transducer Dang 5min to dissolve the sample was cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, with the mobile phase Dilute to the mark.

4.4.5.3 Determination

Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles Imidacloprid peak area relative change After less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.

4.4.5.4 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution imidacloprid peak areas are averaged. Imidacloprid sample the mass fraction according to equation (1).

w1 = A2

· M1 · w

A1 · m2

Where.

w1 --- sample imidacloprid mass fraction, expressed as a percentage;

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

m1 --- imidacloprid standard mass in grams (g);

w --- imidacloprid standard mass fraction, expressed as a percentage;

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

m2 --- sample mass, in grams (g).

4.4.6 Allowable difference

Imidacloprid poor quality score of two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.

4.5 Determination of Moisture

According to GB/T 1600 the "Karl Fischer method".

Determination of 4.6 pH value According to GB/T 1601 carried out.

4.7 Emulsion stability

Standard hard water sample was diluted 200-fold, according to GB/T 1603 test, no oil slick measuring cylinder (cream), and precipitation of heavy oil qualified.

4.8 Low temperature stability test

According to GB/T 19137 in "homogeneous emulsion and liquid preparations" to. Precipitate no more than 0.3mL qualified.

4.9 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. After the heat storage imidacloprid content should not be less than 97% before storage.

4.10 Product inspection and acceptance

Shall comply with GB/T 1604's.

5.1 Marking, labeling, packaging

Imidacloprid EC application glass or plastic PET bottle packaging, bottle net content of 500g or 1000g; carton or net weight 10kg 12kg. Also available upon request or order agreement other forms of packaging, subject to the provisions of GB 4838.

5.2 Storage

Imidacloprid EC package should be stored in well-ventilated, dry coffers. Storage and transportation, to prevent moisture and sunlight, no food, seed, feed Material mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

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

Poisoning should immediately sent to hospital symptomatic treatment.

5.4 Warranty Period

Under the specified storage conditions, imidacloprid EC guarantee period, starting from the date of manufacture of two years.

Appendix A

(Informative)

Other names for imidacloprid, structural formula and basic physicochemical parameters Other name, structural formula and basic physicochemical parameters of the active ingredient imidacloprid product are 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. Insecticidal Melting point. 144 °C Vapor pressure (20 °C). 4 × 10-7mPa Solubility (20 °C, g/L). water 0.61, 0.68 toluene, methylene chloride 55, 1.2 isopropanol, n-hexane is less than 0.1 Stability. pH value of 5 to 11 stable, easy hydrolysis.