GB 28132-2011Imidacloprid micro-emulsion (English PDF)

3.1 Composition and appearance

This product should be compliant imidacloprid, water and suitable additives made, should be transparent or translucent homogeneous liquid without visible suspended Float and precipitates.

3.2 Technical Specifications

Imidacloprid microemulsion should meet the requirements of Table 1.

Table 1 imidacloprid microemulsion quality control program indicators

Item Index

Imidacloprid mass fraction /% 20.0 10.0 1.0 to 1.0 1.2-1.2 pH range of 5.0 to 8.0 Transparent test temperature range (0 °C ~ 50 °C) qualified Emulsion stability (diluted 500 times) Qualified (After 1min) Persistent foaming/mL <= 25 Thermal storage stability of a qualified Low temperature stability a qualified when a normal production, thermal storage stability, low-temperature stability test was measured at least once every three months.

Test Method 4

4.1 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.

4.2 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 to a peak of imidacloprid chromatographic retention time, the relative difference should be 1.5% Fewer.

4.3 Determination of the mass fraction of imidacloprid

4.3.1 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.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

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

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

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

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.3.4 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 microemulsion HPLC is shown in Figure 1.

1 --- imidacloprid.

Figure 1 imidacloprid microemulsion HPLC diagram

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 0.1g (accurate to 0.0002g) imidacloprid standard in 100mL flask, dissolved in methanol and diluted to the mark, 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, with the mobile Phase and dilute to the mark.

4.3.5.2 Preparation of sample solution

Weigh containing imidacloprid 0.1g (accurate to 0.0002g) sample in 100mL flask, dissolved in methanol and diluted to the mark, ultra Acoustic oscillations 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask Mobile phase and dilute to the mark.

4.3.5.3 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.

4.3.5.4 Calculation

Imidacloprid sample mass fraction according to formula (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 --- 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).

4.3.6 Allowable difference

Imidacloprid content parallel determination of the difference between the results, 10% of the microemulsion should be less than 0.5%; 20% of the micro-emulsion should not exceed 0.8% the arithmetic mean value as a measurement result.

4.4 Transparent test temperature range

Samples of 10mL in a 25mL test tube fitted with a thermometer, stirring with a stirring rod and down, placing the tubes on ice-water bath, the temperature control Maintaining 0 deg.] C, the samples were observed whether turbidity, tubes were again placed in a water bath for 2 °C/min speed slowly warmed to 50 °C, View Record Examine whether the samples appear cloudy. It does not appear in the range of 0 ~ 50 °C cloudy qualified.

Determination of 4.5 pH value According to GB/T 1601 carried out.

4.6 Emulsion stability test

The sample was diluted 500-fold, according to GB/T 1603 test, the non-oil slick, no precipitation under qualified.

4.7 Persistent foaming test

4.7.1 Method summary

The sample was mixed with a predetermined amount of standard hard water, after standing foam volume recorded.

4.7.2 Reagents

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

4.7.3 Instruments and Appliances

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

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

4.7.4 Measuring step

Added 180mL graduated cylinder standard hard water, 1.0g sample was weighed into a graduated cylinder (accurate to 0.1g), added to standard hard water from the cylinder Plug at the bottom tick 9cm, the cover plug to the bottom of the cylinder as the center, upside down 30 times (2s). Stand on the test stand 1min, record lather volume.

4.8 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, emulsion stability still it shall meet the standards.

4.9 Low temperature stability test

According to GB/T 19137 in "homogeneous emulsion and liquid preparations" to. 7d after removing the beaker returned to room temperature, with gentle agitation, there should be no visible Particles and oil.

4.10 Product inspection and acceptance

Shall comply with GB/T 1604's. Treatment of extreme values using the rounding value comparison method.

5.1 Marking, labeling, packaging

Imidacloprid microemulsion marking, labeling and packaging should comply with the provisions of GB 4838. Imidacloprid microemulsion with applications within the plug and the outer cover Brown glass bottle or PET bottle packaging, bottle net content is generally 100g, 500g, etc; corrugated packaging boxes or plastic boxes, each containing a net an amount of not more than 10kg. Also available upon request or order agreement other forms of packaging, subject to the provisions of GB 4838.

5.2 Storage

Imidacloprid microemulsion package should be stored in well-ventilated, dry coffers. Storage and transportation to prevent moisture and sun, not with food, seeds, Feed-mixing, 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, warranties of imidacloprid microemulsion two years starting from the date of manufacture.

Appendix A

(Informative)

Other name, structural formula and basic physicochemical parameters of imidacloprid 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.