GB 23551-2009Clomazone emulsifiable concentrates (English PDF)

3.1 Composition and appearance

This product should meet the standards of different Grass Matsubara drugs made of a stable homogeneous liquid, free from visible suspended matter and sediment.

3.2 Technical Specifications

Grass pine EC should be consistent with Table 1 requirements.

Table 1 Song Yi Cao EC Control Project Index

project

index

480g/L 360g/L

Grass loose concentration (20 °C) / (g/L) or mass fraction of a /% + 24-24 480 45.0 + 2.2-2.2 + 18-18 360 35.0 + 1.7-1.7 Penetrant (Azone) mass fraction b /% >= - 2.0 Penetration time/s <= - 150 Moisture /% <= 0.5 pH range of 5.0 to 8.0 Emulsion stability (diluted 200 times) Qualified Low temperature stability Qualified c Thermal storage stability c qualified when a dispute occurs when mass to the mass fraction of arbitration.

b allow additional penetrant, other detection methods and its corresponding index requirements in the National Standardization Technical Committee Pesticide obtained.

Thermal storage stability test when c normal production, low-temperature stability measured at least once every three months.

Test Method 4

4.1 Sampling

According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determined by sampling a random number table method packages, the final sample size not less than 200mL.

4.2 Identification Test

--- The High Performance Liquid Chromatography with different identification test Determination of the mass fraction of loose grass simultaneously. In the same chromatographic operating conditions , The retention time of the standard solution and the sample solution to a chromatographic peaks iso Grass pine peak retention time, the relative difference should be 1.5% Fewer.

4.3 Determination of the mass concentration of pine and grass (mass fraction)

4.3.1 Method summary

Sample was dissolved in methanol, acetonitrile + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and UV detector 236nm wavelength, the sample of the different grass pine reverse phase HPLC separation and determination of external standard.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Grass Song Sample. a known mass fraction >=98.0%.

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5µm filler (or with equivalent effect color the column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.3.4 HPLC operating conditions

Mobile phase. phi (acetonitrile. water) = 50.50, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

Column temperature. room temperature (temperature change should not exceed 2 °C);

Detection wavelength. 236nm;

Injection volume. 5µL;

Retention time. iso

Grass pine 11.0min.

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 differences

EC loose grass HPLC is shown in Figure 1.

1 --- Yi Cao loose.

1 Yi Cao Song EC HPLC diagram

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 0.2g (accurate to 0.0002g) and grass loose standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark.

Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.2 Preparation of sample solution

Weigh Iso

Grass pine 0.2g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark, shake uniform. Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol 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 iso Peak area becomes relatively loose grass After less than 1.2% of the solution in accordance with the sample solution, the sample solution and standard sequence of the standard solution was measured.

4.3.6 Calculation

The measured before and after the two-needle sample solution and sample two different doses of the standard solution Grass Pine Peak area were averaged. Sample different Grass loose mass fraction of 1 (%) according to equation (1) calculation; (2) to calculate the concentration of rho1 (g/L) by the formula.

1 = A2

rho1 =

10 (2)

Where.

A1 --- the average standard solution and grass Pine Peak area;

A2 --- sample solution and grass Pine mean peak area;

Density rho --- 20 °C when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured);

--- Yi Cao Song Sample mass fraction, expressed as a percentage.

4.3.7 Allowable difference

The measurement results grass loose mass fraction of the difference between the two parallel should not exceed 0.8%, and the arithmetic mean as a measurement result.

4.4 Determination of the mass fraction of nitrogen-one

4.4.1 Method summary

Sample was dissolved in acetonitrile to acetonitrile + water as the mobile phase, to use as filler HypersilGOLDC18 stainless steel column and UV detection it is, at a wavelength of 210nm on the sample under nitrogen ketone HPLC separation and determination, external standard.

4.4.2 Reagents and solutions

Acetonitrile. chromatographic pure;

Water. freshly distilled twice-distilled water by membrane filtration;

Azone standard. a known mass fraction >=99.0%.

4.4.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatography data workstations;

Column. 150mm × 4.6mm (i.d.) Stainless steel column. The filler is HypersilGOLDC18, particle diameter of 5 m;

Micro injector. 50µL;

Filter. pore size of 0.45µm.

4.4.4 HPLC operating conditions

Mobile phase. phi (acetonitrile. water) = 90.10, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

Column temperature. room temperature;

Detection wavelength. 210nm;

Injection volume. 10µL;

Retention time. Azone 6.2min.

Above are typical operating parameters can be given operating parameters adjusted as appropriate depending on the characteristics of the instrument, in order to obtain the best results. Texts Type of 360g/L EC in pine and grass Azone HPLC is shown in Figure 2.

1 --- azone.

Figure 2 Yi Cao Song EC Azone determined by high performance liquid chromatogram

4.4.5 Measuring step

4.4.5.1 Preparation of standard solution

Weigh Azone standard 0.02g (accurate to 0.0002g), placed in 100mL flask, add acetonitrile dissolved and diluted to the mark with the mobile phase Degree, shake.

4.4.5.2 Preparation of the sample solution

Weigh the sample 1g (accurate to 0.0002g), placed in 100mL flask, add acetonitrile dissolved in mobile phase and dilute to the mark.

4.4.5.3 Determination

Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculate the response of the needle, two needles to be adjacent ring Relative change value should be less than 1.0%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.

4.4.6 Calculation

The peak area was measured before and after the two-needle sample solution and two doses of the standard sample solution Azone are averaged for sample quality Azone 2 volume fraction (%), according to equation (3) Calculated.

2 = A2

Where.

A1 --- Azone mean standard peak area;

The average value A2 --- sample Azone peak area;

--- Azone standard mass fraction, expressed as a percentage.

4.4.7 Allowable difference

Results of two parallel determination of nitrogen content of ketone relative deviation should not exceed 10% of the arithmetic mean value as a measurement result.

4.5 Determination of the penetration time

4.5.1 Instruments

Beaker.200mL;

Pipette. 2mL;

Straight cylinder. 100mL;

Thermometer. 0 °C ~ 100 °C;

Constant temperature water bath. 25 °C ± 2 °C;

Cotton cloth. 21 × 21 3 shares 3 shares fine canvas, wafers having a diameter of 30.0mm spare.

4.5.2 Measuring step

With pipette sample 0.4mL, the sample was slowly dropped into a beaker filled with distilled water of 200mL, stir gently with a glass rod.

The beaker was placed in a water bath to keep the temperature of the solution in the beaker at 25 °C ± 2 °C. Beaker until the solution surface of the foam disappears and canvas circle Sheet placed on the rear surface of the solution, use a stopwatch, canvas discs until settle to the bottom of the beaker, records from flat to settle to the bottom of the canvas used Time (in seconds). Repeat the test more than 10 times, and the arithmetic mean of the difference between the 20s and the average of the above data rounding, and then averaged Value, that is, penetration time.

4.5.3 Calculation

Where.

--- Like the number of measurement samples.

4.6 Determination of Moisture

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

According to GB/T 1601 carried out.

4.8 Emulsion stability test

Standard hard water sample was diluted 200-fold, according to GB/T 1603 test, the non-oil slick, no precipitation under qualified.

4.9 Low temperature stability test

According to GB/T 19137 in "homogeneous emulsion and liquid preparations", in the bottom of the centrifuge tube educt volume does not exceed 0.3mL qualified.

4.10 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. After the heat storage and grass pine content shall not be less than 97% before the heat storage, emulsion stability should Meet the requirements of this standard is qualified.

4.11 Product inspection and acceptance

Shall comply with GB/T 1604's. Limit the use of numerical treatment rounding value comparison method.