GB 22617-2008Fenoxaprop-P-ethyl emulsifiable, oil in water (English PDF)

4.1 Sampling

According to GB/T 1605-2001 5.3.2 in "liquid formulation sampled" in. Determining sample package using a random number table method, the final sample the amount of not less than 1000mL.

4.2 Identification Test

HPLC --- The identification test with fine Determination oxazole diclofop content simultaneously. In the same chromatographic operation Under the conditions, the sample solution is a two peak retention time Azole grasses standard solution for the retention time of the two peaks of enantiomers relative of the difference should be less than 1.5%.

4.3 Determination of fine azole diclofop, fenchlorazole mass fraction

Determination 4.3.1 oxazole diclofop, fenchlorazole mass fraction

4.3.1.1 Method summary

Sample dissolved in mobile phase, n-hexane and isopropanol as the mobile phase, use ZORBAXSIL as filling a stainless steel column and variable wave Long UV detector, of the sample Oxazole diclofop, fenchlorazole normal phase HPLC separation and determination, external standard. also may Using capillary gas chromatography Oxazole diclofop mass fraction, chromatographic operating conditions, see Appendix A.

4.3.1.2 Reagents and solutions

Hexane. chromatography;

Isopropanol. chromatography;

Oxazole diclofop standard. a known mass fraction >=99.0%;

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

4.3.1.3 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 ZORBAXSIL, 5µm particle size of the filler;

Filter. pore size of about 0.45µm;

Micro injector. 100µL;

Quantitative sample line. 10µL;

Ultrasonic cleaner.

4.3.1.4 HPLC operating conditions

Mobile phase. [Psi] (n-hexane. isopropanol) = 90.10;

Flow rate. 0.8mL/min;

Column temperature. room temperature;

Detection wavelength. 230nm;

Injection volume. 10µL;

keep time.

Oxazole diclofop 4.8min, fenchlorazole 5.5min.

The above operating conditions, the Department of typical operating parameters, according to the characteristics of different instruments and columns for a given operating parameters to make appropriate adjustments to to obtain the best results. typical Oxazole diclofop HPLC water emulsion is shown in Figure 1.

1 --- oxazole diclofop;

2 --- fenchlorazole.

1 fine azole diclofop water emulsion by high performance liquid chromatogram

4.3.1.5 Measurement procedure

4.3.1.5.1 Preparation of standard solution

Weigh

Oxazole diclofop standard 0.05g, fenchlorazole standard 0.03g (accurate to 0.0002g), placed in 100mL volumetric flask.

80mL mobile phase in an ultrasonic bath shaking 5min make sample dissolution, removed after cooling to room temperature, dilute to the mark with the mobile phase, Shake well.

4.3.1.5.2 Preparation of sample solution

Weigh containing

0.05g oxazole diclofop sample (accurate to 0.0002g), placed in 100mL flask, add 80mL mobile phase in the ultrasonic bath shaking 5min make sample dissolution, removed after cooling to room temperature, mobile phase and dilute to the mark, shake, filtration.

4.3.1.5.3 Determination

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

4.3.1.6 Calculation

The measured before and after the two-needle sample solution and two doses of the standard sample solution Oxazole diclofop (fenchlorazole) peak areas are averaged.

Specimen

(1) Calculation azole diclofop (fenchlorazole) mass fraction of 1 (%) according to formula (2) to calculate the concentration of rho1 (g/L) by the formula.

rho1 =

Where.

A1 --- the standard solution, the average oxazole diclofop (fenchlorazole) peak area;

A2 --- sample solution, the average azole diclofop (fenchlorazole) peak area;

--- Standard samples azole diclofop (fenchlorazole) mass fraction,%;

4.3.1.7 Allowable difference

Two parallel determination results relative error should not exceed 5% of the arithmetic mean as a measurement result.

4.3.2 R- enantiomer ratio of measurement

4.3.2.1 Method summary

Sample dissolved in mobile phase, n-hexane and ethanol as the mobile phase, use a stainless steel ChiralcelOK as filler chiral column and variable wave Long UV detector, of the sample Oxazole diclofop R- enantiomer normal phase high performance liquid separation and determination of the spectrum, phase separation may also be used Other chiral column or flow when the phase.

4.3.2.2 Reagents and solutions

Hexane. chromatography;

Ethanol. chromatography;

Oxazole diclofop standard. a known mass fraction >=99.0%.

4.3.2.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (i.d.) Stainless steel chiral column, built ChiralcelOK, filler particle size of 10µm;

Filter. pore size of about 0.45µm;

Micro injector. 100µL;

Quantitative sample line. 20µL;

Ultrasonic cleaner.

4.3.2.4 HPLC operating conditions

Mobile phase. [Psi] (n-hexane. ethanol) = 50.50;

Flow rate. 1.3mL/min;

Column temperature. room temperature;

Detection wavelength. 280nm;

Injection volume. 20µL;

Retention time. R- enantiomer (fine azole diclofop) 8.4min, S- enantiomer 14.5min.

The above operating conditions, the Department of typical operating parameters, according to the characteristics of different instruments and columns for a given operating parameters to make appropriate adjustments to to obtain the best results. Typical fine Oxazole diclofop HPLC water emulsion is shown in Figure 2.

1 --- R- enantiomer (fine azole diclofop);

2 --- S- enantiomer.

Figure 2 oxazole diclofop fine water emulsion by high performance liquid chromatogram

4.3.2.5 Measurement procedure

4.3.2.5.1 Preparation of standard solution

Weigh

Oxazole diclofop standard of about 0.05g, placed in 100mL volumetric flask, dissolved in mobile phase and dilute to the mark.

4.3.2.5.2 Preparation of sample solution

Weigh about containing fine 0.05g oxazole diclofop sample, placed in 100mL volumetric flask, dissolved in mobile phase and dilute to volume, shake, filter.

4.3.2.5.3 Determination

Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles Oxazole diclofop R- enantiomers, S- enantiomer relative change in peak area is less than 1.0% (both enantiomers area ratio should be 50.50, deviation does not exceed 1%. If more than 1%, calculated oxazole diclofop R- enantiomer ratios should be corrected for), then two injection needles sample solution.

4.3.2.6 Calculation

Specimen

Oxazole diclofop R- enantiomer ratio of K, according to equation (3) Calculated.

AR + AS

Where.

AR --- two needles in the sample solution, oxazole diclofop mean R- enantiomer peak area;

AS sample solution --- two needles, oxazole diclofop mean S- enantiomer peak area.

When the standard sample solution when oxazole diclofop R- enantiomer area beyond the area of the two enantiomers and the (50 ± 1)%, the sample azole Wo Grass Ling R- enantiomer ratio of K ', according to equation (4) Calculated.

AR + AS (A'R/A'S)

Where.

A'R --- two doses of the standard solution, oxazole diclofop mean R- enantiomer peak area;

A'S --- two doses of the standard solution, oxazole diclofop mean S- enantiomer peak area.

4.3.3 Fine oxazole diclofop mass fraction calculation

The sperm sample

2 mass fraction (%) oxazole diclofop according to equation (5) to calculate the mass concentration rho2 (g/L) according to equation (6) Calculated.

2 = 1 × K (5)

rho2 = rho1 × K (6)

When the standard sample solution oxazole diclofop R- enantiomer area beyond the area of the two enantiomers and the (50 ± 1)%, sample fine azole Diclofop mass fraction '2 (%), according to equation (7) to calculate the mass concentration rho'2 (g/L) according to equation (8) Calculated.

'2 = 1 × K' (7)

rho'2 = rho1 × K '(8) According to GB/T 1601 carried out.

4.5 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.

4.6 Test dumping

4.6.1 Method summary

Once placed in a container of water emulsion sample placed certain period of time, in accordance with prescribed procedures dumping determined trapped in the sample container Volume; the vessel was washed with water, determination of the amount of sample in a container.

4.6.2 Instruments

With ground joint stopper cylinder. 500mL ± 2mL; cylinder height of 39cm, the upper and lower scale spacing 25cm (or equivalent for the determination of dumping Other containers of).

4.6.3 Test procedure

Mix well enough samples, some of which will be promptly placed already weighed cylinder (including plug), and is attached to 8/10 of the volume of the cylinder, Grinding plugged gag, weighed, placed 24h. The tap is opened, the upright position of the rotating cylinder by a 135 °, pouring 60s, then invert 60s, reweighed Tube and stopper.

After the equivalent of 80% of the cylinder volume of water (20 °C) was poured into a measuring cylinder, stoppered plug grinding mouth, pouring the cylinder 10 times, according to the above tilting operation Pour the contents of the third weighing cylinder and a stopper.

4.6.4 Calculation

The residue was 3 mass fraction (%) and the residue was poured after 4 mass fraction (%) after washing respectively of formula (9) and (10) calculated.

× 100 (9)

× 100 (10)

Where.

4.7 Persistent foaming test

4.7.1 Method summary

A sample with a predetermined amount of standard hard water mixed after recording still foam volume.

4.7.2 Reagents

Standard hard water. rho (Ca 2 ++ Mg2 +) = 342mg/L, pH = 6.0 ~ 7.0. According to GB/T 14825 preparation.

4.7.3 Instruments

With ground joint stopper cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL tick to plug Bottom 4cm ~ 6cm).

Industrial scale. a sense of the amount of 0.1g, load 500g.

4.7.4 Measuring step

The cylinder is added to 180mL standard hard water scale line at set cylinder on balance, weighed into the sample 1.0g (accurate to 0.1g), plus hard water from the bottom of the cylinder to the mark at 9cm, the cover plug for the bottom of the cylinder as the center, upside down 30 times (2s). On the test stand Standing 1min, record lather volume.

4.8 Low temperature stability test

According to GB/T 19137 in "homogeneous emulsion and liquid preparations" to. After mild agitation, it should be no visible particles and oil.

4.9 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. Fine grass azole azole diclofop reconciliation after the mass fraction of heat storage thermal storage mass allow the former dropped Volume fraction of 95%, emulsion stability should continue to meet the standards.

4.10 Product inspection and acceptance

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