GB 28152-2011Pyrimethanil aqueous suspension concentrates (English PDF)

3.1 Composition and appearance

This product should be compliant pyrimethanil original drug, additives and fillers processed and should be mobile, easy to measure the volume of liquid suspension, deposit Discharge may occur during precipitation, but after shaking, restitution should, there should be no lumps.

3.2 Technical Specifications

Pyrimethanil SC shall meet the requirements of Table 1.

Table 1 pyrimethanil SC Control Project Index

project

index

20% 30% 40%

Pyrimethanil mass fraction /% 20.0 40.0 2.0-2.0 1.5-1.5 1.2-1.2 30.0 pH range 6.0 to 10.0 Suspension rate /% >= 90

Table 1 (continued)

project

index

20% 30% 40%

Pourability /%

After pouring the residue <= 5.0 After washing the residue <= 0.5 Wet sieve test (through 75µm test sieve) /% >= 98 Persistent foaming (foam volume after 1min)/mL <= 30 Low temperature stability of a /% qualified Thermal storage stability of a /% qualified when a normal production, low temperature stability, thermal storage stability test was measured at least once every three months.

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 600mL.

4.3 Identification Test

HPLC --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyrimethanil. In the same chromatographic operating conditions , The retention time of the standard solution and the sample solution to a peak of pyrimethanil retention time, the relative difference should be less than 1.5%.

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

When using the above method for identification of effective ingredients have questions, other effective methods can be used for identification.

4.4 Determination of the mass fraction of pyrimethanil

4.4.1 Method summary

Sample dissolved in mobile phase, methanol aqueous phosphoric acid as the mobile phase, use as filler to C18 stainless steel column and UV detector (300nm), the sample of Pyrimethanil high performance liquid chromatography, external standard. It can also be measured using gas chromatography, operation See Appendix B. for conditions

4.4.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Phosphoric acid;

Pyrimethanil standard. Known pyrimethanil mass fraction w>=98.0%.

4.4.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor;

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.

4.4.4 HPLC operating conditions

Mobile phase. [Psi] [methanol. water (adjusted with phosphoric acid to pH = 3)] = 75.25, filtered through a filter membrane and degassed;

Flow rate. 1.0mL/min;

Column temperature. room temperature;

Detection wavelength. 300nm;

Injection volume. 5µL;

Retention time. pyrimethanil about 5.5min.

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 pyrimethanil SC HPLC is shown in Figure 1.

1 --- pyrimethanil.

Figure 1 pyrimethanil SC high performance liquid chromatogram

4.4.5 Measuring step

4.4.5.1 Preparation of standard solution

Weigh pyrimethanil standard 0.1g (accurate to 0.0001g), a 50mL volumetric flask, add the mobile phase was shaken mobile phase and dilute to Mark and shake. With pipette 5mL said test solution to another 50mL volumetric flask mobile phase and dilute to the mark.

4.4.5.2 Preparation of sample solution

Weigh containing pyrimethanil 0.1g sample (accurate to 0.0001g), a 50mL volumetric flask, add the mobile phase was shaken with dilute phase flow Release to the mark. With pipette 5mL said test solution to another 50mL volumetric flask mobile phase and dilute to the mark. through Membrane filter.

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 Pyrimethaml 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.

4.4.6 Calculation

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

w1 = A2

· M1 · w

A1 · m2

Where.

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

A2 --- sample solution, pyrimethanil amine mean peak area;

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

w --- Sample pyrimethanil mass fraction, expressed as a percentage;

A1 --- standard solution, pyrimethanil amine mean peak area;

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

4.4.7 Allowable difference

Pyrimethanil parallel determination of the mass fraction of the difference between the two results, the 20% pyrimethanil content should be less than 0.5%, and 30% of the mass fraction of Pyrimethanil the number should be less than 0.6%, 40% pyrimethanil content should not exceed 0.8%, respectively, the arithmetic mean value as a measurement result.

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

4.6 Determination of the suspension rate

According to GB/T 14825 performed. Weigh 1g sample (accurate to 0.0001g). The cylinder with 50mL methanol remaining 25mL suspended Floating liquid and precipitate all transferred to 100mL volumetric flask with methanol to the mark, under ultrasonic oscillations 5min, shake, filtration.

4.4 Determination of pyrimethanil according to quality, calculate the suspension rate (gas chromatography. the inner cylinder remaining 25mL suspension and sediment transfer all to 100mL beaker, vacuum drying oven at 60 °C to nearly dry, measurement method, see Appendix B pyrimethanil quality, calculate the hanging Floating rate).

4.7 Test dumping

4.7.1 Method summary

Will be placed in the container suspending sample placed after a certain time, in accordance with the procedure laid dumping determined trapped in the sample container Volume; the vessel was washed with water, the amount of the sample container and then measured.

4.7.2 Instruments

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

4.7.3 Measuring step

Mix well enough samples, some of which will be placed in time already weighed cylinder (including plug), and attached to the cylinder volume of 8 Office, plug Tight grinding gag, weighed, placed 24h. The tap is opened, the upright position of the rotating cylinder by a 135 °, pouring 60s, then invert 60s, re-weighed amount Tube and stopper.

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

4.7.4 Calculation

The residue mass fraction and mass fraction of the residue washed after dumping respectively formula (2) and (3) Calculated.

w2 = m2-m0m1-m0

w3 = m3-m0m1-m0

Where.

The residue mass fraction w2 --- after dumping, expressed as a percentage;

After m2 --- dumping, quality cylinder, grinding gag and residue, in grams (g);

m0 --- cylinder, quality is more important after grinding gag constant in units of grams (g);

m1 --- cylinder, grinding gag and quality of the sample, in grams (g);

The residue mass fraction w3 --- washed in%;

--- Washing m3, the quality of the cylinder, grinding gag and residue, in grams (g).

4.8 Wet sieve test

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

4.9 Persistent foaming

4.9.1 Method summary

The samples and standards prescribed amount of mixing hard water, foam volume after standing record.

4.9.2 Reagents

Standard hard water. rho (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0.

4.9.3 Instruments

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

Balance. a sense of the amount of 0.1g, range 500g.

4.9.4 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), added to hard water Plug from the cylinder to the mark at the bottom of 9cm, back cover plug for the bottom of the cylinder as the center, upside down 30 times (2s). On test bench on standing 1min, record lather volume.

4.10 Low temperature stability test

According to GB/T 19137 method "suspension formulation" provision was. 4.8 Determination by wet sieve test, and the results meet the standard requirements qualified.

4.11 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. After the thermal storage, pyrimethanil content should not be lower than the measured thermal storage mass fraction ago 97% rate is still suspended shall meet the standards.

4.12 Product inspection and acceptance

Shall comply with GB/T 1604's.

5.1 Marking, labeling, packaging

Pyrimethanil suspending signs, labels, packaging shall comply with the provisions of GB 3796.

Pyrimethanil SC packaging applications, clean, dry cover with plastic bottles, net weight 80g, 100g, 200g. also may According to user requirements or other forms of ordering agreement package, subject to the provisions of GB 3796.

5.2 Storage

Pyrimethanil SC 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

Pyrimethanil as low toxicity fungicides, are swallowed and inhaled toxic, irritating to the eyes, the FDA should wear protective equipment, after application Wash with soap, if ingested, immediately sent to hospital symptomatic treatment.

5.4 Warranty Period

Under the specified conditions of storage, pyrimethanil guarantee amine suspension of two years from date of manufacture.

Appendix A

(Informative)

Other names pyrimethanil, structural formula and basic physicochemical parameters this product is an active ingredient pyrimethanil other name, structural formula and basic physicochemical parameters are as follows.

ISO common name. Pyrimethanil CAS Registry Number. 53112-28-0 CIPAC Numeric Code. 714 Chemical name. N- (4,6- dimethyl-pyrimidin-2-yl) aniline Structure.

Empirical formula. C12H13N3 Molecular Weight.199.25 Biological activity. bactericidal Melting point. 96.3 °C Vapor pressure (25 °C). 2.2 × 10-3Pa Solubility (20 °C, g/L). water 0.121 (pH = 6.1,25 °C), 389 acetone, ethyl acetate, 617, 1000 dichloromethane, n-hexane 23.7, 412 toluene, methanol 176 Stability. Stability in water pH dependent, 54 °C save 14d stability.

Appendix B

(Informative)

Pyrimethanil mass fraction of gas chromatographic method B.1 Method summary Sample was dissolved in dimethylformamide, di-n-butyl phthalate as the internal standard, using a HP-5 capillary column for the filler and hydrogen Flame ionization detector, the sample of Pyrimethanil and measured by gas chromatography, internal standard.

B.2 Reagents and solutions dimethylformamide;

Pyrimethanil standard. a known mass fraction w>=98.0%;

Internal standard. di-n-butyl phthalate, should not interfere with the analysis of impurities;

Internal standard solution. Weigh-n-butyl phthalate 3.5g, set 250mL flask, dissolved in dimethyl formamide and diluted to Mark and shake.

B.3 Instruments

Gas chromatograph. with a hydrogen flame ionization detector;

Chromatography or chromatography workstation processor;

Column. 30m × 0.32mm (id) capillary column bonded HP-5 (5% phenyl methyl silicone), a film thickness of 0.25µm.

B.4 GC operating conditions Temperature (°C). 180 column temperature, the gasification chamber 250, the detector chamber 260;

Gas flow rate (mL/min). carrier gas (N2) 2.0, hydrogen gas 30, air 300;

Injection volume. 1.0µL;

Retention time (min). 3.9 pyrimethanil, internal standard 6.3.

Said gas chromatography system operating conditions typical operating parameters. It is given the operating parameters adjusted as appropriate depending on the characteristics of the instrument to to obtain the best results. Typical pyrimethanil SC and the internal standard gas chromatography is shown in Figure B.1.

1 --- pyrimethanil;

2 --- internal standard.

Figure B.1 pyrimethanil SC and the internal standard gas chromatograph

B.5 measuring step

B.5.1 preparation of standard solution Weigh pyrimethanil standard 0.05g (accurate to 0.0001g), placed in a glass bottle with a stopper with a pipette 5mL internal standard solution, Shake well.

Preparation B.5.2 the sample solution Weigh sample containing about Pyrimethaml 0.05g (accurate to 0.0001g), and placed in a stoppered glass vial with pipette 5mL internal standard solution Liquid, shake.

B.5.3 Determination

Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculated for each needle pyrimethanil and the internal standard peak area the ratio of repeatability to be two adjacent needles Pyrimethaml relative change compared with the internal standard peak area of less than 1.2%, the standard sample solution in accordance with the specimen Solution, sample solution, the order of the standard solution was measured.

B.6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution pyrimethanil and the internal standard peak area ratio of the average, respectively.

Pyrimethanil sample mass fraction w1 (%) according to equation (B.1) Calculated.

r2 · m1 · w

r1 · m2

Where.

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

r2 --- sample solution, pyrimethanil and mean internal standard peak area ratio;

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

w --- Sample pyrimethanil mass fraction, expressed as a percentage;

r1 --- standard solution, pyrimethanil and mean internal standard peak area ratio;

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

B.7 allowable difference Pyrimethanil parallel determination of the mass fraction of the difference between the two results, the 20% pyrimethanil content should be less than 0.5%, and 30% of the mass fraction of Pyrimethanil the number should be less than 0.6%, 40% pyrimethanil content should not exceed 0.8%, respectively, the arithmetic mean value as a measurement result.