GB 28151-2011Pyrimethanil wettable powders (English PDF)

3.1 Composition and appearance

This product should be compliant pyrimethanil original drug with suitable additives and fillers processing is made uniform loose powder, there should be no lumps.

3.2 Technical Specifications

Pyrimethanil WP shall comply with the requirements in Table 1.

Table 1 pyrimethanil WP Control Project Index

project

index

20% 40%

Pyrimethanil mass fraction /% 20.0 40.0 2.0-2.0 1.2-1.2 Moisture /% <= 3.0 pH range 6.0 to 10.0

Table 1 (continued)

project

index

20% 40%

Suspension rate /% >= 80 Wetting time/s <= 90 Fineness (through 45µm standard sieve) /% >= 98 Thermal storage stability of a /% qualified when a normal production, heat storage stability test for detection of 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 "on solid preparation sampling" approach. Determining sample package using a random number table method; the final sample size not less than 300g.

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 WP HPLC is shown in Figure 1.

1 --- pyrimethanil.

Figure 1 pyrimethanil WP High Performance Liquid Chromatographic

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 the mobile phase Dilute to the mark. With pipette 5mL said test solution to another 50mL volumetric flask mobile phase and dilute to the mark.

By membrane filtration and set aside.

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 poor quality score of two parallel determination results, 20% pyrimethanil WP should be no more than 0.5%, 40% wettable Pyrimethanil Powders should not exceed 0.8%, respectively, the arithmetic mean value as a measurement result.

4.5 Determination of Moisture

According to GB/T 1600 in the "azeotropic method".

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

4.7 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 Suspension 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. into the cylinder remaining 25mL of the suspension was added 5mL accurate Internal standard solution, then add 5mL chloroform extracted thoroughly shaken to make it, to stand, to take lower organic phase, refer to Appendix B of the method for determining pyrimethanil Amine quality, calculate the suspension rate. )

4.8 Determination of wetting time

According to GB/T 5451 carried out.

4.9 Determination of fineness

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

4.10 Thermal storage stability test

According to GB/T 19136 in "powder formulations" 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.

4.11 Product inspection and acceptance

Shall comply with GB/T 1604's.

5.1 Marking, labeling, packaging

Pyrimethanil wettable powder marking, labeling and packaging should comply with the provisions of GB 3796.

Pyrimethanil WP packaging applications, clean, dry bag or aluminum foil composite film bag, net weight 50g, 100g, 200g, 250g. Also available upon request or order agreement other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

Pyrimethanil WP package should be stored in well-ventilated, dry coffers. Storage and transportation, to prevent moisture and sunlight, no food, seed Child, 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, once ingested, immediately sent to hospital symptomatic treatment.

5.4 Warranty Period

Under the specified conditions of storage, pyrimethanil guarantee amine wettable powder, 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 chloroform, di-n-butyl phthalate as the internal standard, using a HP-5 capillary column as filler and flame Ionization detector to sample the Pyrimethanil gas chromatography separation and determination of internal standard.

B.2 Reagents and solutions Chloroform;

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, dissolve and dilute to the mark with chloroform Degree, 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 WP and the internal standard gas chromatography is shown in Figure B.1.

1 --- pyrimethanil;

2 --- internal standard.

Figure B.1 pyrimethanil WP 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 according to formula (B.1) Calculated.

w1 = 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 poor quality score of two parallel determination results, 20% pyrimethanil WP should be no more than 0.5%, 40% wettable Pyrimethanil Powders should not exceed 0.8%, respectively, the arithmetic mean value as a measurement result.

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