GB 28133-2011Chlortoluron wettable powders (English PDF)

3.1 Composition and appearance

This product should meet the criteria of the drug and chlorotoluron appropriate processing auxiliaries and fillers are made as a loose powder consisting of uniform, without clumps.

3.2 Project and indicators

Chlorotoluron WP shall comply with the requirements of Table 1.

Table 1 chlorotoluron WP Control Project Index

Item Index

Chlorotoluron mass fraction /% 25.0 ± 1.5 1,1-dimethyl-3- (4-methylphenyl) urea mass fraction a /% <= 0.3 1-methyl-3- (3-chloro-4-methylphenyl) urea mass fraction a /% <= 0.3 Suspension rate /% >= 65 Moisture /% <= 3.0 TABLE 1 (cont.) Item Index pH of 6.0 to 9.0 Wetting time/s <= 90 Fineness (45µm test sieve) /% >= 96 (After 1min) Persistent foaming/mL <= 60 Passing a heat storage stability when a normal production, was measured at least once every three months.

Test Method 4

4.1 Sampling

In accordance with GB/T 1605-2001 of "solid preparation sampling" approach. Determined by randomly sampling package, not the amount of the final sample Less than 300g.

4.2 Identification Test

This identification test can be carried out simultaneously with the determination of the mass fraction of chlorotoluron. Chromatography under the same operating conditions, the color of a sample solution the peak retention time of the standard solution chlorotoluron peak retention time of which relative difference should be less than 1.5%.

4.3 Determination of mass fraction chlorotoluron

4.3.1 Method summary

Sample was dissolved in methanol, an aqueous solution of phosphoric acid to pH4.0 and acetonitrile as mobile phase, using a C18 packing of a stainless steel column and UV detection Detector, the sample chlorotoluron and high performance liquid chromatography assay.

4.3.2 Reagents and solutions

Phosphoric acid;

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Chlorotoluron Sample. chlorotoluron known mass fraction w>=99.0%.

4.3.3 Instruments

HPLC. UV detector with tunable wavelength;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (id) stainless steel column, built SHIMADZUVP-ODS5µm filler (or equivalent Effects column);

Filter. membrane pore size of about 0.45 m;

Ultrasonic cleaning.

4.3.4 HPLC operating conditions

Mobile phase. [Psi] [acetonitrile. water (phosphoric acid to adjust pH = 4)] = 50.50;

Flow rate. 1.0mL/min;

Column temperature. room temperature (a temperature change should be less than 2 deg.] C);

Detection wavelength. 243nm;

Injection volume. 25µL.

Retention time. chlorotoluron about 5.6min.

It is typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameter adjusted as appropriate, in order to obtain the best results.

25% HPLC chlorotoluron wettable powder shown in Figure 1.

1 --- chlorotoluron.

1 to 25% Wettable powders HPLC chlorotoluron FIG.

4.3.5 Determination Step

4.3.5.1 Preparation of standard solution

Chlorotoluron standard weighed about 0.1 g of (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol ultrasound volume. Pipette 5.0mL of this solution to another 50mL volumetric flask, diluted with methanol.

The sample solution prepared 4.3.5.2 Containing samples weighed approximately 0.1g of chlorotoluron (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol ultrasound volume.

The solution was pipetted 5.0mL at another 50mL volumetric flask, diluted with methanol. With 0.45µm pore size membrane filter, the filtrate was a sample Solution.

4.3.5.3 Determination

Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected, the needle until two adjacent peaks chlorotoluron area becomes relatively of less than 1.0%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.3.6 Computing

The two needle and the sample solution was measured before and after the two doses of the standard sample solution chlorotoluron peak area are averaged. Chlorotoluron mass fraction Number according to formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

--- sample mass W1 fraction chlorotoluron, expressed in%;

A2 --- sample solution, chlorotoluron average peak area;

M1 --- Sample mass in grams (G);

W --- Sample mass fraction in chlorotoluron, expressed in%;

A1 --- the standard solution, the average peak area chlorotoluron;

--- M2 sample mass, in grams (g).

4.3.7 Allows poor

The measurement results of the two parallel error should not exceed 1.0%, and the arithmetic mean value as a measurement result.

Determination of methyl-3- (4-methylphenyl) and 1- methyl-3- (3-chloro-4-methylphenyl) by mass of 1,1-4.4

4.4.1 Method summary

Sample was dissolved in methanol, an aqueous solution of phosphoric acid to pH4.0 and acetonitrile as mobile phase, using a C18 packing of a stainless steel column and UV detection , A sample of 1,1-dimethyl-3- (4-methylphenyl) and 1- methyl-3- (3-chloro-4-methylphenyl) for high performance liquid chromatography separation and Determination.

4.4.2 Reagents and solutions

Phosphoric acid;

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

1,1-dimethyl-3- (4-methylphenyl) urea standards. A known mass fraction w>=99.0%;

1-methyl-3- (3-chloro-4-methylphenyl) urea standards. A known mass fraction w>=99.0%.

4.4.3 Instruments

HPLC. UV detector with tunable wavelength;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (id) stainless steel column, built SHIMADZUVP-ODS5µm filler (or equivalent Effects column);

Filter. membrane pore size of about 0.45 m;

Ultrasonic cleaning.

4.4.4 HPLC operating conditions

Mobile phase. [Psi] [acetonitrile. water (phosphoric acid to adjust pH = 4)] = 50.50;

Flow rate. 1.0mL/min;

Column temperature. room temperature (a temperature change should be less than 2 deg.] C);

Detection wavelength. 243nm;

Injection volume. 25µL;

Retention time. 1,1-dimethyl-3- (4-methylphenyl) urea from about 3.7min; 1- methyl-3- (3-chloro-4-methylphenyl) urea about 5.1min.

It is typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameter adjusted as appropriate, in order to obtain the best results.

Chlorotoluron wettable powder 25% by HPLC of impurity in Figure 2.

1 --- 1,1-dimethyl-3- (4-methylphenyl) urea;

2 --- 1-methyl-3- (3-chloro-4-methylphenyl) urea.

2 to 25% Wettable powders chlorotoluron FIG impurities by HPLC

4.4.5 Determination Step

4.4.5.1 Preparation of standard solution

Weigh 1,1-dimethyl-3- (4-methylphenyl) Standards and 1-methyl-3- (3-chloro-4-methylphenyl) urea standard each about 0.04g (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol ultrasound, constant volume. The solution was pipetted 1.0mL 50mL volumetric flask to the other , Treated with methanol to volume.

The sample solution prepared 4.4.5.2 Chlorotoluron weighed 25% wettable powder of about 0.27 g of the sample (nearest 0.0002g), a 50mL volumetric flask, washed with methanol ultrasound Dissolving, constant volume. With 0.45µm pore size membrane filter, the filtrate as a sample solution.

4.4.5.3 Determination

Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution injection, each needle relative response value is calculated, the two phases to be adjacent to the needle Response changes less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.4.6 Computing

The two doses of the standard solution was measured before and after the sample solution and a sample two needles 1,1-dimethyl-3- (4-methylphenyl) Standards and 1-methyl -3- (3-chloro-4-methylphenyl) urea peak area are averaged. 1,1-dimethyl-3- (4-methylphenyl) urea [1-methyl-3- (3-chloro-4-methyl Phenyl) urea] mass fraction according to formula (2).

wi2 = Ai2

· Mi1 · wi0

Ai1 · m2

Where.

wi2 --- 1,1- dimethyl-3- (4-methylphenyl) urea [1-methyl-3- (3-chloro-4-methylphenyl) ureido] mass fraction in% representation;

--- AI2 sample solution, 1,1-dimethyl-3- (4-methylphenyl) urea [1-methyl-3- (3-chloro-4-methylphenyl) ureido] peak area level the mean;

mi1 --- 1,1- dimethyl-3- (4-methylphenyl) urea [1-methyl-3- (3-chloro-4-methylphenyl) ureido] Sample mass values 150 ,unit Grams (G);

--- Sample WI0 1,1-dimethyl (4-methylphenyl) urea [1-methyl-3- (3-chloro-4-methylphenyl) ureido] -3- mass score in% Representation;

AI1 --- the standard solution, 1,1-dimethyl-3- (4-methylphenyl) urea [1-methyl-3- (3-chloro-4-methylphenyl) ureido] peak area level the mean;

--- M2 value of the sample mass, in grams (g).

4.4.7 Allows poor

The measurement results of the two parallel opposing difference should be not more than 10%, and the arithmetic mean value as a measurement result.

4.5 Determination of the suspension rate

In accordance 14825-2006 GB/T "4.1 Method 1" is executed. He said sample of about 1.0g (accurate to 0.0002g), remain in the bottom of the cylinder 110 all suspensions and the residue was moved 100mL volumetric flask, dissolved in methanol ultrasound, constant volume. The solution was pipetted in another 10.0mL 50mL volumetric flask, diluted with methanol. With 0.45µm pore size membrane filter, the filtrate as a sample solution. 4.3 Determination of chlorotoluron by mass, (3) calculate suspensibility by the formula.

w2 = m1-m2m1 ×

9 × 100

Where.

--- suspension w2 of the sample rate, expressed in%;

M1 --- suspension formulation sample quality taken an active ingredient, in grams (G);

--- M2 remain in the active ingredient suspension 25mL bottom of the cylinder mass in grams (G);

--- conversion factor.

4.6 Determination of Moisture

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

4.7 PH value measured

Carried out according to the method specified in the 1601 GB/T .

4.8 Determination of wetting time

Carried out according to the method specified in GB/T 5451 in.

4.9 Determination of fineness

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

4.10 Persistent foaming test

4.10.1 Method summary

Mixing a predetermined amount of the sample with standard hard water, the foam volume recorded on standing.

4.10.2 Reagent

Standard hard water. rho (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0, according to GB/T 14825-2006 formulation.

4.10.3 Instruments

Stoppered graduated cylinder. 250mL [division value 2mL, (0 ~ 250) mL tick length between 20.0cm ~ 21.5cm, 250mL carved Line from the bottom of the stopper 4cm ~ 6cm];

Industrial balance. a sense of the amount of 0.1g, range 500g.

4.10.4 Measuring step

The cylinder was added to 180mL standard hard water scale line, and then the sample was added 1.0g, to the nearest 0.2g. Hard water is added to the cylinder plug from the bottom 9cm scale line portion, the plug cover to the bottom of the cylinder as the center, upside down 30 times (2s). Standing on the bench 1min, Foam volume recorded.

4.11 Thermal storage stability test

Carried out according to the method specified in "Powder Formulation" GB/T 19136 in. Chlorotoluron measured by the mass fraction of 4.3, the suspension ratio of 4.5 was measured.

After the heat storage mass fraction chlorotoluron, suspension rate indicator should still meet the requirements of Table 1 is acceptable.

4.12 Product inspection and acceptance

Shall comply with the relevant provisions of GB/T 1604's. Limit values rounding processing using the value comparison method.

5.1 Mark, label

Flag chlorotoluron WP, the label shall comply with the GB 3796, GB 20813 of the relevant provisions.

5.2 Packaging

Chlorotoluron wettable powder composite bag, the packaging material is appropriate plastic/plastic [BOPET (BOPA, BOPP) /dr.PO (modified PO)], a plastic/aluminum foil [BOPET (BOPA, BOPP) /dr.AL/ex.PO (modified PO)]. Net weight of not more than 500g, outside Packaging of corrugated cardboard boxes, each net content should not exceed 20kg. According to customer requirements, the use of other forms of packaging, subject to the provisions of GB 3796.

5.3 Storage

Package airiness, dry place. Storage and transportation, to prevent moisture and sunlight, not with food, seed, feed mix, avoid Eye contact with the skin, mouth and nose to prevent inhalation.

5.4 Security

Chlorotoluron herbicide is a low toxicity. The FDA should wear protective equipment should be washed with soap and water immediately after use. Such as drug Strayed into contact with skin or eyes, wash - with plenty of water; if eating poisoned, immediately fed with plenty of water and induce vomiting hospital symptomatic treatment.

5.5 Quality assurance of Under the provisions of storage and transportation conditions, chlorotoluron WP quality guarantee period of two years from date of manufacture.

Appendix A

(Informative)

Other names chlorotoluron and impurities, and the basic physicochemical parameters of the formula Other names, structural formulas and physicochemical parameters of the product substantially chlorotoluron active ingredients are as follows.

ISO common name. Chlorotoluron CIPAC Numeric Code. 217 CAS Registry Number. 15545-48-9 Chemical Name. 1,1-dimethyl-3- (3-chloro-4-methylphenyl) urea Structure.

Empirical formula. C10H13ClN2O Molecular weight. 212.7 Biological activity. weeding Melting point. 148.1 °C Vapor pressure. 0.005mPa (25 °C) Solubility (25 °C, g/L). 0.074 water, acetone, 54, 51 dichloromethane, ethanol, 48, 3 toluene, n-hexane 0.06, 21 n-octanol, acetic acid Ethyl ester 21 Stability. stable to UV light, strong acid or alkali decomposition slowly.

Impurities present standard names and structural formulas are as follows.

Chemical Name. 1,1-dimethyl-3- (4-methylphenyl) urea Structure.

Chemical Name. 1-Methyl-3- (3-chloro-4-methylphenyl) urea Structure.