GB 28134-2011Chlortoluron technical material (English PDF)

3.1 Composition and appearance

Chlorotoluron original drug appearance is white to pale yellow powder, without visible foreign matter.

3.2 Project and indicators

Chlorotoluron original drug should meet the requirements of Table 1.

Table 1 chlorotoluron original drug control project indicators

Item Index

Chlorotoluron mass fraction /% >= 95.0 1,1-dimethyl-3- (4-methylphenyl) urea mass fraction a /% <= 0.8 1-methyl-3- (3-chloro-4-methylphenyl) urea mass fraction a /% <= 0.8 Loss on drying /% <= 1.0 Mass of acetone insolubles fraction a /% <= 0.5 pH of 6.0 to 8.0 when a normal production, was measured at least once every three months.

Test Method 4

4.1 Sampling

Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Randomly sampled is determined by the package, the amount of the final sample number to 100g.

4.2 Identification Test

This identification test can be carried out simultaneously with the determination of the mass fraction of chlorotoluron. Under the same chromatographic operating conditions, the main sample solution Chromatography Retention time peak with 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 , A sample of chlorotoluron and high performance liquid chromatography assay.

4.3.2 Reagents and solutions

Phosphoric acid. AR;

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Chlorotoluron Sample. A 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 = 4.0)] = 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.

1 --- chlorotoluron.

FIG 1 chlorotoluron original drug HPLC 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, dissolve and dilute to volume with methanol, shake uniform. With pipetted 5.0mL above solution was placed further 50mL volumetric flask, dissolved in methanol and diluted to the mark.

The sample solution prepared 4.3.5.2 Chlorotoluron containing weighed about 0.1 g of (accurate to 0.0002g) sample, placed in a 50mL volumetric flask, dissolved in methanol and diluted to the mark with Degree, shake. With the above solution pipetted 5.0mL In another 50mL volumetric flask, dissolved in methanol and diluted to the mark.

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%, in order standard solution, sample solution, the sample solution and standard solution into the sample analysis.

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. Sample chlorotoluron Mass fraction by formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

W1 --- chlorotoluron sample mass fraction in%;

A2 --- average sample solution chlorotoluron peak area;

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

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

A1 --- standard solution chlorotoluron average peak area;

--- 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 = 4.0)] = 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.

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

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

FIG 2 chlorotoluron original drug impurities by HPLC FIG.

4.4.5 Determination Step

4.4.5.1 Preparation of standard solution

Weigh 1,1-dimethyl-3- (4-methylphenyl) urea Standards and 1-methyl-3- (3-chloro-4-methylphenyl) urea each about 0.04 standard g, fine Accurate to 0.0002g, a 50mL volumetric flask, dissolved in methanol ultrasound volume. The solution was pipetted 1.0mL to 50mL another capacity Flask, diluted with methanol, shake.

The sample solution prepared 4.4.5.2 Chlorotoluron original drug weighed sample of about 0.1g, accurate to 0.0002g, a 50mL volumetric flask, dissolved in methanol ultrasound volume. use 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 is injected until the peak area of the adjacent two pins is smaller than the relative change 1.2%, according to the standard solution, sample solution, the sample solution and standard solution were sequentially measured.

4.4.6 Computing

The two doses of the standard solution was measured before and after the two needles in the sample solution and a sample of 1,1-dimethyl-3- (4-methylphenyl) urea [1-methyl-3- (3-Chloro-4-methylphenyl) ureido] peak area are averaged. 1,1-dimethyl-3- (4-methylphenyl) urea [1-methyl-3- (3-chloro-4-methylphenyl) Ureido] 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 Units of G (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 loss on drying

4.5.1 Instruments

Oven. (105 ± 2) °C;

Weighing bottle. diameter 50mm, height 20mm;

Dryer.

4.5.2 Determination Step

The weighing bottle placed in an oven bake IH, placed in a desiccator taken cooled to room temperature, weigh (accurate to 0.0002g), repeating the steps Step, until a constant weight weighing bottle. 10g sample placed in a weighing bottle (paved weighed to the nearest 0.0002g), the weighing bottle placed in an oven , No capping, drying IH, taken affix cool to room temperature in a desiccator weigh (accurate to 0.0002g).

4.5.3 Computing

Loss on drying the sample by the formula (3) is calculated.

w3 = m1-m2m × 100

Where.

W3 --- Loss on drying, expressed in%;

M1 --- sample mass before drying and weighing bottles in grams (G);

--- M2 sample mass after drying and weighing bottles in grams (G);

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

4.6 Determination of acetone insolubles

According to GB/T 19138 carried out.

4.7 PH value measured

Carried out in GB/T 1601.

4.8 Product testing and acceptance

Product inspection and acceptance shall comply with GB/T 1604's. Process limit values, the comparison value using the rounding method.

5.1 Mark, label

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

5.2 Packaging

Chlorotoluron appropriate to the original drug compound bag, paper packaging material should/plastic, plastic/plastic. Net weight should not exceed 50kg. can According to user requirements or ordering agreement, other forms of packaging, it should comply with 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 drug in contact with eyes or skin, wash - plenty of water; if ingested poison, should immediately that is fed with plenty of water and induce vomiting hospital symptomatic treatment.

5.5 Acceptance of

Chlorotoluron of acceptance of the original drug for three months. From the date of delivery, product quality inspection is completed within three months, the indicators should meet Together standards.

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.

This standard name and basic physicochemical parameters of impurity of the formula as follows.

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

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