GB 29383-2012Nicosulfuron technical material (English PDF)

3.1 Appearance

White to yellowish brown granular or powdery solid, without visible foreign matter and modifiers added.

3.2 Technical Specifications

Nicosulfuron original drug shall comply with the requirements in Table 1.

Table 1 nicosulfuron original drug quality control program indicators

Item Index

Nicosulfuron mass fraction /% >= 92.0 Dimethylformamide insolubles mass fraction a /% <= 0.3 Moisture /% <= 5.0 the pH range of 3.0 to 7.0 when a normal production, dimethylformamide insolubles content was measured at least once every three months.

Test Method 4

Safety Tips. to use this standard shall have practical experience of laboratory work. This standard does not indicate any safety issues. Make with those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the provisions of relevant state laws and regulations.

4.1 General provisions

This standard reagent in the absence of water and other requirements stated, refer to three predetermined analytical reagents and GB/T 6682-2008 of water. The test results performed by determining 4.3.3 rounding value in comparison 8170-2008 GB/T .

4.2 Sampling

Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determining Sample packages with a random number table method; final sample size not less than 100g.

4.3 Identification Test

Infrared spectroscopy --- standard sample and the infrared 4000cm-1 ~ 400cm-1 absorption spectrum range should not significantly different.

Sample IR spectrum shown in Figure 1.

FIG 1 nicosulfuron standard infrared spectra

The present liquid chromatography --- identification test can be carried out simultaneously with the measurement nicosulfuron mass fraction. Chromatography under the same operating conditions, Sample solution of a chromatographic peak with a retention time of the standard solution nicosulfuron retention time of the peaks, the relative difference should 1.2% or less.

4.4 Determination of nicosulfuron mass fraction

4.4.1 Method summary

Sample was dissolved in acetonitrile aqueous ammonia solution, acetic acid aqueous acetonitrile as the mobile phase, used as a filler stainless SymmetryC18 Column and a UV detector (240nm), the sample nicosulfuron and high performance liquid chromatography assay.

4.4.2 Reagents and solutions

Acetonitrile (HPLC grade);

Water. The new secondary steam distilled water;

glacial acetic acid;

Aqueous ammonia (NH3 · H2O). w (NH3) = 26% ~ 30%;

Ammonia solution. psi (H2O.NH3 · H2O) = 300.1;

Ammonia solution in acetonitrile. [Psi] (acetonitrile. ammonia solution) = 50.50;

Nicosulfuron Sample. nicosulfuron known mass fraction, w >=97.0%. (At 105 °C, 1h drying after use)

4.4.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor or workstation;

Color 250mm × 4.6mm (id) stainless steel column, SymmetryC185µm filler contents (or equivalent effect. Column Spectrum column);

Filter. membrane pore size of about 0.45 m;

Microsyringe. 50µL;

Quantitative sampling tube. 5µL;

Ultrasonic cleaning.

4.4.4 HPLC operating conditions

Mobile phase. psi (CH3CN.H2O) = 40.60, water with glacial acetic acid adjusted to pH 3.0;

Flow rate. 1.0mL/min;

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

Detection wavelength. 240nm;

Injection Volume. 5µL;

Retention time. nicosulfuron about 6.0min.

Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.

Typical nicosulfuron HPLC TC shown in Figure 2.

1 --- nicosulfuron.

Figure 2 HPLC nicosulfuron original drug

4.4.5 Determination Step

4.4.5.1 Preparation of standard solution

Weigh 0.05 g of (accurate to 0.0002g) nicosulfuron standard, a 50mL volumetric flask, 40mL of acetonitrile was added aqueous ammonia solution, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaken, ammonia water diluted to the mark with acetonitrile. Pipette with a pipette to the solution 10mL to 50mL volumetric flask, dilute to volume with acetonitrile and aqueous ammonia solution, shake.

4.4.5.2 Preparation of sample solution

Tobacco was weighed 0.05 g of ethyl (accurate to 0.0002g) sample, placed in a 50mL volumetric flask, 40mL of acetonitrile was added aqueous ammonia solution Solution, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaken, ammonia water diluted to the mark with acetonitrile. Pipette with a pipette to the solution 10mL to 50mL volumetric flask, dilute to volume with acetonitrile and aqueous ammonia solution, shake.

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 two adjacent needles nicosulfuron peak area becomes relatively After less than 1.2% of, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.4.5.4 Computing

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

w1 = A2

· M1 · w

A1 · m2

Where.

W1 --- sample nicosulfuron content, expressed in%;

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

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

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

W --- nicosulfuron standard mass fraction in%;

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

4.4.6 Allows poor

Results replicates difference nicosulfuron content twice, should not exceed 1.2%, and the arithmetic mean value as a measurement result.

Determination of insoluble material content of the amide methyl two 4.5

4.5.1 Reagents

dimethylformamide.

4.5.2 Instruments

Erlenmeyer flask. with a ground stopper, 250mL;

Sand core glass crucible. G3;

Oven. 105 °C ± 2 °C.

4.5.3 Determination Step

5g sample weighed (accurate to 0.01g), placed in 250mL Erlenmeyer flask, was added 100mL of dimethylformamide was heated at reflux 10min until all solubles were dissolved, the solution was filtered with a constant weight of the crucible, and then dimethylformamide 60mL conical flask was washed with three portions, and Filtration. The crucible was placed in an oven (105 °C ± 2 °C) dried 30min, then cooled to room temperature and weighed.

Dimethylformamide insolubles content according to formula (2).

w2 = m1-m0m × 100

Where.

--- dimethylformamide w2 of insolubles content, expressed in%;

After constant weight mass M1 --- crucible and the insolubles in grams (G);

M0 --- crucible mass in grams (G);

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

4.5.4 Allows poor

The measurement results of the two parallel relative deviation should not exceed 30%, and the arithmetic mean value as a measurement result.

4.6 Determination of Moisture

According to GB/T 1600 in the "Karl Fischer method", allowing the use of equivalent accuracy trace moisture analyzer.

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.

5.1 Marking, labeling, packaging

Flag nicosulfuron original drug, labeling and packaging should comply with the provisions of GB 3796; clean nicosulfuron original drug use bags lined with plastic Bag or cardboard drum lined with clean plastic bag, barrel net quality is generally 20kg. The user may also request or order agreement Other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

Nicosulfuron original drug package airiness, dry place; storage and transportation, prevent moisture and sunlight, no food, seeds and feed Feed mix, to avoid contact with the skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

This is a moderately toxic herbicide. Ingestion and inhalation are toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using this product Necessary to wear protective clothing. After application with soap and rinse with water. Coverage should be immediately sent to hospital for symptomatic treatment.

5.4 Acceptance of

Nicosulfuron original drug acceptance period of one month. From the date of delivery, product quality inspection completed within a month, the indicators should break Together standards.

Appendix A

(Informative)

Other names nicosulfuron, the basic structure and physico-chemical parameters this product is an active ingredient of smoke other names, structural formulas and physicochemical parameters of ethyl substantially as follows.

Common name. nicosulfuron ISO common name. nicosulfuron CAS Registry Number. 111991-09-4 Chemical Name. 2- (4,6-dimethoxypyrimidin-2-ylcarbamoyl sulfamoyl) -N, N- dimethyl-nicotinamide Structure.

Empirical formula. C15H18N6O6S Molecular weight. 410.4 Biological activity. Herbicides Melting point. 141 °C ~ 144 °C Vapor pressure. 1.6 × 10-11Pa (20 °C) Solubility (25 °C, g/kg). Water 3.59 (pH = 5 buffer solution), 12.2 (pH = 7 buffer solution), 39.2 (pH = 9 buffer solution Solution); acetone 18; Ethanol 4.5; chloroform, dimethylformamide, 64; 23 acetonitrile; toluene 0.37; n-hexane