GB 28127-2011Chlorsulfuron technical material (English PDF)

3.1 Appearance

White powdery solid.

3.2 Technical Specifications

Chlorsulfuron TC should meet the requirements of Table 1.

Table 1 TC control chlorsulfuron Item Index

Item Index

Chlorsulfuron mass fraction /% >= 95.0 Moisture content /% <= 0.5 the pH range of 3.0 to 6.0 Mass acetone insoluble fraction a /% <= 0.5 when a normal production, the acetone insoluble matter content 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. Determined by sampling a random number table method packages, the amount of the final sample not less than 100g.

4.2 Identification Test

Optionally one of the following methods. When not identified using a method, it should then be determined using another method.

Infrared spectroscopy and chlorsulfuron --- Sample Sample infrared 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference.

Chlorsulfuron standard infrared spectra of Figure 1.

FIG 1 chlorsulfuron standard IR spectrum

HPLC --- This identification test can be carried out simultaneously with the determination of the mass fraction of chlorsulfuron. In the same chromatographic operating conditions Next, a peak in the sample solution and the retention time chlorsulfuron retention time of the standard solution chlorsulfuron peaks, the relative difference should 1.5% or less.

4.3 Determination of the mass fraction of chlorsulfuron

4.3.1 Method summary

Sample solution was dissolved in methanol with aqueous ammonia, acetic acid in acetonitrile and water as mobile phase, using Nova-PakC18 filler to a stainless steel column and a UV detector (230nm), the sample chlorsulfuron and high performance liquid chromatography assay.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Acetic acid;

Water. The new secondary steam distilled water;

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

Ammonia solution. [Psi] (ammonia. water) = 1.300;

Ammonia in methanol. [Psi] (ammonia solution. methanol) = 1.4;

Chlorsulfuron Sample. chlorsulfuron known mass fraction, w>=98.0%.

4.3.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor or workstation;

Color 150mm × 3.9mm (id) stainless steel column Nova-PakC18,5µm 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.

4.3.4 HPLC operating conditions

Mobile phase. [Psi] (acetonitrile. water. glacial acetic acid) = 40.60.0.5;

Flow rate. 1.0mL/min;

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

Detection wavelength. 230nm;

Injection Volume. 5µL;

Retention time. chlorsulfuron about 4.3min.

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 chlorsulfuron HPLC TC shown in Figure 2.

1- chlorsulfuron.

Figure 2 HPLC original drug chlorsulfuron

4.3.5 Determination Step

4.3.5.1 Preparation of standard solution

Weigh 0.05g chlorsulfuron standard (accurate to 0.0002g), a 100mL volumetric flask, dilute to volume with methanol solution of ammonia, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaking.

4.3.5.2 Preparation of sample solution

Weigh 0.05g of chlorine-containing specimens chlorsulfuron (accurate to 0.0002g), a 100mL volumetric flask, dilute to the mark with methanolic ammonia Degrees, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaking.

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 until the two needles chlorsulfuron relative change in peak area adjacent After less than 1.2%, 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 chlorsulfuron peak area are averaged. Sample chlorsulfuron Mass fraction by formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

--- the mass fraction of the sample W1 chlorsulfuron, expressed in%;

A2 --- sample solution, the average peak area chlorsulfuron;

M1 --- chlorsulfuron standard mass in grams (G);

W --- chlorsulfuron standard mass fraction in%;

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

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

4.3.7 Allows poor

Results difference chlorsulfuron replicates should be less than twice the mass fraction of 1.2%, and the arithmetic mean value as a measurement result.

4.4 Determination of moisture content

Carried out in GB/T 1600 in the Karl Fischer method.

4.5 PH value measured

Carried out in GB/T 1601.

4.6 Determination of the mass fraction of acetone insoluble

According to GB/T 19138 carried out.

4.7 Product testing and acceptance

It should conform to GB/T 1604 a predetermined limit value value comparison treatment using the rounding method.

5.1 Marking, labeling, packaging

Flag chlorsulfuron original drug, labeling and packaging should comply with the provisions of GB 3796. Drugs chlorsulfuron original clean plastic bag lined Bag or fiber drum lined with clean plastic bag, barrel net content is generally 25kg. The user may also request or order agreement Other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

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

5.3 Security

This product is a low toxicity of sulfonylurea herbicides. Are swallowed and inhaled toxic, it can penetrate through the skin. When using this product to avoid contact with the skin, After application with soap and rinse with water. Poisoning should immediately sent to hospital for symptomatic treatment.

5.4 Acceptance of

Chlorsulfuron original drug acceptance period is one month. From the date of delivery, product quality inspection completed within one month, the indicators should be consistent standard requirement.

Appendix A

(Informative)

Other names chlorsulfuron, structural formulas and physicochemical parameters of the basic this product is an active ingredient chloro other names, structural formulas and physicochemical parameters of the basic metsulfuron follows.

ISO common name. Chlorsulfuron CAS Registry Number. 64902-72-3 CIPAC Numeric Code. 391 Chemical name. 1- (2-chlorophenyl) -3- (4-methoxy-6-methyl-1,3,5-triazin-2-yl) urea Structure.

Empirical formula. C12H12ClN5O4S Molecular weight. 357.8 Biological activity. weeding Melting point. about 174 °C ~ 178 °C Vapor pressure (25 °C). 3nPa Solubility (22 °C, g/L). 57 acetone; dichloromethane 102; 14 methanol; toluene 3; hexane 0.01; water 0.1 ~ 0.125 (25 °C, pH4.1), 0.3 (25 °C, pH5) Stability. when dry, light stability; in the soil, due to hydrolysis and microbial degradation and damage; half-life in soil 150d ~ 160d.