GB 28150-2011Chlorsulfuron water dispersible granules (English PDF)

3.1 Composition and appearance

This product should meet the criteria of the drug and chlorsulfuron suitable auxiliaries and processed into filler, dry, flowable uniform particles, no See the foreign objects and lumps.

3.2 Technical Specifications

Chlorsulfuron water dispersible granules should meet the requirements of Table 1.

Table 1 chlorsulfuron control water dispersible granules Item Index

project

index

25% 75%

Chlorsulfuron mass fraction /% 2.5-2.5 25.0 1.5-1.5 75.0 Moisture content /% <= 2.0 TABLE 1 (cont.) project index 25% 75% the pH range of 5.0 to 7.0 Wetting time/s <= 15 Wet sieve test (Test through 44µm sieve) /% >= 98 Suspension rate /% >= 90 Particle size (355µm ~ 1430µm) /% >= 98 Dispersibility /% >= 80 Persistent foaming (amount of foam after 1min)/mL <= 40 Passing a heat storage stability test when a normal production, the thermal storage stability test 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 "commodity solid preparation sampling" approach. Determining Sample packages with a random number table method; final draw Sample size should be no less than 1000g.

4.3 Identification Test

The present liquid chromatography --- identification test can be carried out simultaneously with the determination of the mass fraction of chlorsulfuron. Chromatography under the same operating conditions, the test Comp retention time of the standard solution chlorsulfuron peak retention time of a peak solution, the relative difference of 1.5% should be or less.

4.4 Determination of the mass fraction of chlorsulfuron

4.4.1 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.

4.4.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Glacial 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%.

4.4.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor;

Column. 150mm × 3.9mm (id) stainless steel column Nova-PakC18 filler contents (or equivalent effect 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.CH3COOH) = 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 water dispersible granules by HPLC is shown in Figure 1.

1 --- chlorsulfuron.

FIG 1 chlorsulfuron water-dispersible granules by HPLC FIG.

4.4.5 Determination Step

4.4.5.1 Preparation of standard solution

Weigh 0.05g chlorsulfuron standard (accurate to 0.0001g), a 100mL volumetric flask, dilute to volume with methanol solution of ammonia, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaking.

4.4.5.2 Preparation of sample solution

Weigh 0.05g of chlorine-containing specimens chlorsulfuron (accurate to 0.0001g), a 100mL volumetric flask, diluted with methanol solution of ammonia to Scale, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaken and filtered.

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 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.

4.4.6 Computing

The mass fraction of the sample according to chlorsulfuron formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

W1 --- chlorsulfuron sample mass fraction in%;

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

M1 --- Sample 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).

4.4.7 Allows poor

Results replicates difference chlorsulfuron twice the mass fraction of 75% water dispersible granule should be less than 1.0%; 25% water-dispersible granules should not 0.5%, respectively, and the arithmetic mean value as a measurement result.

4.5 Determination of Moisture

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

4.6 PH value measured

Carried out in GB/T 1601.

4.7 Determination of the suspension rate

Proceed as GB/T 14825-2006 4.1. Weigh 0.2g of chlorine-containing specimens chlorsulfuron (accurate to 0.0001g), the bottom of the cylinder 25mL whole suspension was transferred to 100mL volumetric flask, with ammonia in methanol to volume, shaken at 3min ultrasound, static Set, after filtration, was measured according to 4.4 mass chlorsulfuron, calculate suspensibility.

4.8 Determination of wetting time

Carried out in GB/T 5451.

4.9 Determination of fineness

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

Determination of particle size 4.10

4.10.1 Instruments

Group standard sieve. aperture (355µm ~ 1430µm);

Sieve Shaker. amplitude of 25mm, 1400 times/min.

4.10.2 Measuring step

The standard sieve vertically stacked, placed in a small sieve large particle size above a particle size sieve, sieve bottoms receiving pan while the combination of a good set of fixed sieve vibrating sieve Machine, accurately weighed sample 100g water dispersible granules (accurate to 0.1 g of), placed on the top sieve, stamped seal, shock promoter sieve shaker 5min, Collecting a predetermined size range sieve was weighed (to the nearest 0.1g).

4.10.3 Computing

The particle size of the sample according to the formula (2).

w2 = m1m × 100

Where.

--- size w2 of the sample, expressed in%;

--- M1 predetermined oversize mass within the particle diameter range in grams (G);

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

Determination dispersible 4.11

4.11.1 Method summary

The amount of water in water dispersible granules was added under stirring and mixing to prepare a suspension, after standing for some time, removing a top 9/10 Suspension, and 1/10 bottom drying the precipitate was measured gravimetrically.

4.11.2 Reagents and equipment

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

Beaker. 1000mL, inner diameter (102 ± 2) mm;

Electric mixer. with speed control (0 ~ 1000) r/min;

Stainless steel stirring rod (see FIG. 2). with 4 fixed propeller stirring blade stirring bar, the angle between the blades is 45 °;

A rotary vacuum evaporator;

Stopwatch.

4.11.3 Measuring step

At 20 °C ± 1 °C, standard hard water was added to the 900mL beaker, stir bar is fixed in the center of the beaker, stirring the beaker from the blade bar Bottom 15mm, and a stirring blade pitch rotation direction advancing the rod to ensure that the liquid swirls up stir bar, a speed of opening 300r/min of A stirrer, a water-dispersible granules 9g sample (to the nearest 0.1g) was stirred in water was added, stirring was continued for 1min. Close stirring, the suspension was Stand for 1min, 9/10 withdrawn suspension (810mL), the entire operation should be completed within 30s ~ 60s, slender glass tube and held beginning tip in the final level, and the suspension is possible without stirring, 90mL of water was distilled off remaining suspension using a rotary vacuum evaporator, from 60 °C ~ at 70 deg.] C and dried to constant weight, weighed (to the nearest 0.1g).

4.11.4 Computing

Dispersion of the sample according to equation (3) is calculated.

w3 = 10

(M-m1)

9m × 100

Where.

W3 --- dispersibility of the sample, expressed in%;

m --- the mass of the sample taken, in grams (G);

After mass M1 --- dried residue, in grams (g).

In millimeters

FIG 2 stainless stirring rod

4.12 Persistent foaming test

4.12.1 Method summary

A predetermined amount of sample is mixed with standard hard water, the foam volume recorded on standing.

4.12.2 Reagent

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

4.12.3 Instruments and Appliances

Stoppered graduated cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL scale line to the bottom of the stopper 4cm ~ 6cm);

Industrial balance. a sense of the amount of 0.1g.

4.12.4 Measuring step

Was added 180mL graduated cylinder standard hard water, 1.0g sample was weighed into a measuring cylinder (to the nearest 0.1 g of), was added to the standard hard water from the cylinder 9cm scale line of the bottom plug, 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.

4.13 Thermal storage stability test

According to GB/T 19136 in the "solid preparation" performed. After the heat storage mass chlorsulfuron fraction should be not less than 97% of the average content before storage, the suspension shall comply with the requirements for the standard rate is still qualified.

4.14 Product inspection and acceptance

Shall comply with the provisions of GB/T 1604's.

5.1 Marking, labeling, packaging

Flag chlorsulfuron water dispersible granules, labeling, packaging should meet the requirements of GB 3796; chlorsulfuron water dispersible granules aluminized plastic applications or composite aluminum bag. The user may also request or order protocol, other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

Chlorsulfuron package WDG airiness, dry place; storage and transportation, prevent moisture and sunlight, no food, seed Promoter, feed-mixing, 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 Warranty Period

Warranty. Storage conditions specified in, chlorsulfuron guarantee water dispersible granules, from two years from the production date.

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.

1102-