GB 28155-2011Nicosulfuron oil-based suspension concentrates (English PDF)

3.1 Composition and appearance

This product should be compliant nicosulfuron original drug is made as flowability, easy to measure the volume of off-white liquid suspension, the storage process can Precipitation can occur, but after shaking, restitution should, there should be no lumps.

3.2 Technical Specifications

Nicosulfuron oil dispersible suspensions shall comply with the requirements in Table 1.

Table 1 nicosulfuron oil dispersible suspension control project indicators

project

index

40g/L 100g/L

Nicosulfuron mass fraction /% or concentration of a (20 °C) / (g/L) 10.0 1.0 to 1.0 4.1 0.4-0.4 404-410010-10

Table 1 (continued)

project

index

40g/L 100g/L

pH range of 3.0 to 7.0 Suspension rate /% >= 90 Wet sieve test (through 75µm test sieve) /% >= 98 Persistent foaming (foam volume after 1min)/mL <= 30 Dispersion stability qualified Dumping of b /% After pouring the residue <= After washing the residue <= 5.0 0.8 Thermal storage stability b qualified Low temperature stability Qualified b when a dispute occurs when mass to the mass fraction of arbitration.

B when normal production, dumping, thermal storage stability test, measuring low temperature stability test at least once every three months.

Test Method 4

Safety Tips. Use of this standard shall have practical experience of laboratory personnel work. This standard does not point out all of the safety issues. Make with those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the relevant national regulations.

4.1 General provisions

This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in water. Test results determined in accordance with GB/T 8170-2008 4.3.3 Rounding the value comparison method.

4.2 Sampling

According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determined by sampling a random number table method packages, the final sample size not less than 600mL.

4.3 Identification Test

HPLC --- The identification test can be carried out simultaneously with the determination of nicosulfuron mass fraction. In the same chromatographic operating conditions , The retention time of the standard solution and the sample solution to a peak of nicosulfuron chromatographic retention time, the relative difference should be 1.5% Fewer.

4.4 Determination of nicosulfuron mass fraction

4.4.1 Method summary

Sample was dissolved in acetonitrile, glacial acetic acid in aqueous acetonitrile as the mobile phase, to use as filler SymmetryC18 stainless steel column and ultraviolet Detector (240nm), the sample of nicosulfuron high performance liquid chromatography and determination.

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%;

Aqueous ammonia solution. Psi (H2O.NH3 · H2O) = 300.1;

Acetonitrile aqueous ammonia solution. Psi (acetonitrile. ammonia solution) = 50.50;

Nicosulfuron standard. a known mass fraction w>=97.0% (at 105 °C, 1h drying after use).

4.4.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or workstation;

Column. 250mm × 4.6mm (id) stainless steel column contents SymmetryC18,5µm filler;

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.4.4 HPLC operating conditions

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

Flow rate. 1.0mL/min;

Column temperature. room temperature (temperature change should not exceed 2 °C);

Detection wavelength. 240nm;

Injection volume. 5µL;

Retention time. nicosulfuron about 6.0min.

It said operating parameters are typical, according to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results.

Typical nicosulfuron oil dispersible suspensions HPLC is shown in Figure 1.

1 --- nicosulfuron.

Figure 1 nicosulfuron oil dispersible suspensions HPLC Fig.

4.4.5 Measuring step

4.4.5.1 Preparation of standard solution

Weigh 0.05g nicosulfuron standard (accurate to 0.0001g), a 50mL volumetric flask, add 40mL acetonitrile aqueous ammonia solution, Ultrasonic oscillation 5min to dissolve the sample was cooled to room temperature, shake, dilute to the mark with acetonitrile ammonia. Using a pipette to take the above solution 10mL to 50mL volumetric flask, dilute ammonia solution with acetonitrile to the mark.

4.4.5.2 Preparation of sample solution

Weigh Tobacco ethyl 0.05g sample (accurate to 0.0001g), a 50mL volumetric flask, add 40mL acetonitrile aqueous ammonia solution Liquid ultrasonic oscillations 5min to dissolve the sample was cooled to room temperature, shake, dilute to the mark with acetonitrile ammonia. Using a pipette to take the above solution 10mL to 50mL volumetric flask, dilute ammonia solution with acetonitrile to the mark.

4.4.5.3 Determination

Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles nicosulfuron peak area becomes relatively After less than 1.2% of the solution in accordance with the sample solution, the sample solution and standard sequence of the standard solution was measured.

4.4.6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution nicosulfuron peak areas are averaged. Sample nicosulfuron Metsulfuron mass fraction w1 according to equation (1) to calculate the mass concentration according to the formula (1 ') Calculated.

w1 = A2

· M1 · w

A1 · m2

rho1 =

A2 · m1 · rho · w × 10 A1 · m2 (1') where.

w1 --- nicosulfuron mass fraction, expressed as a percentage;

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

m1 --- standard mass in grams (g);

Concentration rho1 --- nicosulfuron, in units of grams per milliliter (g/mL);

Density rho --- 20 °C when the sample in grams per milliliter (g/mL) (according to GB/T 4472 of "density meter method" determination);

w --- standard samples nicosulfuron mass fraction, expressed as a percentage;

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

m2 --- sample mass, in grams (g).

4.4.7 Allowable difference

Nicosulfuron mass fraction (concentration) of two parallel determination results relative difference should be less than 4%, and the arithmetic mean as measured Given result.

4.4.8 PH value measurement

According to GB/T 1601 carried out.

4.4.9 Determination of the suspension rate

According to GB/T 14825-2006 4.3 performed. Weigh Tobacco ethyl 0.1g sample (accurate to 0.0001g), the remaining the suspension and the precipitate was transferred to a 100mL flask with 60mL acetonitrile aqueous ammonia solution 3 times 25mL all wash residue Into the 100mL flask, under ultrasonic oscillations 5min, cooled to room temperature, volume, shaken, filtered, measured by 4.4 of nicosulfuron Quality, calculate the suspension rate.

4.4.10 Wet sieve test

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

4.4.11 Persistent foaming

4.4.11.1 Method summary

The sample was mixed with a predetermined amount of standard hard water, after standing foam volume recorded.

4.4.11.2 Reagent

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

4.4.11.3 Instruments and appliances

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

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

4.4.11.4 Determining step

Added 180mL graduated cylinder standard hard water, 1.0g sample was weighed into a graduated cylinder (accurate to 0.1g), added to standard hard water from the cylinder Plug at the bottom tick 9cm, the cover plug to the bottom of the cylinder as the center, upside down 30 times (2s). Stand on the test stand 1min, record lather volume.

4.4.12 Dispersion stability

4.4.12.1 Method summary

Dispersions are prepared according to the provisions of concentrations, were placed in two graduated emulsion tube upright standing for some time, and then invert emulsion tube several times to observe the most First, placing a certain time and re-dispersion of the dispersion liquid dispersion.

4.4.12.2 Instruments and reagents

Emulsion tube. borosilicate glass conical bottom centrifuge tube, length 15cm, scale to 100mL;

The rubber stopper. supporting and emulsion tube with 80mm long glass exhaust pipe (outer diameter of 4.5mm, an inner diameter of 2.5mm, see Figure 2);

Graduated cylinder. 250mL;

Adjustable lamp. 60W with Pearl foam;

Standard hard water. rho (Ca2 Mg2) = 342mg/L, according to GB/T 14825-2006 formulated.

4.4.12.3 Procedure

At room temperature, respectively, to two 250mL graduated cylinder was added to 240mL standard hard water scale line, each with a pipette to the graduated cylinder Solution of the sample 5g (or other predetermined number), the pipette tip as close as possible to the surface when dropped, but not in the water below. Finally, add the standard hard Water to the mark. Wear cloth gloves to the middle of the cylinder axis, upside down 30 times to ensure that the graduated cylinder liquid gently flows, the recoil does not occur, Every time reversal for an 2s (elapsed time with a stopwatch observed), with one cylinder and creams do precipitation test, another test cylinder do redispersed.

1) initial dispersion. was observed, recorded precipitation, cream or oil slick.

2) place a certain time after dispersion.

Volumetric precipitation.

Good dispersion prepared immediately after the dispersion was transferred to a 100mL emulsion tube stoppered at room temperature (23 °C ± 2 °C) upright 30min, lights illuminate the emulsion tube, adjust the light angle and position to achieve the best observation of the two-phase interface, if there is precipitation (usually reflected light More than the transmitted light precipitation was observed), record precipitation volume (accurate to ± 0.05mL).

Millimeters

2 rubber with a glass tube of the exhaust plug the top of the cream (or oil slick) volume determination.

Good dispersion prepared immediately after it was poured into the emulsion tube, pipe from top to 1mm, wear protective gloves, stuffed with rubber exhaust pipe Stopper, emulsifying exclude all air tube, remove the dispersion liquid overflow, the emulsion inverted tube, kept at room temperature for 30min, no liquid from the milk the open end of the discharge pipe would not have sealed glass tube, it has formed a record volume of cream or oil slick. Determination of the total volume of the emulsion tube, and (2) correcting the measured volume of cream or oil slick.

Cream or oil slick measuring correction factor by volume, according to the formula (2 ') Calculated.

F = 100V0

V2 '= F × V2 (2')

Where.

F --- the total volume of the emulsion tube correction factor;

V0 --- total volume of the emulsion tube;

V2 '--- precipitation measured volume and the volume of cream or oil slick;

Precipitation volume and cream or oil slick volume V2 --- measurements.

3) Re-dispersion measurement.

Good dispersion after the preparation, only the second cylinder was allowed to stand at room temperature for 24h, as described previously inverted cylinder 30, was added to the dispersion additionally Emulsion tube, standing 30min, according to the aforementioned method for determining the volume and the volume of precipitation cream or oil slick.

4.4.12.4 Measurement results

Initially dispersion completely dispersed After a certain time dispersion (30min later) precipitation <=5mL Cream or oil slick <=3mL Re-dispersible (24h later) precipitation <=1mL Cream or oil slick <=2mL the measurement results meet the above requirements is eligible.

4.4.13 Dumping Determination

4.4.13.1 Method summary

Will be placed in the container suspending sample placed after a certain time, in accordance with prescribed procedures dumping determined trapped in the sample container Volume; the vessel was washed with water, and then measuring the amount of container.

4.4.13.2 Instrument

With ground joint stopper cylinder. 500mL ± 2mL; cylinder height 39cm, between the upper and lower scale distance 25mL (or equivalent for the determination of dumping Down of other containers).

4.4.13.3 Test procedure

Mix well enough samples, some of which will be placed in a timely manner has been weighed measuring cylinder (including plug) (accurate to 0.01g), the amount of loading Tube 8 at the plugged plug grinding mouth, placing a determined time (24h). The tap is opened, the upright position of the rotating cylinder by a 135 ° dumping 60s, then pour Set 60s, re-weighing and measuring cylinder plug (accurate to 0.01g).

Would be equivalent to 80% of the cylinder volume of water (20 °C) was poured into a measuring cylinder, stoppered plug grinding mouth, the cylinder upside down 10 times, according to the above tilting operation Pour the contents of the third and weighing cylinder plug (accurate to 0.01g).

4.4.13.4 Calculation

Mass fraction and mass fraction of residue after washing the sample after pouring the residue, respectively according to formula (3) and (4) Calculated.

w3 = m2-m0m1-m0 ×

100 (3)

w4 = m3-m0m1-m0 ×

100 (4)

Where.

Mass fraction w3 --- sample after pouring the residue, expressed in%;

Mass fraction w4 --- washed residue, expressed in%;

After m2 --- dumping, quality cylinder, grinding gag and residue, in grams (g);

m0 --- cylinder, quality is more important after grinding gag constant in units of grams (g);

m1 --- cylinder, grinding gag and quality of the sample, in grams (g);

--- Washing m3, the quality of the cylinder, grinding gag and residue, in grams (g).

4.4.14 Low temperature stability test

According to GB/T 19137 in "suspended preparations" in wet sieve test still meet the standards for qualified.

4.4.15 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. After the heat storage (45 °C ± 2 °C) 42d nicosulfuron content should not be lower than the previous receptacles 95% suspension rate is still should meet the standard requirements for the qualification.

4.5 Product testing and acceptance

Product inspection and acceptance shall comply with GB/T 1604's.

5.1 Marking, labeling, packaging

Nicosulfuron oil dispersible suspension with a clean, dry glass bottle or PET bottle packaging, bottle net content of 10mL (g), 50mL (g), 500mL (g), external corrugated cartons, each net capacity 4L, 10L or 100L, 200L vat packaging. Also available upon request or Ordering protocol uses other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

Nicosulfuron oil dispersible suspension package should be stored in ventilated, dry warehouse; storage and transportation to prevent moisture and sun, not with food Material, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

This product is moderately toxic herbicide. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using this product Wear the necessary protective clothing. After spraying wash with soap and water. Coverage should be immediately sent to hospital symptomatic treatment.

5.4 Warranty Period

Under the specified storage conditions, nicosulfuron to ensure the suspension of dispersed oil, starting from the date of manufacture of two years.

Appendix A

(Informative)

Smoke Other name, structural formula and basic physicochemical parameters of ethyl the active ingredients of tobacco products other name, structural formula and basic physicochemical parameters ethyl follows.

Common name. nicosulfuron ISO common name. Nicosulfuron CAS Registry Number. 111991-09-4 Chemical Name. 2- (4,6-dimethoxy-pyrimidin-2-yl-carbamoyl-sulfamoyl) -N, N- dimethyl-nicotinamide Structure.

Empirical formula. C15H18N6O6S Molecular Weight. 410.4 Biological activity. Herbicides Melting point. 141 °C ~ 144 °C Vapour 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); 18 acetone; Ethanol 4.5; chloroform, dimethylformamide, 64; 23 acetonitrile; toluene, 0.37; n-hexane