GB 28156-2011Fluoroglycofen-ethyl emulsifiable concentrates (English PDF)

3.1 Composition and appearance

This product should be compliant Fluoroglycofen ether emulsifier dissolved drug and formulated in a suitable solvent, it should be stable homogeneous liquid Body, no visible suspended matter and sediment.

3.2 Technical Specifications

B fluoroglycofen EC shall comply with the requirements of Table 1.

Table 1 B fluoroglycofen EC quality control program indicators

Item Index

Fluoroglycofen ether mass fraction /% 10.0 20.0 1.2-1.2 1.0 to 1.0 Moisture content /% <= 0.5 pH range 4.0 to 6.0 Emulsion stability (diluted 200 times) Qualified

Table 1 (continued)

Item Index

Low temperature stability a qualified Thermal storage stability of a qualified when a normal production, low-temperature storage stability and thermal stability test, measured at least once every six 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. Determining sample package using a random number table method; the final sample size not less than 250mL.

4.3 Identification Test

Liquid chromatography --- The identification test can be carried out simultaneously with the determination of ethyl fluoroglycofen mass fraction. In the same chromatographic operating conditions , The retention time of the standard solution and the sample solution to a chromatographic peaks in the B fluoroglycofen chromatographic retention time, the relative difference should 1.5% or less.

Gas Chromatography --- The identification test can be carried out simultaneously with the determination of ethyl fluoroglycofen mass fraction. In the same chromatographic operating conditions , The retention time of the standard solution and the sample solution to a chromatographic peaks in the B fluoroglycofen chromatographic retention time, the relative difference should 1.5% or less.

4.4 Determination of B fluoroglycofen mass fraction

4.4.1 Capillary gas chromatography (Arbitration Act)

4.4.1.1 Method summary

Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using a HP-5 fused silica capillary column coated walls, and hydrogen fire Flame ionization detector, a sample with acetic fluoroglycofen capillary gas chromatography and determination.

4.4.1.2 Reagents and solutions

Chloroform;

B fluoroglycofen standard. a known mass fraction w>=99.0%;

Dicyclohexyl phthalate ester. not interfere with the analysis of impurities;

Internal standard solution. Weigh 7.5g dicyclohexyl phthalate esters into 1000mL volumetric flask, dissolved with chloroform, constant volume, Shake well.

4.4.1.3 Instruments

Gas chromatograph. with flame ionization detector;

Column. 30m × 0.32mm (id) quartz capillary column, wall coated HP-5, film thickness 0.25µm;

Chromatographic data processor or chromatography workstation.

4.4.1.4 GC operating conditions

Temperature (°C). Room 230 column, the gasification chamber 260, detection chamber 280;

Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 30, air 300, the compensation gas 25;

Split ratio. 30.1;

Injection volume. 1.0µL;

Retention time. Fluoroglycofen ether about 10.8min, internal standard about 7.9min.

GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results. Typical B fluoroglycofen EC and the internal standard gas chromatography is shown in Figure 1.

1 --- internal standard;

2 --- Fluoroglycofen ether.

Figure 1 B fluoroglycofen EC and the internal standard gas chromatograph

4.4.1.5 Measurement procedure

4.4.1.5.1 Preparation of standard solution

Weigh Fluoroglycofen ether standard 0.05g (accurate to 0.0002g), placed in a glass bottle stopper, with a pipette accurately added 5mL within Standard solution, shake.

4.4.1.5.2 Preparation of the sample solution

Weigh containing ethyl fluoroglycofen 0.05g of the sample (accurate to 0.0002g), placed in a glass bottle stopper, and with the 4.4.1.5.1 with the use of a pipette accurately added internal standard solution 5mL, shake.

4.4.1.5.3 Determination

Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles Fluoroglycofen ether and the internal standard After the relative change in the peak area ratio was less than 1.2%, according to the solution, sample solution, sample solution, standard sequence of standard solution for analysis Determination.

4.4.1.5.4 Calculation

The measured before and after the two-needle sample solution and two doses of the standard sample solution Fluoroglycofen ether and the internal standard peak area ratios are flat all. Sample B fluoroglycofen content according to equation (1).

w1 = r2 × m1 × wr1 × m2 (1) where.

w1 --- sample Fluoroglycofen ether mass fraction, expressed as a percentage;

r2 --- sample solution Fluoroglycofen ether and the average internal standard peak area ratio;

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

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

r1 --- standard samples Fluoroglycofen ether and the average peak area ratio of the internal standard solution;

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

4.4.1.6 Allowable difference

The difference between two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.

4.4.2 High Performance Liquid Chromatography

4.4.2.1 Method summary

Sample was dissolved in acetonitrile, methanol and acetic acid water as the mobile phase, use as filler in Nova-PakC18 stainless steel column and ultraviolet detection Detector (230nm), the sample of Fluoroglycofen ether HPLC separation and determination.

4.4.2.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. chromatographic pure;

Glacial acetic acid;

Water. The new secondary steam distilled water;

Fluoroglycofen ether Sample. Known Fluoroglycofen ether content w>=99.0%.

4.4.2.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or workstation;

Color 150mm × 3.9mm (id) stainless steel column, built-Nova-PakC18,5µm filler (or the equivalent effect. Column the column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.4.2.4 HPLC operating conditions

Mobile phase. Psi (CH3OH.H2O.CH3COOH) = 75.25.0.2;

Flow rate. 1.0mL/min;

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

Detection wavelength. 230nm;

Injection volume. 5µL;

Retention time. B fluoroglycofen about 7.0min.

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 B fluoroglycofen EC HPLC is shown in Figure 2.

1 --- Fluoroglycofen ether.

Figure 2 B fluoroglycofen EC HPLC diagram

4.4.2.5 Measurement procedure

4.4.2.5.1 Preparation of standard solution

Weigh 0.1g Fluoroglycofen ether standard (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with acetonitrile, ultrasonic Oscillation 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask with acetonitrile Dilute to the mark.

4.4.2.5.2 Preparation of sample solution

Weigh containing ethyl fluoroglycofen sample of 0.1g (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with acetonitrile, super Acoustic oscillations 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask Acetonitrile and diluted to the mark, shake.

4.4.2.5.3 Determination

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

4.4.2.5.4 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution Fluoroglycofen ether peak areas are averaged. Sample B Fluoroglycofen mass fraction w2 according to equation (2).

w2 = A2

· M1 · w

A1 · m2

Where.

Quality w2 --- sample Fluoroglycofen ether fraction, in%;

A2 --- sample solution B carboxymethyl fluoride grass ether the average peak area;

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

w --- B fluoroglycofen standard mass fraction, expressed as a percentage;

A1 --- Sample mean fluoride grass ether peak areas of ethyl in solution;

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

4.4.2.6 Allowable difference

Difference fluoride grass ether twice the mass fraction of the results of parallel determination Methyl and should not exceed 0.5%, and the arithmetic mean as a measurement result.

4.5 Determination of moisture content

According to GB/T 1600 the "Karl Fischer method".

Determination of 4.6 pH value According to GB/T 1601 carried out.

4.7 Emulsion stability test

Standard hard water sample was diluted 200-fold, according to GB/T 1603 test. No oil slick measuring cylinder (cream), and precipitation of heavy oil qualified.

4.8 Low temperature stability test

According to GB/T 19137 in "homogeneous emulsion and liquid preparations", in the bottom of the centrifuge tube educt volume does not exceed 0.3mL qualified.

4.9 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. After the thermal storage, Fluoroglycofen ether content should not be lower than the measured Fluoroglycofen before hot storage 97% by mass of ether; emulsion stability compliance.

4.10 Product inspection and acceptance

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

5.1 Marking, labeling, packaging

B fluoroglycofen EC marking, labeling and packaging should comply with the provisions of GB 4838.

B fluoroglycofen EC 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 Association Propose the use of other forms of packaging, subject to the provisions of GB 4838.

5.2 Storage

B fluoroglycofen EC packages should be stored in well-ventilated, dry coffers. Storage and transportation, to prevent moisture and sunlight, no food, seed Child, feed-mixing, avoid contact with skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

The goods on the skin moderate irritation of the eyes has a strong stimulating effect. When using this product to wear rubber gloves and goggles, wear the necessary Protective clothing. After application, immediately wash with soap and water. Such as skin, eyes accidentally stained with the product, rinse immediately with plenty of water. error Clothing should be immediately sent to hospital symptomatic treatment.

5.4 Warranty Period

Under the provisions of storage and transportation conditions, Fluoroglycofen ether guarantee EC, from the date of manufacture of two years.

Appendix A

(Informative)

Other name, structural formula and basic physicochemical parameters Fluoroglycofen ether Other name, structural formula and basic physicochemical parameters Fluoroglycofen ether as follows.

Generic Name. B fluoroglycofen ISO common name. Fluoroglycofen-ethyl CAS Registry Number. 77501-90-7 Chemical Name. O- [5- (2-chloro -alpha, alpha, trifluoro - on - tolyloxy) -2-nitrobenzoyl] hydroxy ethyl Structure.

Empirical formula. C18H13ClF3NO7 Molecular Weight. 447.8 Biological Activity. herbicides;

Melting point. 65 °C;

Vapor Pressure. Less than 133Pa (25 °C) Solubility (25 °C). water 0.6mg/L; most organic solvents greater than 100g/kg Stability. 0.25mg/L aqueous solution at 22 °C about the DT50 231d (pH5), 15d (pH7), 0.15d (pH9); a water suspension it was due to the rapid decomposition of ultraviolet light; and soil degradation due to rapid microbial, DT50 about 11h.

1102-

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