GB 23550-200935% Isocarbophos emulsifiable concentrates (English PDF)

4.2 Identification Test Liquid chromatography

--- The identification test can be carried out simultaneously with the determination of the mass fraction of Isocarbophos. Under the same chromatographic operating conditions, The sample solution to a chromatographic retention time and standard solution in the retention time of the main peaks, the relative difference should be less than 1.5%.

4.3.1 High performance liquid chromatography (Arbitration Act)

4.3.1.1 Method summary Sample was dissolved in methanol, methanol + water as the mobile phase, to use as filler BDSHypersilC18 stainless steel column and UV detector (225nm), the sample Isocarbophos high performance liquid chromatography and determination.

4.3.1.2 Reagents and solutions Methanol; Water. The new secondary steam distilled water; Isocarbophos standards. a known mass fraction >=99.0%.

4.3.1.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or workstation; Color 150mm × 4.6mm (i.d.) Stainless steel column, built BDSHypersilC185µm filler (or the equivalent effect. Column The column); Filter. filter pore size of about 0.45µm; Micro injector. 50µL; Quantitative sample line. 5µL; Ultrasonic cleaner.

4.3.1.4 HPLC operating conditions Mobile phase. phi (CH3OH.H2O) = 60.40; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 °C); Detection wavelength. 225nm; Injection volume. 5µL; Retention time. Isocarbophos about 5.6min. 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. A typical 35% Isocarbophos EC HPLC is shown in Figure 1. 1

--- Isocarbophos. 1 35% Isocarbophos EC HPLC diagram

4.3.1.5 Measurement procedure 4.3.1.5.1 Preparation of standard solution Weigh 0.1g Isocarbophos standard (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic transducer Dang 5min to dissolve the sample was cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with methanol Release to the mark. 4.3.1.5.2 Preparation of sample solution Weigh 0.3g (accurate to 0.0002g) Isocarbophos sample, placed in 50mL volumetric flask, dilute to the mark with methanol, ultrasonic transducer Dang 5min to dissolve the sample was cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with methanol Release to the mark.

4.3.1.6 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles Isocarbophos 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.

4.3.1.7 Calculation 1 sample mass fraction (%) Isocarbophos, according to equation (1). 1 = A2 (1) Where. A1

--- the standard solution, the average Isocarbophos peak area; A2

--- sample solution, the average Isocarbophos peak area;

--- Isocarbophos standard mass fraction, expressed as a percentage.

4.3.1.8 allowable difference Isocarbophos poor quality score of two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.

4.3.2 Gas Chromatography

4.3.2.1 Method summary Sample was dissolved in ethyl acetate, n-butyl sebacate to as the internal standard, using the 5% OV-3 packed column, and a hydrogen flame ionization detector , A sample of Isocarbophos gas chromatographic separation and determination.

4.3.2.2 Reagents and solutions Ethyl acetate; N-butyl sebacate. Do not interfere with the analysis of impurities; Isocarbophos standards. a known mass fraction >=99.0%; Internal standard solution. Weigh 5g-n-butyl sebacate in 250mL volumetric flask, dissolved in ethyl acetate and diluted to the mark, shake; Fixative. OV-3; Carrier. 101 silanized carrier body (180µm ~ 250µm).

4.3.2.3 Instruments Gas chromatograph. with flame ionization detector; Column. 1m × 3mm (. I.d) glass column (or stainless steel column), built-in 5% OV-3/101 silylation white support body (180µm ~ 250

m) filler. Chromatographic data processor or chromatography workstation.

4.3.2.4 GC operating conditions Temperature (°C). Room 210 column, the gasification chamber 270, detection chamber 270; Gas flow rate (mL/min). carrier gas (N2) 60, hydrogen gas 40, air 400; Injection volume. 0.6µL; Retention time. Isocarbophos about 6.1min, internal standard about 9.5min. 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. A typical 35% Isocarbophos EC and the internal standard gas chromatography is shown in Figure 2. 1

--- Isocarbophos; 2

--- internal standard. 2 35% Isocarbophos EC and the internal standard gas chromatograph

4.3.2.5 Measurement procedure 4.3.2.5.1 preparation of standard solution He said water Isocarbophos standard 0.2g (accurate to 0.0002g), placed in a glass bottle stopper, with a pipette accurately added 5mL internal standard Solution, shake. 4.3.2.5.2 preparation of the sample solution Weigh 0.6g (accurate to 0.0002g) Isocarbophos sample placed in a glass bottle stopper, with the same use and 4.3.2.5.1 A pipette accurately added internal standard solution 5mL, shake.

4.3.2.6 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 Isocarbophos internal standard After the peak area ratio of relative change is less than 1.2%, according to the solution, the sample solution, the sample solution, the order of standard sample of standard solution was analyzed Determination.

4.3.2.7 Calculation The peak area was measured before and after the two-needle sample solution and two doses of the standard sample solution Isocarbophos and the internal standard ratio were flat all. Sample Isocarbophos 2 mass fraction (%) according to equation (2). (2) Where. gamma1

--- standard solution Isocarbophos the mean internal standard peak area ratio; gamma2

--- the average of the sample solution Isocarbophos and the internal standard peak area ratio;

--- Standard ISO CARBOPHOS mass fraction, expressed as a percentage.

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

4.5 Determination of acidity

4.5.1 Reagents and solutions Ethanol; Sodium hydroxide standard titration solution Ba (NaOH) = 0.02mol/L, according to GB/T 601 preparation and calibration; Bromophenol blue in ethanol. rho (bromophenol blue) = 1g/L.

4.5.2 measuring step Weigh the sample 2g (accurate to 0.002g), placed in a 250mL Erlenmeyer flask, adding ethanol 20mL, shake the sample solution solution. Add 3 drops of bromophenol blue indicator, titrated with sodium hydroxide standard solution titration to blue is the end. Meanwhile blank determination.

4.5.3 Calculation The acidity of the sample 3 (%), according to equation (3) Calculated. 3 = Ba (Vp Vp 1- 0) × M 100 (3) Where. Ba

--- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L); Vp 1

--- titration of the sample solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL); V0

--- titrate blank solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL);

--- The M sulfuric numerical molar mass in grams per mole (g/mol), [M (12H2SO4 ) = 49g/mol].

4.6 Emulsion stability test Standard hard water sample was diluted 200-fold, according to GB/T 1603 testing and judgment.

4.7 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.

4.8 Thermal storage stability test According to GB/T 19136 in "liquid formulation" to. After the thermal storage, Isocarbophos mass fraction of not less than the measured thermal storage mass fraction ago 90%; emulsion stability should continue to meet the standards.

4.9 product testing and acceptance Product inspection and acceptance shall comply with GB/T 1604's. Treatment of extreme values using the rounding value comparison method. 5 marking, labeling, packaging, storage and transportation 5.1 35% Isocarbophos EC marking, labeling and packaging should comply with the provisions of GB 4838. 5.2 35% Isocarbophos EC with a clean, dry glass bottle or PET bottle packaging, bottle net weight 280g (mL), 320g (mL) Etc., external corrugated cartons, each net content of not more than 20kg. Also available upon request or order agreement, other forms of packages Equipment, subject to the provisions of GB 4838. 5.3 35% Isocarbophos EC packages should be stored in well-ventilated, dry coffers.

5.4 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.

5.5 Security. This product is organic phosphorus pesticides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber to the FDA Gloves wear the necessary protective clothing. After spraying, wash immediately with soap and plenty of water. Such as poisoning, symptomatic treatment should be immediately sent to hospital Therapy. Atropine or pralidoxime detoxification.

5.6 Warranty. Under the provisions of storage and transportation conditions, 35% Isocarbophos EC warranty period, counting from the date of manufacture 2 years. In Bulgaria Isocarbophos content license period should not be less than 32.0%.