GB 24753-2009Isocarbophos technical (English PDF)

4.2 Identification Test Infrared spectroscopy

--- Isocarbophos sample and standard samples in the range 4000cm-1 ~ 400cm-1 infrared absorption spectrum should not significantly the difference. Isocarbophos standard infrared spectrum is shown in Figure 1. Figure

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, >=97.5%.

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. psi (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. Typical Isocarbophos original drug HPLC is shown in Figure 2. 1

--- Isocarbophos. Figure 2 HPLC Isocarbophos original drug

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 aqueous Isocarbophos 0.1g sample (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic Wave 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 A Alcohol diluted to the mark, shake.

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 1.2%, 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, >=97.5%; Internal standard solution. Weigh 5g of 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; Chromatographic data processor or chromatography workstation; Column. 1m × 3mm (. I.d) glass column (or stainless steel column), built-in 5% OV-3/101 silylation white support body (180µm ~ 250

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 gas chromatogram Isocarbophos original drug and the internal standard are shown in Figure 3. 1

--- Isocarbophos; 2

--- internal standard. Figure

4.6 Determination of acidity

4.6.1 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.

4.6.2 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, 0.02mol/L sodium hydroxide standard titration solution, titration to blue is the end. Meanwhile blank Determination.

4.6.3 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].

4.7 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 Flag

5.1 Isocarbophos original drug, labeling and packaging should comply with the provisions of GB 3796.

5.2 Isocarbophos original drug use clean, dry sturdy plastic (iron) pail, barrel net content should not exceed 200kg. It can also be used in accordance with User requirements or other forms of ordering agreement package, subject to the provisions of GB 3796.

5.3 Isocarbophos original drug package 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 highly toxic organophosphate pesticides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and the FDA Rubber gloves, wear the necessary protective clothing. After spraying, wash immediately with soap and plenty of water. Such as poisoning, should be immediately sent to hospital Symptomatic treatment. Atropine or pralidoxime detoxification.

5.6 of acceptance. Acceptance of Isocarbophos original drug for a month. From the date of delivery, product quality inspection completed within a month of its Indicators shall comply with this standard.