GB 22600-20082, 4-D butyl technical (English PDF)

3.1 Appearance

Colorless to brown oily liquid.

3.2 Technical Specifications

2,4-D butyl ester original drug should also meet the requirements of Table 1.

Table 1 2,4-D butyl ester original drug control project indicators

Item Index

Butyl 2,4 mass fraction /% >= 92.0 Free phenol content (2,4-DCP meter) /% <= 1.0 Acidity (2,4 meter) /% <= 1.5 Test Method 4

4.1 Sampling

According to GB/T 1605-2001 "on the original drug product sampling" approach. Determined by sampling a random number table method packages, the final sample size not less than 100g.

4.2 Identification Test

Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of 2,4-D butyl ester. In the same chromatographic operating conditions , The retention time of the standard solution and the sample solution to a peak of 2,4-D butyl retention time, the relative difference should be 1.5% Fewer.

Infrared spectroscopy --- sample and 2,4-butyl standards in the infrared range 4000cm-1 ~ 400cm-1 absorption spectrum should Ignorance Significant differences. 2,4-D butyl standard infrared spectrum is shown in Figure 1.

1 of butyl 2,4-standard infrared spectrum

4.3 Determination of the mass fraction of 2,4-D butyl ester

4.3.1 Method summary

Sample was dissolved in chloroform, di-isobutyl phthalate as internal standard, the use of polyethylene terephthalate and tetrachlorophthalic Apiezon L to fill a stainless steel column and flame ionization detector, the sample of 2,4-butyl ester by gas chromatography separation and determination. also may Determined using capillary gas chromatography, chromatographic operating conditions, see Appendix A.

4.3.2 Reagents and solutions

Chloroform;

2,4-D butyl standard. a known mass fraction >=98.0%;

Internal standard. di-iso-butyl phthalate, should not interfere with the analysis of impurities;

Internal standard solution. Weigh isobutyl phthalate 3.5g, set 250mL flask, add appropriate amount of chloroform was dissolved and diluted to Mark and shake.

4.3.3 Instruments

Gas chromatograph. with a hydrogen flame ionization detector;

Chromatography or chromatography workstation processor;

Column. 2m × 3mm (i.d.) Stainless steel (glass) columns, built-in 1.7% tetrachlorophthalic polyethylene terephthalate and 0.3% Appius Song L/ChromosorbW-AWDMCS180 ~ 250µm filler;

Micro injector. 10µL.

4.3.4 GC operating conditions

Temperature (°C). 170 column temperature, the gasification chamber 260, the detector chamber 260;

Gas flow rate (mL/min). carrier gas (N2) 20, hydrogen gas 30, air 300;

Injection volume. 0.6µL;

Retention time (min). 2,4- 11.0 butylate, internal standard 6.7.

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 2,4-D butyl ester original drug and the internal standard gas chromatography is shown in Figure 2.

1 --- internal standard;

2 --- 2,4-D ester.

Figure 2 GC-butyl 2,4-drug and internal standard

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 2,4-butyl standard 0.1g (accurate to 0.0002g), placed in a glass bottle stuffed with a pipette 5mL internal standard solution Liquid, shake.

4.3.5.2 Preparation of sample solution

Weigh containing 2,4-D butyl ester 0.1g (accurate to 0.0002g) sample, placed in a glass vial stopper, and 4.3.5.1 with the same Pipette internal standard solution 5mL, shake.

4.3.5.3 Determination

Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two needles 2,4-butyl and the internal standard peak adjacent After the area is less than 1.2% relative change, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.

4.3.5.4 Calculation

The measured before and after the two-needle sample solution and two doses of the standard sample solution were 2,4-D butyl ester ratio and the internal standard peak area average. Sample mass fraction of 2,4-D butyl ester 1 (%), according to equation (1).

Where.

--- Standard samples of 2,4-butyl ester content, expressed as a percentage.

4.3.6 Allowable difference

Difference butyl 2,4 mass fraction of two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.

4.4 Determination of free phenols

4.4.1 Method summary

The sample was dissolved in ethanol, ammonia, 4-amino-antipyrine and potassium ferricyanide solution color, absorbance was measured at 520nm place.

Isolated from the calibration curve of standard sample absorbance at the same volume, calculated free phenol content.

4.4.2 Reagents and solutions

2,4-dichlorophenol standard. a known mass fraction >=98.0%;

Ethanol;

Isopropanol;

Ethanol, isopropyl alcohol solution. psi (ethanol. isopropanol. water) = 2.1.3;

Ammonia solution. Ba (NH3 · H2O) = 0.1mol/L;

2,4-DCP standard solution. Weigh 2,4-dichlorophenol standard 0.01g (accurate to 0.0002g), placed in 100mL volumetric flask, add A small amount of ethanol to dissolve, diluted with ethanol to the mark;

4-amino-antipyrine solution. rho = 2g/L;

Ferricyanide solution. rho = 4g/L.

4.4.3 Instruments and equipment

Spectrophotometer;

Microburette. 2mL;

Stoppered cylinder. 30mL;

Quartz cuvette. 1cm.

4.4.4 Measuring step

4.4.4.1 Correction

Followed by microburette draw 0.2mL, 0.5mL, 0.8mL, 1.0mL, 1.2mL, 1.5mL, 2.0mL2,4- dichlorophenol standard Sample solution, adding seven stoppered graduated cylinder, fill with ethanol was added to 10mL, then followed by adding 5mL of isopropanol, 5mL ammonia solution, 5mL4- ammonia Karthikeyan antipyrine 5mL aqueous potassium ferricyanide solution. Each addition are required to shake, and the last intense shaking 1min, standing 5min. Quartz cuvette, ethanol isopropyl alcohol solution as the reference absorbance at 520nm measured.

Draw 10mL ethanol, according to the procedure described above was added to each solution, determine the reagent blank absorbance.

Blank value is subtracted from the phenol solution absorbance measured absorbance, the corresponding volume of phenol solution was plotting a calibration curve.

4.4.4.2 Determination

Weigh containing 2,4-D butyl ester 0.2g (accurate to 0.0002g) sample, placed in 100mL flask, add a small amount of ethanol solution Solution, dilute to the mark with ethanol. With a pipette to the solution of 10mL stoppered measuring cylinder and then followed by adding 5mL of isopropanol, 5mL Ammonia solution, 5mL4- amino antipyrine 5mL aqueous potassium ferricyanide solution. Each addition are required to shake, and the last intense shaking 1min, standing 5min. Quartz cuvette, ethanol isopropyl alcohol solution as the reference absorbance at 520nm measured. Minus empty After the absorbance values of white, from the calibration curve of the absorbance corresponding to 2,4-DCP standard solution volume (mL) to detect.

2 free phenol content (%) according to equation (2).

Where.

Vp --- measured absorbance of the sample corresponding to the volume of phenol solution in milliliters (mL);

--- Sample mass fraction of 2,4-dichlorophenol in%.

4.5 Determination of acidity

4.5.1 Method summary

Sample was dissolved in ethanol and methyl red as indicator titration with standard sodium hydroxide solution was titrated to yellow.

4.5.2 Reagents and solutions

95% ethanol;

Sodium hydroxide standard titration solution Ba (NaOH) = 0.01mol/L, according to GB/T 601 preparation and calibration;

Methyl red ethanol solution. rho (methyl red) = 1g/L.

4.5.3 Measuring step

Weigh the sample 0.5g (accurate to 0.0002g), placed in a 250mL Erlenmeyer flask, add 95% ethanol 50mL, shake the sample Dissolved. Add 3 drops of methyl red ethanol solution of sodium hydroxide standard titration solution is titrated to a yellow endpoint. Meanwhile blank determination.

4.5.4 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 volume consumed sodium hydroxide standard titration solution, in milliliters (mL);

V0 --- titrate blank solution volume consumed sodium hydroxide standard titration solution, in milliliters (mL);

M --- 2,4- drops molar mass in grams per mole (g/mol), [M = 221g/mol].

4.6 Product testing and acceptance

Shall comply with GB/T 1604's. Limit the use of numerical treatment rounding value comparison method.