Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2203-91
2-Methyl-4-chloro-sodium aqueous solution
Published on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implementation on July 1, 1992
W Chemical Industry Standard of the People's Republic of China
2-Methyl-4-chloro-sodium aqueous solution
Subject content and scope of application
HG2203-91
This standard specifies the technical conditions, test methods, inspection rules and marking, packaging, transportation and storage requirements of 2-Methyl-4-chloro-sodium aqueous solution. This standard applies to 2-Methyl-4-chloro-sodium aqueous solution prepared by condensation with o-cresol and monochloroacetic acid as the main raw materials. Active ingredient: 2-methyl-4-chlorosodium
Chemical name: 2-methyl-4-chlorophenoxyacetic acid sodium Structural formula:
Molecular formula: CH:O:CINabZxz.net
CH2COONa
Relative molecular mass: 222.60 (1987 international relative atomic mass) Reference standards
GB1601
GB1604
Method for determination of hydrogen ion concentration of pesticides
Pesticide acceptance rules
GB3796
General rules for pesticide packaging
HG2-14602 2-methyl-4-chlorosodium
3 Technical requirements
3.1 Appearance: Brown or purple-red liquid, without obvious suspended matter and precipitation. 3.22 Sodium 4-chloro-4-methylphenol aqueous solution shall also meet the following index requirements: Item
2 Sodium 4-chloro-4-methylphenol content, % (m/m)
Free phenol (calculated as 4-chloro-2-methylphenol), % (m/m) pH range
Dilution stability
Water insoluble matter\, % (m/m)
Note: 1) is a type inspection item.
4 Test method
4.12 Determination of sodium 4-chloro-4-methylphenol content
Carry out according to 3.1 of HG2-1460, except that the analysis steps are changed to the form of "standard sample, test sample, test sample, standard sample". Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991
Implementation on July 1, 1992
W.4.1.1 Analysis steps
4.1.1.1 Preparation of standard solution
HG2203-91
Weigh 0.13g of 2-methyl-4-chloro-1-yl standard sample to an accuracy of 0.0001g, place it in a 25mL volumetric flask, weigh 0.09g of dimethyl phthalate to an accuracy of 0.0001g, add 20mL of ether and mix. Take 2mL of this solution, place it in a stoppered glass bottle with a capacity of about 15mL, add excess (about 6-8mL) of saturated diazomethane ether solution for esterification, and concentrate to about 0.5mL. 4.1.1.2 Preparation of sample solution
Weigh 1.0g of sample to the nearest 0.0001g, acidify and extract according to 3.1.5 of HG2-1460, and weigh about 0.09g of dimethyl phthalate into the combined ether extract. After shaking, take 4mL of the test solution and place it in a stoppered glass bottle with a capacity of about 15mL. Add 6-8mL of saturated diazomethane ether solution while shaking to completely esterify the sample. Concentrate the test solution to about 0.5mL. 4.1.1.3 Determination
After the instrument is stable, inject several injections of standard sample solution until the peak height ratio of 2-methyl-4-chloro-1-yl chloride to the internal standard is basically stable, and then perform sample analysis in the order of a. Standard sample, b. Sample, c. Sample, d. Standard sample, and the injection volume is about 0.5uL. 4.1.2 Calculation
Average the obtained peak height ratios of a, d and bc, and obtain the mass percentage content of sodium 2-methyl-4-chlorophenoxyacetic acid X1. Calculate m2.P
rim2·m.·P
according to formula (1) where: T1 is the average value of the peak height ratios of 2-methyl-4-chlorophenoxyacetic acid and dimethyl phthalate on the two-shot sample chromatogram; T2 is the average value of the peak height ratios of 2-methyl-4-chlorophenoxyacetic acid and dimethyl phthalate on the two-shot standard sample chromatogram; m1 is the mass of the sample, 8;
m2 is the mass of the standard sample, g
is the mass of the internal standard in the sample solution, g; the mass of the internal standard in the standard sample solution, m
is the ratio of the relative molecular mass of sodium 2-methyl-4-chlorophenoxyacetic acid to 2-methyl-4-chlorophenoxyacetic acid. 1. 11—
4.1.3 Allowable difference
The difference between two parallel determination results should not be greater than 0.5%. 4.2 Determination of free phenol content
4.2.1 Summary of method
Dissolve the sample in alcohol ammonia solution, add 4-aminoantipyrine and potassium ferrocyanide solution for color development, and determine its absorbance. 4.2.2 Reagents and solutions
4-Chloro-2-methylphenol standard, known content, ethanol (GB678);
Acetone (GB686)
Ammonia solution: 0.05mol/L,
Solution A: Dissolve 100g 4-chloro-2-methylphenol in 10mL acetone, dilute to 1L with water, and mix well. (1)
Solution B: Dissolve 0.5g 2-methyl-4-chloroform (without phenol) in 50mL ethanol, add 90mL 0.05mol/L ammonia solution, dilute to 1L with water, and mix well.
4-Aminoantipyrine: 2g/L aqueous solution, prepare with 20g/L stock solution when using (can be stored in a dark place for 3 months). Potassium ferrocyanide (GB644): 4g/L aqueous solution (prepare when using). 4.2.3 Apparatus
Wbzsoso.cOn spectrophotometer,
microburette, 2mL,
stoppered graduated cylinder, 25mL, 7 pcs.
4.2.4 Analysis steps
4.2.4.1 Calibration
HG2203—91
Use a microburette to draw 0.2, 0.4, 0.5, 0.6, 0.8, 1.0 and 1.2 mL of solution A in turn, and put them into 7 stoppered measuring cylinders. Use solution B to make it up to 10 mL, and then add 5 mL of ammonia solution, 5 mL of 4-aminoantipyrine solution and 5 mL of potassium ferrocyanide solution in turn. Shake each time the solution is added, and shake vigorously for 1 min for the last time. Let it stand for 5 min. Measure the absorbance of the solution at a wavelength of 510 nm, using a 1 cm colorimetric cell and distilled water as a reference. Draw 10 mL of solution B, add ammonia solution, 4-aminoantipyrine solution and potassium ferrocyanide solution according to the above steps, and measure the absorbance of the reagent blank.
Subtract the blank value from the absorbance measured by the phenol solution, and plot the volume (mL) of solution A against the absorbance to obtain a calibration curve. 4.2.4.2 Determination
Accurately weigh 0.5g of the sample to the nearest 0.0001g, place it in a 1000mL volumetric flask, add 50mL of ethanol and 90mL of ammonia solution, and dilute to the mark with water. Take 10mL of this solution, put it in a stoppered measuring cylinder, and add 5mL of ammonia solution, 5mL of 4-aminoantipyrine solution, and 5mL of potassium ferricyanide solution in sequence. Each solution should be shaken immediately after it is added. Continue shaking for 1min, let it stand for another 5min, and measure its absorbance. According to the method in 4.2.4.1, measure the blank and subtract the blank value from the absorbance of the sample. Find the volume (mL) of solution A corresponding to the absorbance from the calibration curve. The mass percentage of free phenol is X2 and calculated according to formula (2):
Where: V——volume of solution A, mL, m-
-sample volume,.
4.3 Determination of pH value
Measure according to the pH meter method in GB1600. 4.4 Dilution stability test
4.4.1 Reagents and instruments
Standard hard water: 342ppm,
Measuring cylinder: 100mL,
Constant temperature water bath: 30±1℃.
4.4.2 Test steps
(2)
Pipette 5mL of sample and place it in a 100mL measuring cylinder. Dilute to the mark with standard hard water and mix. Place the dilution in a 30±1℃ water bath and let it stand for 1h. If the dilution is uniform and there is no precipitate, it is qualified. 4.5 Determination of water-insoluble content
Determine according to 3.4 of HG2-1460, and change the sample weight to 10g. 5 Inspection rules
5.1 Pesticide acceptance rules shall be implemented in accordance with GB1604. 5.2 Water-insoluble matter is a type inspection item, and the inspection cycle is 1 month. 5.3 Sampling method: Take samples from 5% of each batch. For small batches, no less than 3 boxes (barrels). Mix the samples evenly, take out about 500mL, and divide them into two clean, dry glass bottles with ground stoppers. Paste labels on the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is sent to the technical supervision and inspection department for inspection, and one bottle is retained. 3
Wbzsoso,cO6 Marking, packaging, transportation and storage
HG2203-91
6.12 The marking and packaging of sodium 4-chloroformate aqueous solution shall comply with the relevant provisions of GB3796. 6.22 Sodium 4-chloro-4-methyl-aqueous solution should be packaged in clean, dry brown glass bottles or plastic bottles. The net weight of each bottle is 0.5kg or 1.0kg. It should be covered with straw covers or foam air cushions and tightly arranged in wooden boxes, cartons or calcium plastic boxes. The net weight of each box should not exceed 20kg. 6.32 Sodium 4-chloro-4-methyl-aqueous solution should be protected from moisture and sunlight during storage and transportation. It should be kept well ventilated and should not be mixed with food, seeds, or feed. It should avoid contact with the skin and prevent inhalation through the mouth and nose.
Additional Notes:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Hou Yukai, Wu Yanfeng, Bai Zonghan, Hu Youwu, Yu Lihua, and Bai Huanzhang. 4
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