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Chemical Industry Standard of the People's Republic of China
HG2207—91
Published on November 18, 1991
Metalaxyl Powder
Implemented on July 1, 1992
Ministry of Chemical Industry of the People's Republic of China
W Chemical Industry Standard of the People's Republic of China
Metalaxyl
Metalaxyl Powder
Subject Content and Scope of Application
HG 2207—91
This standard specifies the technical requirements, inspection methods, inspection rules, and marking, packaging, transportation and storage requirements for metalaxyl powder. This standard applies to metalaxyl powder made from metalaxyl technical by filler adsorption and dilution. Active ingredient: Metalaxyl
Chemical name: N-(2,6-xylyl)-N-(2-methoxyacetyl)-DL-aminopropionic acid methyl ester Structural formula:
Molecular formula: C15H21NO4
CH20CH3
Relative molecular mass: 279.34 (International relative atomic mass in 1987) Reference standards
GB190 Dangerous goods packaging mark
GB1600 Pesticide moisture determination method
Pesticide hydrogen ion concentration determination method
GB1601
GB1605 Commercial pesticide sampling method
HG2-896 Pesticide powder fineness determination method 3 Technical requirements
3.1 Appearance: Light grayish yellow or rose red loose powder. 3.2 Metalaxyl powder shall meet the following technical requirements: Item
Metalaxyl content, %(m/m)
Water content, %(m/m)
Fineness (through 43um sieve), %(m/m)mesh
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991>
Implemented on July 1, 1992
W.4 Test method
4.1 Determination of metalaxyl content
4.1.1 Summary of method
HG2207-91
The sample is extracted with acetone and dibutyl phthalate is used as the internal standard. The metalaxyl powder is separated and determined on a 5% cyclohexanedimethanol succinate polyester column using a hydrogen flame ionization detector. 4.1.2 Reagents and solutions
Metalaxyl standard: known content ≥99.0%, stationary phase: cyclohexanedimethanol succinate polyester (imported); internal standard: dibutyl phthalate;
Carrier: Chromosorb W/AW-DMCS, particle size 180~250um or 102 white silanized carrier, particle size 180~250ums
Acetone (GB686)
Chloroform (GB682).
4.1.3 Instruments
Gas chromatograph: hydrogen flame ionization detector; chromatographic column: 1000mm long, 3mm inner diameter glass column (or stainless steel column), filled with 5% cyclohexanedimethanol succinate polyester/Chro-mosorbW/AW-DMCS, particle size 180~250um (or the above 102 white silanized support, particle size 180~250um) filler; micro syringe: luL;
Centrifuge: with 10mL centrifuge tube.
4.1.4 Operation stepsbZxz.net
4.1.4.1 Preparation of chromatographic column
a. Coating of stationary liquid: Accurately weigh 0.2g of cyclohexanedimethanol succinic acid polyester, dissolve it in 16mL of chloroform, then add 4g of Chromosorb W/AW-DMCS, shake gently to make the carrier completely immersed in chloroform, and after drying, put it in a 100C oven for 1h.
Filling of chromatographic column: Connect a glass funnel to the inlet end of the clean and dried chromatographic column, wrap the outlet end with gauze, and connect it to the vacuum pump through a rubber tube. Turn on the vacuum pump, slowly add the prepared filler from the funnel end, and keep gently vibrating the chromatographic column. After the filler is tightly and evenly filled, remove the chromatographic column and plug a small ball of glass wool at the outlet and inlet ends of the column respectively. c. Aging of the chromatographic column: Connect the inlet end of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the outlet end to the detector for the time being. Pass the carrier gas at a flow rate of about 20mL/min, and maintain it at a column temperature of 240℃ for 24h. After cooling down, connect the column outlet end to the detector. 4.1.4.2 Gas chromatographic operating conditions
Temperature:
Column chamber 205℃,
Vaporization chamber 250℃;
Detection chamber 250℃.
Air flow rate:
Carrier gas (N2) 40mL/min
Hydrogen 50mL/min;
Air 500mL/min.
Recording paper speed:
4mm/min.
Injection volume:
W.bzsoso.cOIRetention time:
Metalaxyl about 7min;
Internal standard about 5min;
Impurity No. 1 about 3min;
Impurity No. 2 about 4min;
Impurity No. 3 about 10min.
HG2207—91
The above operating conditions are the operating parameters on the GC-9A gas chromatograph. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect.
4.1.4.3 Preparation of standard solution and sample solution Standard solution: Weigh 0.12g of metalaxyl, accurate to 0.0001g, and 0.10g of dibutyl phthalate, accurate to 0.0001g, and place them in a clean, dry glass bottle with a stopper, dissolve with 3mL of acetone, shake well, and set aside. Sample solution: weigh a sample of metalaxyl powder containing 0.12g of metalaxyl, accurate to 0.0001g, and 0.10g of dibutyl phthalate, accurate to 0.0001g, and place them in a 20mL stoppered conical bottle. Add 5mL of acetone and shake vigorously for 5min. Then, pour the solution into a 10mL centrifuge tube and centrifuge for 5min (3500r·pm). Take part of the clear liquid and place it in a clean and dry glass stoppered bottle for testing. 4.1.4.4 Determination
Under the above gas chromatography conditions, after the instrument is stable, inject several needles of standard solution until the peak area ratio of two adjacent needles is basically stable (the change is not more than 1.2%), and then analyze in the following order: standard solution;
b. sample solution;
c. sample solution,
d. standard solution.
4.1.4.5 Calculation
Calculate the correction factor f of metalaxyl from the average peak area of metalaxyl and internal standard substance in the chromatograms of the two standard solutions a and d: f
Wherein: mi, m. - are the masses of metalaxyl and internal standard substance in the standard solution, g; Ai, A. - are the average peak areas of metalaxyl and internal standard substance in the chromatograms of the two standard solutions, mm, o
The percentage of metalaxyl standard substance.
Calculate the percentage of metalaxyl from the average peak area of metalaxyl and internal standard substance in the chromatograms of the two sample solutions b and c: -×100
Wherein: - is the correction factor of metalaxyl, mi.ms
are the masses of metalaxyl and internal standard substance in the sample solution, mm, A, A. - is the average of the peak areas of metalaxyl and internal standard on the chromatograms of the two sample solutions, mm2. 4.1.4.6 Allowable difference
The difference between the results of two parallel determinations of this method shall not be greater than 0.6%. 4.2 Determination of water content
Determine according to the "azeotropic distillation method" in GB1600. 4.3 Determination of pH value
Wbzsoso.cOn Determine according to the "pH meter method" in GB1601. 4.4 Determination of fineness
Determine according to the method in HG2-896.
HG2207—91
Figure 1 Gas chromatogram of metalaxyl powder
1—Solvent; 2—Impurity No. 1, 3—Impurity No. 2, 4—Internal standard; 5—Metalaxyl, 6—Impurity No. 3 5 Inspection rules
5.1 Metalaxyl powder should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all metalaxyl powder shipped out of the factory meets the requirements of this standard. Each batch of metalaxyl powder should be accompanied by a quality certificate in a certain format when it leaves the factory. 5.2 The user has the right to verify whether the quality of the metalaxyl powder received meets the requirements of this standard in accordance with the provisions of the standard. 5.3 The sampling method should be carried out in accordance with GB1605. After mixing 200g of the sample evenly, put it into two clean, dry glass bottles with ground stoppers. Labels should be attached to the bottles, indicating the manufacturer's name, product name, batch number, and sampling date. One bottle is used for testing, and the other is sent to the quality supervision and inspection department for storage for arbitration.
5.4. If any of the indicators do not meet the requirements of this standard, re-testing shall be conducted by sampling from twice the amount of packages. If only one indicator does not meet the requirements of this standard, the whole batch of metalaxyl powder cannot be accepted. 5.5. If there is a dispute between the supplier and the buyer over the quality of the product, the two parties may negotiate to resolve it; or select an arbitration institution to conduct arbitration inspection according to the method specified in this standard.
6. Marking, packaging, transportation and purchase and storage
HG2207-91
6.1 Metalaxyl powder is packaged in a hard fiberboard drum with a diameter of 40cm and a height of 54cm. The inner packaging is a thick plastic bag (0.1mm polyethylene bag), each bag contains 20kg, or a double-layer plastic bag (outer layer 0.06mm, inner layer 0.04mm polyethylene bag), each bag contains 100g or 250g. The net weight of each drum is 20kg.
6.2 The packaging barrels and packaging bags should be firmly marked. The content includes: manufacturer name, product name, batch number, production date, net weight, product standard number, production permit (or production license) number and the "toxic substance" mark specified in GB190 and the quality certificate that the product meets the requirements of this standard.
6.3 During storage and transportation, it must be strictly protected from rain and sun, and maintained in good ventilation. It must not be mixed with food, seeds and feed, etc., and avoid contact with the skin to prevent inhalation through the mouth and nose.
6.4 The warranty period of this product is two years.
Additional instructions:
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 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 Liang Qinying, Wu Tiejun, Yang Rongzhu and Mao Ronghua.5
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