Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2208—91
Metalaxyl Wettable Powder
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
Metalaxyl Wettable Powder
1 Subject Content and Scope of Application
HG2208—91
This standard specifies the technical requirements, inspection methods, inspection rules, and marking, packaging, transportation and storage requirements for metalaxyl wettable powder.
This standard applies to wettable powders made from metalaxyl technical by filler adsorption, dilution and additive processing. Active ingredient: Metalaxyl
Chemical name: N-(2,6-xylyl)-N-(2-methoxyacetyl)-DL-aminopropionic acid methyl ester Structural formula:bzxZ.net
Molecular formula: C15H21NO4
CH2OCH3
Relative molecular mass: 279.34 (1987 international relative atomic mass) Reference standards
GB1601
GB1605
GB5451
Marking for dangerous goods packaging
Method for determination of hydrogen ion concentration of pesticides
Sampling method for commercial pesticides
Method for determination of wettability of pesticide wettable powders HG2-896 Method for determination of fineness of pesticide powders 3 Technical requirements
3.1 Appearance: Light yellow loose powder, without lumps. 3.2 Metalaxyl wettable powder shall also meet the following technical requirements: Item
Metalaxyl content, %(m/m)
Suspension rate, %(m/m)
Wetting time, s
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
HG2208-91
The sample is extracted with acetone and dibutyl phthalate is used as the internal standard. The metalaxyl wettable 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 175~246um); micro syringe: luL;
Centrifuge: with 10mL centrifuge tube.
4.1.4 Operation steps
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.
HG2208—91
The above operating conditions are the operating parameters on the GC-9A gas chromatograph. The operating parameters can be appropriately adjusted according to the characteristics of the instrument to obtain the best effect.
Figure 1 Gas chromatogram of metalaxyl wettable powder 1—Solvent, 2—Impurity No. 1, 3—Impurity No. 2, 4—Internal standard, 5—Metalaxyl, 6—Impurity No. 3 4.1.4.3 Preparation of standard solution and sample solution Standard solution: weigh 0.12g of metalaxyl, accurate to 0.0001g of standard substance and 0.10g of dibutyl phthalate, accurate to 0.0001g, put them in a clean, dry glass bottle with a stopper, dissolve with 3mL of acetone, shake well, and set aside. Sample solution: weigh 0.12g of metalaxyl, accurate to 0.0001g of wettable powder sample and 0.10g of dibutyl phthalate. Accurate to 0.0001g, put it in a 20mL stoppered conical bottle, add 5mL acetone, and shake vigorously for 5min; then, pour the solution into a 10mL centrifuge test tube, centrifuge for 5min (3500r·pm), take part of the clear liquid into a clean, dry glass stoppered bottle for testing. 3
W.4.1.4.4 Determination
HG2208-91
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 and the change is not greater than 1.2%), then analyze in the following order: a. 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: mi·As·w
Wherein: mi.m.-
- are the masses of metalaxyl and internal standard substance in the standard solution, AA. mm2 are the average peak areas of metalaxyl and internal standard substance in the chromatograms of the two standard solutions, mm2 are the percentage content of metalaxyl standard substance.
Calculate the percentage of metalaxyl by the average of the peak areas of metalaxyl and internal standard in the chromatograms of the two sample solutions b and c. 11
Where: Yu—Correction factor for metalaxyl; mi, ms
A, A, respectively, are the masses of metalaxyl and internal standard in the sample solution, mm2. 4.1.4.6 Allowable difference
The difference between the results of two parallel determinations of this method shall not exceed 0.5%. 4.2 Determination of suspension rate
4.2.1 Reagents and solutions
Anhydrous calcium chloride (GB3208)
Anhydrous magnesium chloride (GB672),
Standard hard water: 342ug/g, prepared according to the provisions of GB5451. 4.2.2 Instruments
(2)
Graduating cylinder: 250mL, ground glass stopper, the distance between 0~250mL scale should be 20.0~21.5cm, the distance between 250mL scale line and the bottom of the stopper should be 4~6cm;
Glass pipette: about 30cm long, inner diameter about 5mm, inner diameter of the tip is 2~3mm, and the tube mouth is facing upward; constant temperature water bath.
4.2.3 Determination steps
Weigh 2.5g of metalaxyl wettable powder to the nearest 0.0001g, put it in a 100mL beaker, add 10mL standard hard water, stir with a glass rod, after the sample is completely wetted, wash all the samples in the beaker into a 250mL measuring cylinder with standard hard water, add standard hard water to the 250mL scale line, cover the measuring cylinder stopper, put it in a 30±1℃ constant temperature water bath, make the liquid level of the measuring cylinder at least not higher than the horizontal plane of the water bath, when the temperature of the suspension in the measuring cylinder is consistent with the water temperature, take out the measuring cylinder, regularly turn it upside down 15 times (about 0.5min) with the bottom of the measuring cylinder as the axis, so that it becomes a uniform suspension, put the measuring cylinder back into the constant temperature water bath, open the stopper, let it stand for 30min, and then use a pipette to extract 9/10 of the suspension in the upper part of the measuring cylinder by suction (10-30s to complete the extraction). When drawing liquid, the pipette should be attached to the wall of the measuring cylinder and descend with the liquid level. Do not let the lower sediment be vibrated. Then, add 10mL of benzene and 0.03g of dibutyl phthalate to 0.0001g into the measuring cylinder, cover it with a stopper and shake it vigorously for 5 minutes. Let it stand. After stratification, put the organic layer into a 10mL centrifuge test tube and centrifuge it for 5 minutes (3500r.pm). Take the upper part of the liquid and put it into a dry and clean glass bottle with a stopper. Determine it according to the steps specified in 4.1.4.4. 4.2.4 The suspension rate of metalaxyl wettable powder is calculated as follows: a2 = m1 - m2 ×
Wherein: m1
-the mass of metalaxyl in the sample used to prepare the suspension, gm2
the mass of metalaxyl in the 1/10 suspension remaining in the measuring cylinder, g. 4.3 Determination of wetting time
Determine according to the method in GB5451.
4.4 Determination of pH value
Determine according to the "pH meter method" in GB1601. 4.5 Determination of fineness
Determine according to the method in HG2-896.
5 Inspection rules
(3)
5.1 Metalaxyl wettable powder shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all metalaxyl wettable powders shipped out of the factory meet the requirements of this standard. Each batch of metalaxyl wettable powder shall be accompanied by a quality certificate in a certain format when it leaves the factory. 5.2 Users have the right to verify the metalaxyl wettable powders received in accordance with the provisions of the standard. Whether the quality of wettable powder meets the requirements of this standard. 5.3 The sampling method shall 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 are pasted on the bottles, indicating the name of the manufacturer, product name, batch number, and sampling date. One bottle is used for inspection, and the other bottle is sent to the quality supervision and inspection department for storage for arbitration.
5.4 As for the inspection results, if some indicators do not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-inspection. As a result of the re-inspection, even if only one indicator does not meet the requirements of this standard, the entire batch of metalaxyl wettable powder is The agent cannot be accepted. 5.5 When the supply and demand parties have a dispute over product quality, the two parties can negotiate to resolve it, or select an arbitration agency to conduct arbitration inspection according to the methods specified in this standard.
6 Marking, packaging, transportation and storage
6.1 Metalaxyl wettable 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 barrel 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" 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 with good ventilation; it must not be mixed with food, seeds and feed; avoid contact with the skin and prevent inhalation through the mouth and nose.
6.4 The warranty period of this product is two years.
Wo
Additional instructions:
HG 220891
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. W.
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