Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2206—91
Published on November 18, 1991
Metalaxyl Technical
Implemented on July 1, 1992
Ministry of Chemical Industry of the People's Republic of China
WChemical Industry Standard of the People's Republic of China
Metalaxyl Technical
Subject Content and Scope of Application
HG2206—91
This standard specifies the technical requirements, inspection methods, inspection rules, and marking, packaging, transportation and storage requirements for metalaxyl technical. This standard applies to metalaxyl technical prepared by the condensation of N-(2,6-xylyl)-aminopropionic acid methyl ester and methoxyacetyl chloride. Active ingredient: Metalaxyl
Chemical name: N-(2,6-xylyl)-N-(2-methoxyacetyl)-DL-aminopropionic acid methyl ester Structural formula:
Molecular formula: C15H21NO4
CooCH3
CH20CH3
Relative molecular mass: 279.34 (according to the international relative atomic mass in 1987) 2 Reference standards
Dangerous goods packaging mark
Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in chemical reagent test methods GB1605
5 Sampling method for commercial pesticides
3 Technical requirements
3.1 Appearance: yellow to brown solid.
Metalaxyl technical shall also meet the following technical requirements: %(m/m)
Metalaxyl content
Acidity (in H2SO,)
Acetone insoluble matter1)
Note: 1) is a type inspection item.
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991Superior product
First-class product
Qualified product
Implemented on July 1, 1992
W.4 Inspection method
4.1 Determination of metalaxyl content
4.1.1 Summary of method
HG2206-91
The sample was dissolved in acetone, dibutyl phthalate was used as the internal standard, and the metalaxyl technical was 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 above 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-mosorb W/AW-DMCS, particle size 180~250um (or 102 white silanized support, particle size 180~250um); Micro syringe: luL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
a Coating of stationary liquid: Accurately weigh 0.2g cyclohexanedimethanol succinate polyester, dissolve in 16mL chloroform, then add 4g Chromosorb W/AW-DMCS, shake gently to make the support completely immersed in chloroform, and after drying, put it in a 100℃ oven for h.
Filling of chromatographic column: Connect a glass funnel to the inlet of the clean and dry chromatographic column, wrap the outlet 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 inlet and outlet of the column respectively. c. Aging of chromatographic column: Connect the inlet of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the detector to the outlet for the time being. Pass the carrier gas at a flow rate of about 20mL/min, and keep it at a column temperature of 240℃ for 24h. After cooling down, connect the outlet of the column to the detector. 4.1.4.2 Gas chromatographic operating conditions
Temperature:
Column chamber 205℃;
Vaporization chamber 250℃,
Detection chamber 250℃.
Gas flow rate:
Carrier gas (N2) 40mL/min;
Hydrogen 50mL/min;
Air 500mL/min.
Recording paper speed:
4mm/min.
Injection volume:wwW.bzxz.Net
Retention time:
W.bzsoso.cOIMetalaxyl about 7min;
Internal standard about 5min,
Impurity No. 1 about 3min;
Impurity No. 2 about 4min;
Impurity No. 3 about 10min.
HG2206—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.
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, 0.10g of dibutyl phthalate, accurate to 0.0001g, place 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 technical sample, 0.10g of dibutyl phthalate, accurate to 0.0001g, place in a clean, dry glass bottle with a stopper, dissolve with 3mL of acetone, shake well, and set aside. 4.1.4.4 Determination
Under the above gas chromatography conditions, after the instrument is stable, inject several injections of standard solution until the peak area ratio of two adjacent injections is basically stable (the change is not more than 1.2%), and then analyze in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
4.1.4.5 Calculation
According to the average peak area of metalaxyl and internal standard substance in the chromatograms of the two standard solution injections a and d, calculate the correction factor f of metalaxyl: f
Where: mi, m.-respectively represent the mass of metalaxyl and internal standard substance in the standard solution, g; Ai, A.-respectively represent the average peak area of metalaxyl and internal standard substance in the chromatograms of the two standard solution injections, mmD
-the percentage content of metalaxyl standard substance.
The average of the peak areas of metalaxyl and internal standard in the chromatograms of the two sample solutions b and c is used to calculate the percentage of metalaxyl X1: x, -f: nAx100
Where: f—metalaxyl correction factor; mi, ma
—are the masses of metalaxyl and internal standard in the sample solution, A, A respectively. ——are the average of the peak areas of metalaxyl and internal standard in the chromatograms of the two sample solutions, mm2 respectively. 4.1.4.6 Allowable difference
The difference between the results of two parallel determinations in this method shall not exceed 1.5%. 4.2 Determination of acidity
4.2.1 Reagents and solutions
Acetone (GB686);
Sodium hydroxide (GB629) standard solution: c (NaOH) = 0.02 mol/L, prepared and calibrated according to GB601 and then diluted. Bromocresol green: 1g/L ethanol solution, prepared according to GB603. 3
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HG2206—91
Weigh 1g of the sample, accurate to 0.0001g, and place it in a 250mL conical flask. Add 50mL acetone to dissolve the sample, then add 50mL distilled water, shake well, add 5 drops of bromocresol green indicator, and titrate with sodium hydroxide standard solution until the color turns grass green, which is the end point. At the same time, make a blank determination.
4.2.3 Calculation
The percentage of acidity of metalaxyl technical is calculated according to formula (3): X2=: (V1-V2)X0. 049,
Wherein: c—concentration of sodium hydroxide standard solution, mol/L, Vi——volume of sodium hydroxide standard solution consumed by titration sample, mLV2—volume of sodium hydroxide standard solution consumed by titration blank, mL,—weight of metalaxyl technical, g
(3)
0.049—mass of sulfuric acid equivalent to 1.00mL sodium hydroxide standard solution [c(Na0H)-1.000mol/LJ, expressed in grams. 4.3 Determination of acetone insoluble matter
4.3.1 Apparatus and reagents
G4 glass sand core crucible;
Suction filter flask: 500mL;
Acetone (GB686).
4.3.2 Determination steps
Wash the G4 sand core crucible, dry it to constant weight, accurate to 0.0001g, then put it on a 500mL suction filter flask, weigh 10g of sample, accurate to 0.0001g, add 50mL acetone to a 100mL beaker, shake the beaker, and after the solid soluble in acetone is completely dissolved, transfer all of it to the crucible, filter it under vacuum, wash the crucible with 100mL acetone three times, drain it, remove it, and put it in a 110℃ oven to dry it to constant weight, accurate to 0.0001g. The percentage of acetone insoluble matter X3 is calculated according to formula (4): Xas
Wherein: m1——mass of the sand core crucible after constant weight, g, m2m1
m2—total mass of the crucible and acetone insoluble matter after constant weight, gm—sample weight, g.
5 Inspection rules
5.1 Metalaxyl technical should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all metalaxyl technical leaving the factory meets the requirements of this standard. Each batch of metalaxyl technical should be accompanied by a quality certificate in a certain format when leaving the factory. 5.2 The user has the right to verify the quality of the metalaxyl technical received in accordance with the provisions of the standard to see if it meets the requirements of this standard. 5.3 The sampling method should be carried out in accordance with GB1605; mix 200g of the sample evenly and put it into two clean, dry glass bottles with ground stoppers. A label is attached to the bottle, indicating the manufacturer's name, product name, batch number, and sampling date. One bottle is used for inspection, and the other is sent to the quality supervision and inspection department for storage for arbitration.
5.4 If any of the test results do not meet the requirements of this standard, a re-sample should be taken from the packaging barrel with twice the amount for inspection. If only one of the re-inspection results does not meet the requirements of this standard, the entire batch of metalaxyl technical cannot be accepted. 5.5 When the supply and demand parties have a dispute over product quality, the dispute can be resolved through negotiation, or an arbitration agency can be selected to conduct arbitration inspection according to the method specified in this standard.
HG2206-91
Figure 1 Gas chromatogram of metalaxyl technical
1-Solvent; 2-Impurity No. 1, 3-Impurity No. 2; 4-Internal standard, 5-Metalaxyl; 6-Impurity No. 3 5.6Acetone insoluble matter should be inspected at least once a month. 6 Marking, packaging, transportation and purchase and storage
6.1 Metalaxyl technical is packaged in galvanized iron drums, with a net weight of 50kg per drum. 6.2 The drums should be firmly marked. The contents include: 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, and avoid contact with the skin and prevent inhalation through the mouth and nose.
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Additional instructions:
HG 220691
This standard is 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 is 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.
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