Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2213—91
Granubatyl Technical
Issued on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
Chemical Industry Standard of the People's Republic of China
Granubatyl Technical
Subject Content and Scope of Application
HG2213—91
This standard specifies the technical requirements, inspection methods, inspection rules, and marking, packaging, transportation and storage of Granubatyl Technical. This standard applies to Granubatyl Technical synthesized from para-chlorine, diethylamine and carbon oxysulfide. Active ingredient: Gramine Sulfate
Chemical name; S-(4-chloro) N,N-diethylthiocarbamate Structural formula:
Molecular formula: C1H1CINOS
Relative molecular mass: 257.78 (according to the international relative atomic mass in 1987) Reference standards
GB1600
GB1604
GB1605
GB3796
3 Technical requirements
Method for determination of moisture content in pesticides
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
3.1 Appearance: Light yellow to brownish yellow oily liquid (sometimes with crystals). 3.2 Gramocarb should meet the following index requirements: Item
Gramocarb content
Acidity (measured in HSO4)
Acetone insoluble matter
Note: 1) is a type inspection item.
4 Test method
4.1 Determination of chlorpyrifos content
4.1.1 Summary of method
Superior quality product
Approved by the Ministry of Chemical Industry of the People’s Republic of China on 1991-11-18 93.0
% (m/m)
Qualified product
Implemented on 1992-07-01
HG2213—91
The sample was dissolved in anhydrous ethanol, and chlorpyrifos was separated and quantified using di(2-ethylhexyl) succinate as the internal standard, a chromatographic column filled with 5% DEGA/chromosorbW·AW-DMCS and a hydrogen flame ionization detector. 4.1.2 Reagents and solutions
Trichloromethane (GB682); analytical grade; Www.bzxZ.net
Absolute ethanol (GB678); analytical grade;
Granumidil standard: known content;
Diisooctyl succinate (or dipropylene phthalate): internal standard (no impurities interfering with the analysis); Diethylene glycol adipate DEGA): chromatographic stationary liquid (imported, maximum operating temperature 210°C). chromosorbW·AW-DMCS, 150~180μm (80~100 mesh) chromatographic carrier; Internal standard solution: weigh 8g of diisooctyl succinate (accurate to 0.0002g) and place it in a 100mL volumetric flask, dilute to the mark with absolute ethanol and shake well.
4.1.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector; Chromatographic column: 1m long, 4mm inner diameter stainless steel column, filled with 5% DEGA/chromosorbW·AW-DMCS, 150~180μm (80~100 mesh) filler;
Micro syringe: 10uL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
a. Coating of stationary liquid: Weigh 1.00g of diethylene glycol adipate and place it in a 200mL beaker, add 60mL of chloroform to dissolve it, and slowly pour 20g of dry chromosorbW·AW-DMCS150180um (80~100 mesh) carrier into it to completely immerse the carrier. Place the beaker in a fume hood and slowly evaporate the solvent under an infrared lamp until it is dry (the beaker should be tapped and rotated frequently to ensure that it is evenly coated). Then move it to a 90~100℃ oven and dry it for 30 minutes.
b Filling of the chromatographic column: Connect a small funnel to the inlet of the cleaned and dried stainless steel column, fill the outlet with an appropriate amount of glass wool and wrap it with gauze, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, slowly pour the filler from the funnel, and tap the column wall continuously to make the filler fill the chromatographic column evenly and tightly. Remove the chromatographic column, plug the glass wool at the inlet, and press it appropriately to keep the filler from moving. c. Aging of the chromatographic column: Connect the inlet of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the outlet to the detector for the time being. Raise the temperature to 190℃ in stages at a nitrogen flow rate of about 10mL/min, and age it at this temperature for 24 hours. After cooling down, connect the outlet of the column to the detector.
4.1.4.2 Gas chromatography operating conditions
Temperature:
Column chamber 180℃;
Vaporization chamber 250℃;
Detection chamber 250℃.
Gas flow rate:
Carrier gas (Nz) 60mL/min;
Hydrogen 45mL/min;
Air 500mL/min.
Injection volume:
0.60.8uL.
Retention time:
About 11.5min for fenvalerate, about 9.5min for o-fenvalerate; internal standard
Diisooctyl succinate about 6.0min (about 6.5min for dipropylene phthalate). 2
HG2213—91
Gas chromatogram of chloranil technical
1—internal standard; 2—orthochloranil; 3—chloranilThe above chromatographic conditions are typical conditions of SP-501 gas chromatograph. Appropriate adjustments can be made for different types of instruments to obtain the best results. 4.1.4.3 Preparation of standard solution
Weigh 0.13g of chloranil standard (accurate to 0.0002g) and place it in a sample bottle. Use a 1mL pipette to accurately add 1mL of internal standard solution and shake it well.
4.1.4.4 Preparation of sample solution
Weigh 0.14g of chloranil technical (accurate to 0.0002g) and place it in a sample bottle. Use a 1mL pipette to accurately add 1mL of internal standard solution and shake it well.
4.1.4.5 Determination
After the instrument is stable, inject several needles of standard solution until the peak height ratio of two adjacent needles does not change by more than 1.5%. Then, perform the following injection analysis:
a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
Use a micro syringe to inject 0.60.8uL each time. On the chromatograms of the two needles of sample solution and the two needles of standard solution before and after the sample, the difference between the peak height ratio of chloranol and the internal standard divided by the average value should not be more than 1.5%. Otherwise, the injection needs to be repeated. 4.1.5 Calculation
HG2213-91
Average the obtained peak height ratios of a, d and b, c, and the mass percentage content of fenpyrocarb X1 is calculated according to formula (1): Xi_·m·n
In the formula, Xi is the average value of the peak height ratios of fenpyrocarb and internal standard on the chromatogram of the standard solution; 2 is the average value of the peak height ratios of fenpyrocarb and internal standard on the chromatogram of the sample solution; m2 is the mass of the fenpyrocarb standard, g; m2 is the mass of the fenpyrocarb sample, g; and m3 is the mass percentage content of the fenpyrocarb standard. 4.1.6 Allowable difference
The difference between the results of two parallel determinations should not be greater than 1.5%. 4.2 Determination of acidity
4.2.1 Reagents and solutions
Absolute ethanol (GB678): analytical grade;
Sodium hydroxide: (GB629) standard titration solution, [c(NaOH)=0.02mol/L). (1)
Bromocresol green-methyl red mixed indicator: Mix 2mL (1g/L) methyl red ethanol solution and 10mL (1g/L) bromocresol green and shake well.
4.2.2 Determination steps
Weigh 23g of sample (accurate to 0.0002g) and place it in a 250mL conical flask, add 50mL of absolute ethanol and 2 drops of mixed indicator, and titrate with sodium hydroxide standard solution until the end point is light green, and perform a blank determination at the same time. 4.2.3 Calculation
The acidity X2 of gramcarb expressed as mass percentage is calculated according to formula (2): c(V-V2)X0.049
wherein: c——actual concentration of sodium hydroxide standard titration solution, mol/L; Vi
——volume of sodium hydroxide standard titration solution consumed when titrating the sample, mLV3——volume of sodium hydroxide standard titration solution consumed when titrating the blank, mLm——mass of sample, g;
0.049——volume of sodium hydroxide standard titration solution with 1.00mL [c(NaOH)=1.000mol/L), expressed in grams.
4.3 Determination of water content
Determination shall be carried out according to the Karl Fischer method in GB1600. 4.4 Determination of acetone insoluble matter
4.4.1 Reagents and instruments
Acetone (GB686), chemically pure;
G-3 glass frit;
Suction filter bottle: 500mL.
4.4.2 Determination steps
Weigh 50g of sample (accurate to 0.1g) and place it in a 250mL conical flask, add 60mL of acetone, stir to dissolve it, filter the solution through the weighed (accurate to 0.0002g) suction filter, wash it thoroughly with a large amount of acetone (3×30mL), dry it at 110℃ for 30min, cool it and weigh it (accurate to 0.0002g).
4.4.3 Calculate
The mass percentage X of acetone insoluble matter shall be calculated according to formula (3): 4
HG2213-91
m1-m2x100.
Wherein: m1——mass of the crucible and acetone insoluble matter, g; m2——mass, g;
m——mass of the sample, g.
5 Inspection rules
5.1 Carry out in accordance with the acceptance rules for pesticides in GB1604. 5.2 Carry out in accordance with the provisions of GB1605.
5.3 Acetone insoluble matter is a type inspection item, and the inspection cycle is half a year. 6 Marking, packaging, transportation and purchase and storage
6.1 The packaging and marking of the chlorpyrifos technical shall be carried out in accordance with the relevant provisions of GB3796. (3)
6.2 The technical material of Graminexin should be packaged in clean, dry (with protective coating inside) fully galvanized large iron drums. The net weight of the packaging drum should not exceed 200±1kg. 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, feed, etc., and avoid contact with the skin and prevent inhalation through the mouth and nose.
Additional remarks:
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 technically managed by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Hunan Chemical Industry Research Institute, and Zhuzhou Chemical Plant participated in the drafting. The main drafters of this standard are Xiang Yuanying, Yang Fangbin, and Wei Guizhen. 5
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