Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2314-92
Mancozeb Technical
Published on June 1, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1993
Chemical Industry Standard of the People's Republic of China
Mancozeb Technical
Subject Content and Scope of Application
HG231492
This standard specifies the technical requirements, test methods, test rules, and marking, packaging, transportation and storage requirements for Mancozeb Technical. This standard applies to Mancozeb Technical.
Active ingredient: Mancozeb
Chemical name: Coordination complex of ethylene-1,2-bis(dithiocarbamate) manganese and zinc Structural formula:
CH2NH-C-
Molecular formula: (CHgN,SMn) (Zn)
Cited standard
GB1600
GB1604
GB1605
GB3796
3 Technical requirements
Dangerous goods packaging marking
Pictorial marking for packaging, storage and transportation
Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in chemical reagent test methods Method for determining moisture content in pesticides
Pesticide acceptance rules
Commercial pesticide sampling method
General rules for pesticide packaging
3.1 Appearance: Grayish yellow solid powder.
3.2 Mancozeb technical shall meet the requirements of the following table: %(m/m）
Mancozeb content
Manganese content
Approved by the Ministry of Chemical Industry of the People's Republic of China on June 1, 1992First-class product
Qualified product
Implemented on January 1, 1993
High zinc content
HG2314-92
First-class product
Note: 1) and 2) are the mass percentages of the actual measured content of mancozeb. 4 Test method
4.1 Determination of mancozeb contentbzxZ.net
4.1.1 Summary of method
%(m/m)
Qualified products
The sample is decomposed in boiling hydroiodic acid-glacial acetic acid solution to generate carbon disulfide, ethylenediamine salt and hydrogen sulfide gas which interferes with the analysis. The hydrogen sulfide is first absorbed by lead acetate solution, followed by potassium hydroxide-ethanol solution to absorb carbon disulfide and generate potassium ethyl sulfonate. The carbon disulfide absorption solution is neutralized with acetic acid and immediately titrated with iodine standard solution. The reaction formula is as follows:
(CHgN,S,Mn)(Zn)+4rH++2aI-
IHgNCH2CH2NHI+2CS2+Mn2++Zn2+CS2+CHOKC,H,OCSSK
2C,HgOCSSK+I2CH.OC(S)SSC(S)oC2H+2KI4.1.2 Reagents and solutions
Ethanol (GB678);
Glacial acetic acid (GB676) solution: 30% (V/V); Potassium hydroxide (GB2306) ethanol solution Liquid: 110g/L, prepared before use; Hydroiodic acid (HG3-952) glacial acetic acid solution: Mix one part (about) 57% hydroiodic acid solution with nine parts glacial acetic acid (V/V), prepared before use;
Lead acetate (HG3-974) solution: 100g/L; Iodine (GB675) standard titration solution: c(1/2I2)=0.1mol/L, prepared and calibrated according to GB601; Starch indicator solution: 10g/L, prepared according to Article 4.5.20 of GB603; Phenolic indicator solution: 10g/L, prepared according to Article 4.5.22 of GB603. 4.1.3 Instrument:
According to Figure 1.
4.1.4 Determination steps
HG2314-92
Figure 1 Decomposition and absorption device
1-150mL flask; 2-straight condenser; 3-long-necked funnel; 4-first absorption tube 5-second absorption tube; 6-water bath (70-80℃)-gas source
Weigh a sample containing about 0.2g of mancozeb (accurate to 0.0001g) and place it in a clean round-bottom flask. Add 50mL of lead acetate solution to the first absorption tube and keep the temperature at 70-80℃. Add 50mL of potassium hydroxide-ethanol solution to the second absorption tube, connect the decomposition and absorption device, and check the sealing of the device. Turn on the cooling water, turn on the exhaust source, control the exhaust speed, and pass 2-4 bubbles per second through the absorption tube evenly and stably. Add 50mL of hydroiodic acid-glacial acetic acid solution to the round-bottom flask through the long-necked funnel and shake evenly. At the same time, heat quickly and carefully to prevent the reaction liquid from rushing out, keep it slightly boiling for 50 minutes, disassemble the device, stop heating, remove the second absorption tube, wash the contents with 200mL water into a 500mL conical flask, check the absorption tube with phenol indicator solution, wash until there is no residue in the tube, neutralize with acetic acid solution until phenolphthalein fades, then add 3 to 4 drops in excess, immediately titrate with iodine standard titration solution, and keep shaking at the same time. When it is close to the end point, add 5mL starch indicator solution, and continue to titrate until the solution is light gray purple. At the same time, make a blank determination.
4.1.5 Calculation
The mass percentage of mancozeb 1 is calculated according to formula (1): c(V-V2)×0.1355
Wherein: Vi-
-the volume of iodine standard titration solution consumed by titrating the sample, mL; V,-the volume of iodine standard titration solution consumed by titrating the blank, mL; m
-the mass of the sample, g;
-the actual concentration of iodine standard titration solution, mol/LX100
-the mass of mancozeb expressed in grams equivalent to 1.00mL iodine standard titration solution [c(1/2I2)=1.000mol/L]. 0.1355
4.1.6 Allowable difference
The difference between the results of two parallel determinations should not be greater than 1.2%. 4.2 Determination of manganese content
4.2.1 Summary of the method
After the sample is decomposed with concentrated nitric acid, the divalent manganese is oxidized to heptavalent manganese with ammonium persulfate, and titrated with standard ammonium ferrous sulfate solution to determine the manganese content of 3
HG2314-92
. The excess ammonium persulfate is heated and boiled to remove it, and the silver ions catalyze the oxidation of divalent manganese. The reaction formula is as follows:
55:0+2Mn*++8H:0-2MnO+10S0+16H+S:0-+H,0-2HSO-+1/20
MnO-+5Fe2++8H+
-5Fe3++Mn2++4H20
4.2.2 Reagents and solutions
Nitric acid (GB626);
Phosphoric acid (GB282);
Disodium hydrogen phosphate (GB126 3) Solution: 200g/L; Ammonium persulfate (GB655) solution: 150g/; Silver nitrate (GB670) solution: 20g/L;
Sodium chloride (GB1266) solution: 5g/L;
Ammonium ferrous sulfate (GB661) standard titration solution: c[(NH,)zFe(SO,)2)=0.1mol/L, prepared and calibrated according to GB6014.13;
N-phenylanthranilic acid indicator solution: 2g/L. 4.2.3 Determination steps
Weigh a sample of mancozeb containing about 0.02g of manganese (accurate to 0.0001g), place it in a 250mL iodine volumetric flask, add 5mL of concentrated nitric acid and carefully heat it on an electric furnace to decompose the sample. When no brown gas is produced in the flask, stop heating and cool it naturally, add 70mL of water and rinse the flask wall, add 15mL of phosphoric acid, 20mL of disodium hydrogen phosphate solution, 10mL of silver nitrate solution and 20mL of ammonium persulfate solution. After shaking well, immediately place it in a boiling water bath and heat it for 20min, take it out and cool it to room temperature, add 10mL of sodium chloride solution, shake well, and immediately titrate it with standard ammonium ferrous sulfate titration solution. When the solution turns light red, add 34 drops of N-phenylanthranilic acid indicator solution, and continue titrating until the solution changes from purple-red to yellow-green, which is the end point.
4.2.4 Calculation
The mass percentage of manganese2 is calculated according to formula (2):2
Wherein: c-
c·VX0.01099
-actual concentration of standard ammonium ferrous sulfate titration solution, mol/L: the volume of standard ammonium ferrous sulfate titration solution consumed in titration, mL; the mass percentage of mancozeb in the sample; m-mass of the sample, g;
(2)
0.01099-the mass of manganese expressed in grams equivalent to 1.00mL standard ammonium ferrous sulfate titration solution (c[(NH,),Fe(SO,)2]=1.000mol/L).
4.2.5 Allowable difference
The difference between two parallel determination results should not exceed 0.3%. 4.3 Determination of zinc content
4.3.1 Summary of the method
After the sample is decomposed with nitric acid, it is neutralized with sodium hydroxide, and 8-hydroxyquinoline is added to acetic acid-sodium acetate buffer for precipitation. After filtering with a glass sand core crucible, the weight is constant. Ascorbic acid is added to prevent the precipitation of manganese water. The reaction formula is as follows:
4.3.2 Reagents and solutions
Nitric acid (GB626);
Ascorbic acid;
HG2314-92
Sodium hydroxide (GB629) solution 80g/L, 400g/L; 8-hydroxyquinoline (HG3-115) ethanol solution: 10g/L; Acetic acid-sodium acetate buffer solution: Weigh 136g of sodium acetate (CH:COONa·3H2O) and dissolve it in appropriate amount of water, add 108mL of glacial acetic acid (GB676), and dilute to 1000mL.
4.3.3 Apparatus
Glass sand core crucible: G2, G4.
4.3.4 Determination steps
Weigh a mancozeb sample containing about 0.02g zinc (accurate to 0.0001g), place it in a 250mL conical flask, add 20mL concentrated nitric acid, carefully heat until no brown gas is produced, prevent violent boiling, cool, add 50mL water, filter the solution through a G2 glass crucible into a 500mL beaker, wash it with 150mL water for 5 times, add 0.5g ascorbic acid, dissolve it, neutralize it with 400g/L sodium hydroxide solution to pH~2, and then neutralize it with 80g/L sodium hydroxide solution to pH~4, add 20mL buffer solution, heat it to 80℃, add 15mL 8-hydroxyquinoma solution while stirring, keep it at 80℃ for 25min, stir it from time to time, filter it with a constant weight G4 glass crucible, use 10mL hot water each time, stir the precipitate and wash it 7 times, and dry it at 110-115℃ to constant weight. 4.3.5 Calculation
Mass percentage of zinc a: Calculate according to formula (3): 2e-m2x0.1717
Wherein: m1—mass of sample, g,
m2—mass of precipitate, ;
1——mass percentage of mancozeb in sample; 0.1717——conversion coefficient of 8-hydroxyquinoline zinc to zinc. 4.3.6 Allowable difference
The difference between two parallel determination results shall not exceed 0.2%. 4.4 Determination of moisture
Determine according to the azeotropic distillation method in GB1600. 5 Inspection rules
(3)
5.1 Mancozeb technical shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all mancozeb technical shipped out of the factory meets the requirements of this standard. Each batch of mancozeb technical shipped out of the factory shall be accompanied by a quality certificate in a certain format. And comply with other provisions of GB1604.
5.2 The user has the right to inspect the quality of the received mancozeb technical in accordance with the provisions of this standard to see if it meets the requirements of this standard. 5.3 Sampling method: Factory inspection and user acceptance shall be carried out in accordance with the technical sampling method in GB1605; after mixing the samples evenly, put them into two clean, dry glass bottles with ground mouths. Labels shall be affixed to the bottles, indicating the manufacturer's name, product name, batch number, and sampling date. One bottle shall be sent for inspection and one bottle shall be retained.
5.4 If any index in the inspection results does not meet the requirements of this standard, re-sampling shall be conducted from twice the amount of packaging. If the re-inspection results show that even if only one index does not meet the requirements of this standard, the entire batch of mancozeb technical shall be unqualified. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation; or the statutory inspection agency shall conduct arbitration analysis according to the inspection method specified in this standard.
6 Marking, packaging, transportation and storage
6.1 The marking and packaging of mancozeb technical shall comply with the relevant provisions of GB3796. 5
HG2314—92
The packaging materials of mancozeb technical can be iron drums, non-combustible plastic drums, paper drums lined with double-layer plastic bags, and strictly sealed to prevent moisture absorption.
6.3 The packaging mark shall also include the trademark, pesticide product registration number and production license (production permit) number, comply with the provisions of GB190, and the quality certificate of the product meeting the requirements of this standard.
6.4 During storage and transportation, it shall be strictly prevented from moisture and sunlight, and good ventilation shall be provided. It shall not be mixed with food, seeds and feed, and avoid contact with skin to prevent absorption 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 was drafted and technically coordinated by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Lou Shaowei, Gao Xiaohui, Zhang Bulong and Shi Liancheng. This standard adopts the (United Nations) Food and Agriculture Organization FAO34/TC/tS/9 "Mancozeb Technical Specifications (80)".3 The packaging mark should also have the trademark, pesticide product registration number and production license (approval) number, and comply with the provisions of GB190 and the quality certificate of the product meeting the requirements of this standard.
6.4 During storage and transportation, it should be strictly protected from moisture and sunlight, and well ventilated. It should not be mixed with food, seeds and feed, and avoid contact with the skin and prevent absorption through the mouth and nose.
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 was drafted and technically coordinated by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard were Lou Shaowei, Gao Xiaohui, Zhang Bulong and Shi Liancheng. This standard refers to the (United Nations) Food and Agriculture Organization FAO34/TC/tS/9 "Mancozeb Technical Specifications (80)". 63 The packaging mark should also have the trademark, pesticide product registration number and production license (approval) number, and comply with the provisions of GB190 and the quality certificate of the product meeting the requirements of this standard.
6.4 During storage and transportation, it should be strictly protected from moisture and sunlight, and well ventilated. It should not be mixed with food, seeds and feed, and avoid contact with the skin and prevent absorption through the mouth and nose.
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 was drafted and technically coordinated by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard were Lou Shaowei, Gao Xiaohui, Zhang Bulong and Shi Liancheng. This standard refers to the (United Nations) Food and Agriculture Organization FAO34/TC/tS/9 "Mancozeb Technical Specifications (80)". 6
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