Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2315-92
Mancozeb Wettable Powder
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 Wettable Powder
Subject Content and Scope of Application
HG2315-92
This standard specifies the technical requirements, inspection methods, inspection rules, and marking, packaging, transportation and storage requirements for mancozeb wettable powder.
This standard applies to wettable powders made from mancozeb technical materials, additives and fillers that meet industry standards. Active ingredient: Mancozeb
Chemical name: Coordination complex of ethylene-1,2-bis(dithiocarbamate) manganese and zinc Structural formula:
CH,NH-C
CH2-NH-
Molecular formula: (C,HN,S,Mn)(Zn)
2 Reference standards
Dangerous goods packaging mark
GB1600
GB1601
GB1604
GB16 05
GB3796
GB5451
Picture mark for packaging, storage and transportation
Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in test methods of chemical reagents Determination of moisture content of pesticides
Determination of hydrogen ion concentration of pesticides
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
Determination of wettability of pesticide wettable powders HG 2—896
Determination of fineness of pesticide powders
3 Technical requirements
3.1 Appearance: Grayish yellow loose powder, without lumps. 3.2 Mancozeb wettable powder shall meet the requirements of the following indicators: Approved by the Ministry of Chemical Industry of the People's Republic of China on June 1, 1992 and implemented on January 1, 1993
Mancozeb content, % (m/m)
Manganese content\, % (m/m)
Zinc content\, % (m/m)
Water content, % (m/m)
Suspension rate, % (m/m)
Fineness (through 45um sieve), % (m/m)Wetting time, s
pH value (1% aqueous dispersion)
Hot-stick stability (54±2℃, 14 days)3)>
HG2315-92
Note: 1) and 2) are the mass percentages of the actual measured content of mancozeb, and shall be inspected at least once a month; 3) shall be inspected at least once every six months.
4 Test method
4.1 Determination of mancozeb content
4.1.1 Summary of method
6.0～9.0
The sample is decomposed in boiling hydroiodic acid-glacial acetic acid solution to generate carbon disulfide, ethylenediamine salt and hydrogen sulfide gas. 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:
(CHN,SMn)(Zn)+4H++2I-
IHsNCH2CH2NHsI+2rCS+rMn+uZn2+CS2+C2HgOK
-C,H.OCSSK
2CH0CSSK+1-CH0C(S)SSC(S)OCH+2KIReagents and solutions
Ethanol (GB678);
Glacial acetic acid (GB676) solution: 30% (V/V); Potassium hydroxide (GB2306) ethanol Solution: 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; Phenolphthalein indicator solution: 10g/L, prepared according to Article 4.5.22 of GB603. 4.1.3 Instruments
According to Figure 1.
4.1.4 Determination steps
HG231592
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℃) to evacuate moisture
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 24 bubbles per second evenly and stably through the absorption tube. Add 50mL of hydroiodic acid-glacial acetic acid solution to the round-bottom flask through the long-necked funnel and shake it 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 phenolic acid indicator solution, wash until there is no residue in the tube, neutralize with acetic acid solution until the phenolic acid fades, then add 3 to 4 drops in excess, immediately titrate with iodine standard titration solution, and shake continuously. 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 mancozeb1 is calculated according to formula (1): c(V1-V2)×0.1355
Wherein: V
The volume of iodine standard titration solution consumed by titrating the sample, mL; The volume of iodine standard titration solution consumed by titrating the blank, mL: V
m——the mass of the sample, g;
The actual concentration of the iodine standard titration solution, mol/L; (1)
0.1355——The mass of mancozeb expressed in grams equivalent to 1.00mL of iodine standard titration solution Cc(1/212)=1.000mol/). 4.1.6 Allowable difference
The difference between the results of two parallel determinations should not exceed 1.0%. 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. 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:0F-+H,02HSO3-+1/202
MnO-+5Fe2++8H+
+5Fe3++Mn2++4H20
4.2.2 Reagents and solutions
Nitric acid (GB626);
Phosphoric acid (GB282);
Disodium hydrogen phosphate ( GB1263) 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,),Fe(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 mancozeb sample 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 bottle, stop heating and cool it naturally, add 70mL of water and rinse the bottle 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 ammonium ferrous sulfate standard 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-volume of standard ammonium ferrous sulfate titration solution consumed in titration, mL;-mass percentage of mancozeb in the sample; m-mass of the sample, g;
(2)
0.01099-mass of manganese expressed in grams equivalent to 1.00mL standard ammonium ferrous sulfate titration solution (c[(NH4+)zFe(SO4+)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
The sample is decomposed with nitric acid, neutralized with sodium hydroxide, precipitated with 8-hydroxyquinoline in acetic acid-sodium acetate buffer, filtered with glass core and weighed to a constant value. Ascorbic acid is added to prevent the precipitation of manganese water. The reaction formula is as follows:
Zn2++2
4.3.2 Reagents and solutions
Nitric acid (GB626);
Ascorbic acid;
HG231592
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.bzxz.net
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 into a 500mL beaker with a G2 glass crucible, wash it with 150mL water for 5 times, add 0.5g ascorbic acid, dissolve it and neutralize it with 400g/L sodium hydroxide solution to pH~2, then neutralize it with 80g/L sodium hydroxide solution to pH~4, add 20mL buffer solution, heat it to 80℃, add 15mL 8-hydroxyquinoline solution while stirring, protect 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 of the mass percentage of zinc: Calculate according to formula (3): m2X0.1717
Wherein: ml——mass of sample, g;
m2——mass of sediment;
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 should not exceed 0.2%. 4.4 Determination of suspension rate
4.4.1 Summary of method
(3)
Use standard hard water to prepare a suspension of known concentration. Under specified conditions, let it stand for 30 minutes, and determine the content of mancozeb in the bottom 1/10 of the suspension. Calculate the suspension rate of the sample based on the content of mancozeb in the sample. 4.4.2 Reagents and solutions
Calcium chloride anhydrous;
Magnesium chloride anhydrous;
Standard hard water: 342ug/g, prepared according to the provisions of GB5451. 4.4.3 Instruments
Measuring cylinder: 250mL, with ground glass stopper, the distance between 0~250mL scale should be 20.0~25.5cm, and the distance between 250mL scale line and the bottom of the stopper should be 4~6cm;
Glass pipette: about 40cm long, inner diameter about 5mm, with a hole of about 2~3mm at one end, and the other end of the pipette is connected to the corresponding vacuum source,
Glass constant temperature water bath: 30±1℃;
Stopwatch.
4.4.4 Determination steps
Weigh 0.5g of the sample (accurate to 0.0001g), place it in a beaker containing 50mL of standard hard water (30±1℃), shake it by hand to make a 5
HG2315-92
circular motion for 2min, place the suspension in a water bath at the same temperature for 13min, then wash it all into a 250mL stoppered cylinder with 30±1℃ standard hard water, dilute to the scale, and cover the stopper. With the bottom of the cylinder as the axis, turn the cylinder upside down 30 times within 1min, then place it vertically in a constant temperature water bath without vibration, open the stopper, and place it for 30min. Use a pipette to remove 9/10 (i.e. 225mL) of the suspension in 10-15s, do not shake or stir up the sediment in the cylinder, and ensure that the top of the pipette is always a few millimeters below the liquid surface. Use a long pipette to draw the remaining 1/10 (i.e. 25 mL) of the suspension into a G2 funnel pre-padded with quantitative filter paper for filtration. Rinse the bottom of the measuring cylinder three times with 15 mL of water, and put the washing liquid into the G2 funnel for suction filtration until it is almost dry. Put the filter cake together with the filter paper into a round-bottom flask, and determine the content of mancozeb according to the steps specified in Article 4.1.4 to calculate its suspension rate. 4.4.5 Calculation
First calculate the mass of mancozeb contained in the remaining 1/10 of the suspension. The mass percentage of the suspension rate of mancozeb wettable powder is 4, calculated according to formula (4): 10 (ml-m2)
...o...
Where: m1—the mass of mancozeb in the sample; m2——the mass of mancozeb in the remaining 1/10 of the suspension in the volume, g. 4.4.6 Allowable difference
The difference between the results of two parallel determinations should not be greater than 5%. 4.5 Determination of pH value
4.5.1 Reagents
Newly boiled and cooled water: pH 5.5~7.0. 4.5.2 Apparatus
100mL measuring cylinder with ground stopper;
pH meter equipped with glass electrode system.
4.5.3 Determination steps
.........(4)
Weigh 10g of sample, put it into a measuring cylinder containing about 50mL of water, add water to 100mL, shake vigorously for 1min, let the suspension settle for 1min, and determine the pH value of the mixed solution according to the relevant provisions of the "pH meter method" in GB1601. 4.6 Determination of thermal storage stability
4.6.1 Apparatus
Glass bottle: 100mL, with ground stopper;
Oven: can be controlled at a constant temperature of 54±2℃;
Dryer: without desiccant.
4.6.2 Determination steps
Weigh 20.0g of the sample and place it in a glass bottle. After the stopper is tightly closed, seal the bottle mouth with a polytetrafluoroethylene film, place the glass bottle in a 54±2℃ oven, and store for 14 days. Take out the glass bottle and place it in a desiccator to cool. Complete all test items within 24 hours. After hot storage, the effective component of mancozeb is allowed to drop to 90% of the content measured before the donation, and the actual suspension rate should not be less than 42%. 4.7 Determination of fineness
Determine according to the HG2-896 medium wet sieving method.
4.8 Determination of wetting time
Determine according to the method in GB5451.
4.9 Determination of moisture
Determine according to the azeotropic distillation method in GB1600. 5 Inspection rules
5.1 Mancozeb wettable powder should be inspected by the quality supervision and inspection department of the manufacturer. All technical indicators listed in this standard are type inspection items. Under normal production conditions, manganese and zinc are inspected at least once a month, and heat storage stability is inspected at least once every six months. Other items are factory inspection items. The manufacturer should ensure that all mancozeb wettable powders shipped meet the requirements of this standard. Each batch of mancozeb wettable powder shipped should 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 whether the quality of the mancozeb wettable powder received meets the requirements of this standard in accordance with the provisions of this standard.
5.3 Sampling method: Factory inspection and user acceptance should be carried out in accordance with the sampling method for wettable powders in GB1605; after mixing the samples evenly, put them into two clean, dry glass bottles with ground mouths, and affix labels on the bottles, indicating the manufacturer's name, product name, batch number, and sampling date. One bottle is sent for inspection and one bottle is retained. 5.4 If any of the indicators in the test results do not meet the requirements of this standard, samples should be taken from twice the amount of packages for retesting. If only one indicator does not meet the requirements of this standard, the entire batch of mancozeb wettable powder will be considered unqualified. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation; or the legal inspection agency can conduct arbitration analysis according to the inspection methods specified in this standard.
6 Marking, packaging, transportation and purchase and storage
6.1 The marking and packaging of mancozeb wettable powder shall comply with the relevant provisions of GB3796. 6.2 Mancozeb wettable powder products should be packaged in double-layer plastic bags or kraft paper bags lined with plastic bags. The net weight of each bag is usually 0.1, 0.2, 0.25, 0.5 and 1.0 kg. After sealing, they are packed into cartons. The net weight of each box does not exceed 25 kg, or other types of packaging are used according to user requirements. Each bag (barrel) is accompanied by a product manual and a factory certificate. The packaging should be tight to prevent moisture absorption. 6.3 The packaging mark should also have the trademark, pesticide product registration number and production license (production permit) 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 prevented from moisture and sunlight, and good ventilation should be maintained. It should not be mixed with food, seeds and feed, and should avoid contact with the skin and absorption through the mouth and nose.
6.5 The warranty period of mancozeb wettable powder is 1 year from the date of production. Within two months, the product quality should meet the requirements of this standard. From the third month, the actual measured content of mancozeb in 70% wettable powder is allowed to decrease by 1.2% per month, and the actual measured content of mancozeb in 50% wettable powder is allowed to decrease by 0.9% per month. Six months after the date of publication, the suspension rate within 1 year should not be less than 45%. 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/WP/TS/9 "Mancozeb Wettable Powder Trial Specification (80)".
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