Some standard content:
Ministry of Chemical Industry of the People's Republic of China
Ministry Standard
Isopyranoblast emulsifiable concentrate
HG2-1419-81
Ministry of Chemical Industry of the People's Republic of China
3 Standard
Isopyranoblast emulsifiable concentrate
HG2-1419-81
Group 23
This standard applies to emulsifiable concentrates prepared with Isopyranoblast crude oil, emulsifiers and solvents. Its main use is agricultural fungicide. Active ingredient: 0,O-diisopropyl-S-phenylthiophosphate. Molecular formula: CisH21O:PS
Structural formula:
Molecular weight: 288.35 (according to the international atomic weight in 1979)o
I Technical Conditions
1. Appearance: light yellow or light brown transparent liquid. 2. Isoblast emulsifiable concentrate shall meet the following index requirements:
0,0-diisopropyl-S-phenylthiophosphate content, % Emulsion stability
Moisture content, %
Acidity (in H,SO,), %
II. Inspection rules
3 Isoblast emulsifiable concentrate shall be inspected by the technical inspection department of the manufacturer, and the manufacturer shall ensure that all Isoblast emulsifiable concentrate shipped out of the factory meets the requirements of this standard. Each batch of Isoblast emulsifiable concentrate shipped out of the factory shall have a quality certificate in a certain format. 4. During the guaranteed use period, the user unit has the right to verify the quality of the received Isoblast emulsifiable concentrate in accordance with the provisions of this standard to verify whether its indicators meet the requirements of this standard. 5. The amount of each batch of Isoblast emulsifiable concentrate shall not exceed the maximum capacity of each mixing pot. Ministry of Chemical Industry of the People's Republic of China
Shanghai Chemical Industry Bureau
January 1, 1983
Shanghai Pesticide Factory
HG2-1419-81
6. Sampling method: Take one sample from each batch of products, the sampling volume shall not be less than 0.5 kg, seal and store, and stick a label with the following: name of the manufacturer, product name, batch number, sampling date, and send it to the inspection department for inspection. 7. If one of the indicators in the inspection results does not meet the standard, double sampling should be carried out for verification. If even one indicator does not meet the requirements, the batch of products shall be rejected. III. Inspection method
8.0, Determination of the content of O-diisopropyl-S-benzyl thiophosphate (1) Instruments and reagents
a. Instrument:
Shanghai 100 gas chromatograph.
b. Reagents:
Support: 101 silanized white support or 101 white acid-washed support (60-80 mesh); stationary liquid: phenyl silicone rubber (maximum operating temperature 230℃); Isoblastine standard: pure Isoblastine; internal standard: dibutyl phthalate (HGB3135-59); solvent: acetone (GB686-78);
Chloroform (chloroform) (GB682-78). (2) Preparation and operation of chromatographic column
First weigh 3 grams of phenyl silicone rubber and place it in a round-bottom flask. Dissolve it completely with acetone and chloroform, then add 97 grams of 6080 mesh 101 silanized white support or 101 white acid-washed support, so that the support is completely immersed in the stationary liquid phenyl silicone rubber solution and shake it thoroughly. Place the round-bottom flask in a water bath at 80°C, slowly drive away the solvent, and shake the flask from time to time. After the solvent is driven away, dry it under an infrared lamp, then use a standard sieve to sieve out the 60-80 mesh part and load it into a stainless steel column with a length of 2 meters and an inner diameter of 4 mm. Load this packed column into the constant temperature box of the chromatograph, do not connect it to the identifier first, and pass a low flow of carrier gas. Slowly heat it to 210°C in sections (more than 2 hours), and then age it at this temperature for 24 hours at a carrier gas flow rate of 30 ml per minute. Then connect the outlet end of the column to the identifier. When the instrument enters the normal working state under specific operating conditions, that is, after the baseline is stable, a certain amount of sample with internal standard is injected. If a stable relative response value can be obtained, the measurement work can be started.
(3) Working conditions
Column temperature: 165°C;
Vaporization chamber temperature: 200°C;
Detection chamber temperature: 200°C;
Carrier gas (H2): column head pressure 1 kg/cm, flow rate 70 ml/min Hydrogen flow rate (H2): 50 ml/min;
Air flow rate: 600 ml/min;
Sensitivity: X100;
Attenuation: X1;
Paper speed 2 mm/min;
Injection volume: about 0.5 μL;
Relative retention value Viso: 0.64.
(4) Preparation of pure Isoblast
Take a certain amount of industrial Isoblast crude oil (content greater than 80%) and evaporate the solvent under reduced pressure to make its content above 95%. Then freeze it at -10°C until Isoblast crystals precipitate, discard the mother liquor, then dissolve the Isoblast crystals in a small amount of methanol at room temperature, filter out mechanical impurities. Then freeze it at -10°C until crystals precipitate, discard the mother liquor, repeat the crystallization 3 to 5 times, and finally take out the crystals for vacuum drying.
(5) Identification of pure Isoblast
HG 2—1419—81
&. Use thin layer chromatography to qualitatively test the components of pure Irvine Blight. Use silica gel G produced by Qingdao Ocean Chemical Plant to make plates. The developing solvent is benzene: acetone = 8:2. The prepared pure Irvine Blight has only one main spot (R, = 0.48) after thin layer chromatography. b. Determine the total phosphorus content by weight method to be more than 99%. c. Determine the melting point of the pure product to be above 20°C.
(6) Quantitative steps
a. Preparation of standard solution
Accurately weigh 0.1 g of dibutyl phthalate (accurate to 0.0002 g) into a clean penicillin bottle, then Then weigh in 0.1g (accurate to 0.0002g) of pure Isoblast (or standard containing 0.1g of Isoblast), dilute it with 5ml acetone, shake well and set aside. b. Sample determination
Accurately weigh 0.1g (accurate to 0.0002g) of dibutyl phthalate into a clean penicillin bottle, then weigh in 0.2g (accurate to 0.0002g) of sample, dilute it with 5ml acetone, shake well. When the instrument enters a stable working state, use a micro-syringe to alternately inject the above standard solution and sample solution for determination. The injection speed should be kept consistent each time, and the response value should reach 60-70% of the full scale. c. Content calculation
Wdong·hcake×100
Isoblast net %=
hstandard·Wsample
Wstandard—when preparing standard solution·weight of dibutyl phthalate Isoblast net weight
(a constant after preparation);
W#—when preparing sample: weight of dibutyl phthalate"sample weight
hstandard—when adding standard sample·peak height of dibutyl phthalate"Isoblast net peak height
hsample—when adding sample: peak height of dibutyl phthalate. Isoblast net peak height
9. Determination of moisture| |tt||According to GB1600-79 "Determination of moisture content in pesticides". 10. Determination of emulsifiable concentrate stability:
According to GB1603-79 "Determination of stability of pesticide emulsions". 11. Determination of acidity
(1) Reagents and solutions
Sodium hydroxide (GB629-81): 0.1N standard solution; methyl red (HG3-958-76): 0.2% ethanol solution; anhydrous ethanol (GB678-78): 50% aqueous solution. (2) Instruments
Burette: 25 ml;
Erlenmeyer flask: 250 ml.
(3) Determination procedure
Accurately weigh about 1 gram of sample into an erlenmeyer flask, add 30 ml of 50% ethanol aqueous solution and 3 drops of methyl red indicator solution, and titrate with 0.1N sodium hydroxide standard solution until it turns orange-yellow. Acidity % (X,) is calculated as follows:
HG2—1419—81
N·VX0.0490
2×100
Wherein: N—equivalent concentration of sodium hydroxide standard solution, N; V—volume of sodium hydroxide standard solution consumed during titration, milliliters; 0.0490—milligram equivalent of sulfuric acid; Www.bzxZ.net
G—sample weight.
IV. Packaging, marking, storage and transportation
12. Irradiated emulsifiable concentrate is packaged in glass bottles, with a net weight of 0.5 or 1 kg per bottle, and is padded with straw covers, straw mats or corrugated paper, and is tightly arranged in boxes, with no more than 20 bottles per box.
13.Each batch of packaged finished products should be accompanied by a quality certificate, the bottle mouth must be sealed, and the box must be firm. The certificate includes: manufacturer name, product name, batch number, production date, net weight and proof that the product quality complies with this standard and the number of this standard. 14 Each box and each bottle should be marked with: manufacturer name, product name, batch number, production date, net weight and this standard number, instructions for use, and marked with the words "toxic" and "fireproof". 15. During storage and transportation, it must be strictly prevented from moisture and sunlight, maintain good ventilation, and must not be mixed with food, seeds, and feed. Avoid contact with the skin and prevent inhalation through the mouth and nose.
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