Some standard content:
Ministry of Chemical Industry of the People's Republic of China
Ministry Standard
Isoblast Crude Oil
HG2-1418-81
Ministry Standard of the Ministry of Chemical Industry of the People's Republic of China
Isoblast Crude Oil
This standard applies to industrially synthesized Isoblast Crude Oil. Its main purpose is to prepare Isoblast EC. Active ingredient: 0,O-diisopropyl-S-phenylthiophosphate. Molecular formula: C1sH21O:PS
Structural formula:
Molecular weight: 288.35 (according to the international atomic weight in 1979)0
I. Technical conditions
1. Appearance: light yellow or light brown liquid. 2. Isoblast clean crude oil should meet the following index requirements:
0,0-diisopropyl-S-phenylthiophosphate content, % moisture content, %
II. Acceptance
HG2-1418-81
Group 23
3. Isoblast clean crude oil should be inspected by the technical inspection department of the manufacturer. The manufacturer should ensure that all Isoblast clean crude oil shipped out of the factory meets the requirements of this standard. Each batch of Isoblast clean crude oil shipped out of the factory should 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 clean crude oil in accordance with the provisions of this standard to verify whether its indicators meet the requirements of this standard. 5 Sampling method: Take one sample from each batch of products, the sampling amount is not less than 0.5 kg, seal and store, and stick a label, indicating: the name of the manufacturer, product name, batch number, sampling date, and send it to the inspection department for inspection. 6. If one of the indicators in the test results does not meet the standard, double sampling should be carried out for verification. If even one of the indicators does not meet the requirements, the batch of products shall be rejected. Issued by the Ministry of Chemical Industry of the People's Republic of China Shanghai Municipal Bureau of Chemical Industry
January 1, 1983
Shanghai Pesticide Factory
HG2-1418-81
III. Test Methods
7. Determination of the content of O,O-diisopropyl-S-phenylthiophosphate (1) Instruments and reagents
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: Isoblastine pure product 99.5%; 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 60-80 mesh 101 silanized white support or 101 white acid-washed support, so that the support is completely immersed in the solution of the stationary liquid phenyl silicone rubber and shake it thoroughly. Place the round-bottom flask in a water bath at 80℃. 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 60-80 parts, 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℃ 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 of the column to the identifier. When the instrument enters the normal working state under specific operating conditions, that is, when the baseline is stable, inject a certain amount of sample with internal standard. If a stable relative response value can be obtained, the measurement work can be started.
(3) Working conditions
Column temperature: 165℃;wwW.bzxz.Net
Vaporization chamber temperature: 200℃;
Detection chamber temperature: 200℃;
Carrier gas (N,): column head pressure 1 kg/cm2, 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) 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 weigh 0.1 g of pure isopyrite (or a standard containing 0.1 g of isopyrite), dilute it with 5 ml of acetone, shake well and set aside. b: Sample determination: Accurately weigh 0.1 g (accurate to 0.0002 g) of dibutyl phthalate into a clean penicillin bottle, then weigh 0.13 g (accurate to 0.0002 g) of sample, dilute it with 5 ml of 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. Calculation of content
Isoblast net %=
Wm·hsent×100
hstandard·Wsample
HG2-1418-81
W—When preparing standard solution: weight of dibutyl phthalate Isoblast net weight
W#——When preparing sample: weight of dibutyl phthalate" sample weight
standard——When adding standard sample·peak height of dibutyl phthalate" peak height of Isoblast net
hsample—When adding sample·peak height of dibutyl phthalate·peak height of Isoblast net
8. Determination of moisture
According to GB1600-79 "Determination of moisture in pesticides". IV. Packaging, marking, storage and transportation
9. The packaging of Isoblast net crude oil shall temporarily adopt the emulsion packaging standard. 10. 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 standard number. 11. 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". 12. 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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