Dibutyl tin oxide detection method
A technology of dibutyltin oxide and detection method is applied in the directions of measuring device, preparation of test samples, instruments, etc., to achieve the effects of high detection accuracy and simple method
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[0015] Example 1: Put 0.1g DBTO in a 25ml volumetric flask, add 2ml 4mol / l magnesium bromopropane, heat to about 60°C, sonicate for 15 minutes, after the white powder is dissolved (no exothermic reaction occurs), take it out and cool; Add 5ml of 1mol / l sulfuric acid and cool while dripping to destroy the excess Grignard reagent. Add 3.5ml of methanol, add water to 25ml, shake for 10 minutes, stand still for layering, and take the machine layer for color profiling.
[0016] Chromatographic conditions: carrier gas: N 2 , Carrier gas pressure: 0.1MPa, supporting gas: air, supporting gas pressure: 0.05MPa, gas: hydrogen, gas pressure: 0.1MPa, capillary column: Se-30, vaporization chamber temperature: 250°C, detection chamber temperature: 250°C , Column temperature: 180℃.
Example Embodiment
[0017] Example 2: Put 0.1g DBTO in a 25ml volumetric flask, add 2ml of 4mol / l propylmagnesium chloride Grignard reagent, heat to about 60℃, ultrasonic for 15 minutes, after the white powder is dissolved, take it out and cool, add 5ml ring Hexane, use 1N H 2 SO 4 5ml destroy excess Grignard reagent, add 3.5ml methanol, H 2 O 5ml, shake for 10min, statically separate into layers, and take the organic layer for analysis. Sepu conditions are the same as above.
Example Embodiment
[0018] Example 3: Take 0.1g of DBTO and place it in a 25ml volumetric flask, add 4mol / l of ethylated magnesium bromide (CH 3 CH 2 MgCl 2 ) 2ml of Grignard reagent, heated to about 60℃, ultrasonic for 15 minutes, after the white powder is dissolved, take it out and cool, add 5ml of butyl ether, use 1N H 2 SO 4 5ml to destroy excess Grignard reagent, add 3.5ml of ethanol, H 2 O5ml, shake for 10min, statically separate into layers, and take the organic layer for analysis.
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