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

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

CN101241111AInactive Publication Date: 2008-08-13JIANGSU YOKE TECH
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Take 0.1g DBTO and place it in a 25ml volumetric flask, add 2ml 4mol / l bromopropane magnesium, heat to about 60°C, ultrasonic for 15 minutes, after the white powder is dissolved (no exothermic reaction), take out and cool; Add 5ml of 1mol / l sulfuric acid, cool while adding dropwise to destroy the excess Grignard reagent, add 3.5ml of methanol, add water to 25ml, shake for 10 minutes, let it stand still to separate layers, take the organic layer for chromatographic analysis.

[0016] Chromatographic conditions: carrier gas: N 2 , carrier gas pressure: 0.1MPa, auxiliary gas: air, auxiliary 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°C.

Embodiment 2

[0017] Example 2: Take 0.1g DBTO and place it in a 25ml volumetric flask, add 2ml of 4mol / l propane magnesium chloride Grignard reagent, heat to about 60°C, and ultrasonicate for 15 minutes. After the white powder dissolves, take it out and cool it, add 5ml ring Hexane with 1N H 2 SO 4 5ml to destroy excess Grignard reagent, add methanol 3.5ml, H 2 O 5ml, shake for 10min, static layer, take the organic layer for analysis. Color Pu conditions as above.

Embodiment 3

[0018] Embodiment 3: Get 0.1g DBTO and place in 25ml volumetric flask, add the ethyl magnesium bromide (CH 3 CH 2 MgCl 2 ) Grignard reagent 2ml, heated to about 60°C, ultrasonicated for 15 minutes, after the white powder was dissolved, took it out and cooled, added 5ml butyl ether, and washed with 1N H 2 SO 4 5ml to destroy excess Grignard reagent, add ethanol 3.5ml, H 2 O5ml, shake for 10min, static layer, take the organic layer for analysis.

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Abstract

The present invention relates to a method for detecting content of dibutyltin oxide (DBTO) by chromatography exactly. Wherein, the dibutytin oxide and excessive 1-8 C alkyl derivatives grignard reagent are reacted under ultrasonic action, residual grignard reagent is destroyed by excessive acid, organic non-polar solvent is added to extract to obtain dibutyltin alkyl substitution which is insoluble in water and has lower boiling point, content of dibutyltin alkyl substitution is detected by organic phase chromatography. The dibutyltin oxide precision detection can be realized by equivalent conversion of dibutyltin alkyl substitution which can be analyzed by chromatography. The present invention is simple, feasible and the detection precision is high, the problem that no method in present can detect exactly the dibutyltin oxide content is solved.

Description

technical field [0001] The invention relates to a detection method capable of accurately measuring the content of dibutyltin oxide (DBTO) by using a color spectrum. Background technique [0002] The organic compound of metal tin, dibutyltin oxide (DBTO), its content detection has a very important impact on the application of DBTO. DBTO is a white powder. Due to its special structure, it is insoluble in most organic solvents and only soluble in strong acids. In addition, it is a high-boiling compound whose boiling point is much higher than the maximum operating temperature limit of chromatography, so it cannot be directly processed. Chromatographic analysis of samples, so its content detection is extremely difficult. At present, the determination of DBTO content is usually only possible by measuring the content of tin in DBTO, and then calculating and deducing it according to the molecular formula. However, DBTO often contains other tin compound impurities, such as monobuty...

Claims

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Application Information

Patent Timeline
13 Aug 2008
Publication
CN101241111A
IPC
G01N30/00; G01N1/28
Inventors
沈琦; 周乐群