Determination method of content of fusel in ethylene carbonate

A ethylene carbonate and determination method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large damage to the injection needle, poor precision, easy crystallization, etc., and achieve the effect of improving accuracy and accurate detection

Inactive Publication Date: 2016-02-10
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Abstract
  • Description
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Problems solved by technology

However, there are still some defects in the above-mentioned technology: the error of chemical titration is large and the accuracy is poor, and the accuracy of gas chromatography is relatively high. Accurate Quantitative Analysis of Fusel Alcohols in Esters
Moreover, the existing gas phase detection methods all adopt the direct injection of samples. However, the characteristics of ethylene carbonate samples are very easy to crystallize at room temperature. The analyzed chromatogram is asymmetrical, and the non-sharp tailing seriously affects the accuracy of the detection results

Method used

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  • Determination method of content of fusel in ethylene carbonate
  • Determination method of content of fusel in ethylene carbonate
  • Determination method of content of fusel in ethylene carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (a) Put the ethylene carbonate in an oven to melt, after the melting is complete, use a needle to measure 400mL of the melted ethylene carbonate into a 500mL volumetric flask, and then use acetone to dilute to a certain dilution factor obtained by the graduation line ’S stock solution;

[0029] (b), respectively weigh about 0.1g of ethylene glycol and diethylene glycol in a 100mL volumetric flask, use the solution in (a) to make up to the mark to obtain the standard of ethylene glycol and diethylene glycol with a concentration of 1000ppm liquid;

[0030] (c) To prepare standard samples with different concentration gradients of the 1000 ppm ethylene glycol and diethylene glycol standard solutions in (b), the stock solution in (a) should be used as the diluent;

[0031] (d), set the chromatographic conditions:

[0032] Chromatographic column: DB-WAXETR (60m*0.32mm*0.32um) Inlet temperature: 250℃; detector temperature 250℃; sampling mode: splitless injection; split ratio 20:1; co...

Embodiment 2

[0036] (a) Put the ethylene carbonate in an oven to melt. After the melting is complete, use a needle to measure 400mL of the melted ethylene carbonate into a 500mL volumetric flask, and then use benzene to dilute to a certain dilution factor obtained by the graduation line ’S stock solution;

[0037] (b), respectively weigh about 0.1g of ethylene glycol and diethylene glycol in a 100mL volumetric flask, use the solution in (a) to make up to the mark to obtain the standard of ethylene glycol and diethylene glycol with a concentration of 1000ppm liquid;

[0038] (c), according to the needs, prepare the standard samples of 1000 ppm ethylene glycol and diethylene glycol in (b) into standard samples with different concentration gradients, and use the stock solution in (a) as the diluent;

[0039] (d), set the chromatographic conditions:

[0040] Chromatographic column: DB-FFAP, inlet temperature: 250°C; detector temperature: 250°C; sampling mode: splitless injection; split ratio 20:1; co...

Embodiment 3

[0044] (a) Put the ethylene carbonate in an oven to melt, after the melting is complete, use a needle to measure 400mL of the melted ethylene carbonate into a 500mL volumetric flask, and then use acetonitrile to dilute to a certain dilution factor obtained by the graduation line ’S stock solution;

[0045] (b), respectively weigh about 0.1g of ethylene glycol and diethylene glycol in a 100mL volumetric flask, use the solution in (a) to make up to the mark to obtain the standard of ethylene glycol and diethylene glycol with a concentration of 1000ppm liquid;

[0046] (c), according to the needs, prepare the standard samples of 1000 ppm ethylene glycol and diethylene glycol in (b) into standard samples with different concentration gradients, and use the stock solution in (a) as the diluent;

[0047] (d), set the chromatographic conditions:

[0048] Chromatographic column: DB-WAX, inlet temperature: 250°C; detector temperature: 250°C; sampling method: splitless injection; split ratio 20...

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Abstract

The invention particularly relates to a determination method of the content of fusel in ethylene carbonate. The determination method comprises the following steps: preparing a plurality of ethylene carbonate solutions containing the fusel with different concentrations; carrying out gas chromatography and drawing an external standard curve according to a peak area and the corresponding concentration of the fusel; after diluting a to-be-detected sample ethylene carbonate to certain times by using a solvent to obtain a to-be-detected solution; detecting the to-be-detected solution according to pre-set chromatographic conditions to obtain a corresponding peak area; and calculating to obtain the content of the fusel according to the drawn external standard curve. Compared with the prior art, the gas chromatography is firstly adopted, and the external standard curve is drawn according to the peak area and the corresponding concentration of the fusel as a standard; after the sample to be detected is prepared into the solution, the solution is compared with the standard and the content of the fusel is finally calculated; damages to a gas chromatograph are reduced; and meanwhile, the accuracy of a detection result is also improved and the content of the fusel in ethylene carbonate can be accurately detected.

Description

Technical field [0001] The present invention relates to the field of lithium ion battery manufacturing, in particular to a method for measuring the content of fusel alcohol in ethylene carbonate in the electrolyte of lithium ion battery. Background technique [0002] With the increasing demand for energy saving and environmental protection in recent years, the application of lithium batteries has become more and more widespread. Lithium-ion battery electrolyte is composed of electrolyte salt and solvent. Ethylene carbonate (EC) is an important solvent in the electrolyte. The fusel in the solvent may induce free radical reactions during the battery charge and discharge cycle, accelerate the decomposition of the solution and affect the stability of the battery performance. Therefore, the accurate determination of the fusel content in ethylene carbonate is of great significance. [0003] At present, there are relatively mature technologies to determine the content of ethylene carbona...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 董晓莲何薇徐三善孙孝元史利涛
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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