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Filler column and gas chromatography and its preparation and organic analysis method

A technology of gas chromatograph and packed column, which is applied in the fields of packing column, gas chromatograph including the packed column and the preparation of the packed column, and the analysis of organic matter in battery electrolyte, which can solve the problems of high cost and large quantitative analysis error , to achieve the effect of large column capacity and reduced error

Inactive Publication Date: 2008-01-16
BYD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the shortcomings of large quantitative analysis error and high cost of the prior art capillary column for analyzing organic matter in battery electrolyte, and to provide a packed column capable of accurately analyzing organic matter in battery electrolyte at low cost

Method used

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  • Filler column and gas chromatography and its preparation and organic analysis method
  • Filler column and gas chromatography and its preparation and organic analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] This example illustrates the effect of using the packed column provided by the invention to analyze organic matter in battery electrolyte.

[0035] (1) Clean the glass tube

[0036] Cut out a hollow glass tube of 1 m × 3 mm (inner diameter), soak it in chromic acid lotion for 12 hours, wash the glass tube with water, ethanol, and acetone in sequence, and dry it in an oven at 100°C for later use.

[0037] (2) Preparation of mixed stationary phase

[0038] In a fume hood, take 1 gram of polyethylene glycol-20000 and dissolve it in about 50 ml of propanol, then mix it with 9 grams of 80-100 mesh 101 acid-washed silanized white support, evaporate acetone in a water bath at 60 ° C, and then infra-red Thoroughly dry under the lamp to obtain stationary phase A.

[0039] In a fume hood, take 1 gram of phenylmethylpolysiloxane with 50% phenyl group content and dissolve it in about 50 ml of propanol, and then mix it evenly with 9 grams of 80-100 mesh 101 acid-washed silanized w...

Embodiment 2

[0062] Prepare and use the packed column according to the method of Example 1, the difference is: the hollow tube is a stainless steel tube of 1.5 meters × 4 mm (inner diameter), soaked for 12 hours with 10% sodium hydroxide, and then sequentially Wash the stainless steel tube with water, ethanol, and acetone, and dry it in an oven at 100°C; the mixed stationary phase uses 60-80 mesh 88 acid-washed silanized white support; the mixed stationary phase includes 15 grams of stationary phase A and 5 grams of stationary phase Phase B; And test the same sample as Example 1 under the following chromatographic conditions:

[0063] Vaporization chamber temperature: 270°C

[0064] Detector (FID): 270°C, air: hydrogen = 10:1;

[0065] Column temperature: The column temperature rise program starts from 80°C at 15°C / min to 100°C, then at 40°C / min to 130°C, and then keeps warm for 3 minutes, then at 40°C / min to 200°C, and then at 25°C ℃ / min rises to 230℃ and keeps warm for 3 minutes;

[0...

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Abstract

A packed column comprises a hollow pipe body and a stationary phase distributed in the pipe body; wherein the stationary phases comprises a stationary phase (A) and a stationary phase (B), both of which are mixed together; the stationary phase (A) is composed of polyethylene glycol and a carrier thereof; the stationary phase (B) is composed of phenyl methyl polysiloxane and the carrier thereof. The invention substitutes the mixed stationary phase packed column comprising polyethylene glycol and phenyl methyl polysiloxane for an organic substance in a capillary tube column quantitative analysis battery electrolyte solution in the prior art, which greatly lowers analysis cost, improves the accuracy of quantitative analysis and guarantees the quality of a battery.

Description

technical field [0001] The present invention relates to a packed column, a gas chromatograph, its preparation, and an analysis method for organic matter, in particular to a packed column, a gas chromatograph including the packed column, a preparation method for the packed column, and an organic matter in battery electrolyte analysis method. Background technique [0002] At present, battery electrolytes, especially lithium-ion battery electrolytes, often contain dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), diethyl carbonate (DEC), ethylene carbonate (EC), propylene carbonate (PC) ), vinylene carbonate (VC), vinyl sulfite (ES), propane sultone (PS), phenylcyclohexane (CHP), biphenyl and other organic substances. If these organic substances in the battery electrolyte are added in an appropriate amount, they can improve the quality of the battery, such as increasing the capacity of the battery, improving the low-temperature discharge performance of the battery, cycle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60
Inventor 付昌维
Owner BYD CO LTD
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