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Method for cleaning gas chromatographic column for analyzing trace impurities in high-purity carbonic ester

A gas chromatographic column and trace impurity technology, applied in the field of gas chromatographic column cleaning, can solve the problems of long time-consuming, cumbersome process, unsuitable for daily operation, etc., and achieve the effect of short time-consuming, simple operation, and no component residue

Inactive Publication Date: 2021-05-14
江苏思派新能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in most cases, the high-temperature aging method has no obvious effect on trace residues with a relatively long retention time, and frequent high-temperature aging will damage the service life of the chromatographic column; cleaning the chromatographic column with a solvent requires disassembly of the chromatographic column, and professional tools are required for operation. The process is cumbersome and time-consuming, not suitable for daily operation

Method used

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  • Method for cleaning gas chromatographic column for analyzing trace impurities in high-purity carbonic ester

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Effect test

Embodiment 1

[0025] After the diethyl carbonate sample analysis instrument has been running for a period of time, it is found that there are 1-10ppm impurity peaks remaining after the diethyl carbonate chromatographic peak, and aging at a temperature 20°C lower than the maximum temperature of the chromatographic column has no obvious effect. Perform the following operate:

[0026] Step 1: Select the diethyl carbonate sample analysis method on the chromatograph to pre-run the instrument;

[0027] Step 2: After the instrument is ready, inject an ultra-pure dimethyl carbonate sample (a dimethyl carbonate content above 99.99%) to run;

[0028] Step 3: After the operation is finished, continue to select the diethyl carbonate sample analysis method to make the instrument pre-run;

[0029] Step 4: After the instrument is ready, run without sample injection;

[0030] Step 5: After the operation is over, perform the verification of no-injection operation, and the aging invalid impurities have bee...

Embodiment 2

[0033] After running the propylene carbonate sample analysis instrument for a period of time, it is found that there are 1-10ppm impurity peaks remaining after the propylene carbonate chromatographic peak, and aging at a temperature 20°C lower than the maximum temperature of the chromatographic column has no obvious effect, and the following operations are performed:

[0034] Step 1: Select the propylene carbonate sample analysis method on the chromatograph to make the instrument pre-run;

[0035] Step 2: After the instrument is ready, inject ultra-pure ethanol samples (more than 99.99% ethanol content) to run;

[0036] Step 3: After the operation is finished, continue to select the propylene carbonate sample analysis method to make the instrument pre-run;

[0037] Step 4: After the instrument is ready, run without sample injection;

[0038] Step 5: After the operation is over, perform the verification of no-injection operation, and the aging invalid impurities have been elim...

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Abstract

The invention discloses a method for cleaning a gas chromatographic column for analyzing trace impurities in high-purity carbonic ester. The method aims to solve the problem that measurement accuracy is influenced by chromatographic column residues in analysis of trace impurities in high-purity carbonic ester, a sample injection cleaning method is adopted, the method is a chromatographic method for keeping sample analysis, and a cleaning agent is injected into a chromatograph for operation, and then one-time non-injection operation is executed. The cleaning agent is an organic solvent capable of dissolving the carbonic ester to be detected, is extremely high in content and lower in boiling point, and does not easily cause component residues; and meanwhile, trace impurity residues can be dissolved out, and the trace impurity residues can be completely eliminated through sample injection-free operation. The method does not need to disassemble and assemble an instrument, is simple to operate and short in time consumption, does not damage the chromatographic column, and has a cleaning elimination rate of trace impurity residues greater than 99%.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a cleaning method for a gas chromatographic column used for analyzing trace impurities in high-purity carbonates. Background technique [0002] High-purity carbonate is mainly used as a solvent in the battery electronics industry, and its impurity content is very high; therefore, in the analysis of trace impurities in high-purity carbonate, the repeatability and reproducibility of chromatographic analysis are required for qualitative and quantitative trace impurities. very high. During gas chromatographic analysis, more or less component residues on the chromatographic column or pyrolysis residues of components, process introduction, etc. will lead to distortion of the analysis results. Therefore, regular targeted maintenance is required, such as high-temperature aging, and even cleaning the chromatographic column with solvents. However, in most cases, the high-temper...

Claims

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Application Information

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IPC IPC(8): B08B3/08G01N30/02
CPCB08B3/08G01N30/02
Inventor 吴雷雷祝秀林黄金豆杨丽
Owner 江苏思派新能源科技有限公司
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