Purification method of acetonitrile for liquid chromatography-mass spectrometer

A technology of liquid chromatography and purification method is applied in the field of purification of acetonitrile used in a liquid chromatography-mass spectrometer, and can solve the problems of difficult to remove impurities, difficult to acetonitrile, difficult to purify, etc., and to reduce the cost required for imports, The production process is simple and the effect of expanding the scope of application

Inactive Publication Date: 2015-11-25
上海星可高纯溶剂有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a mobile phase solvent, the higher the purity, the better the separation effect of organic matter in the sample, and the high-purity solvent can avoid the phenomenon of insufficient ionization of the analyte caused by the existence of impurities, especially metal ions. In the mass spectrometry analysis, it complexes with the measured substance and produces interference peaks in the mass spectrometer, which leads to misjudgment of the determination of molecular weight and other parameters, and greatly reduces the accuracy of the liquid chromatography-mass spectrometry measurement results
[0004] As a solvent with excellent performance, acetonitrile can dissolve various organic, inorganic and gaseous substances, but its purification is very difficult
Because industrial acetonitrile is made from petrochemical products, the product con

Method used

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  • Purification method of acetonitrile for liquid chromatography-mass spectrometer

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Embodiment 1

[0022] The method for purifying acetonitrile for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0023] a. Take the raw material acetonitrile, add sulfuric acid to it for vibration, generate sulfate ester precipitates, and let it stand at -30°C, discard the water layer after layering, and filter the organic layer to remove sulfate ester precipitates , retain the filtrate. Then activated carbon was added to the filtrate and stirred for 1 hour. After the stirring is completed, potassium permanganate is added for oxidation treatment to remove impurities containing double bonds such as acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 8. After the oxidation treatment...

Embodiment 2

[0029] The method for purifying acetonitrile for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0030] a. Take the raw material acetonitrile, add sulfuric acid and nitric acid to it for oscillation, generate sulfate and nitrate precipitates, and let it stand at 20°C, discard the water layer after layering, and filter the organic layer, The sulfate ester precipitate was removed and the filtrate was retained. Immediately after, activated carbon was added to the filtrate and stirred for 2 hours. After the stirring is completed, potassium permanganate is added for oxidation treatment to remove impurities containing double bonds such as acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, an...

Embodiment 3

[0036] The method for purifying acetonitrile for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0037] a. Take the raw material acetonitrile, add sulfuric acid to it for vibration, generate sulfate ester precipitates, and let it stand at -10°C, discard the water layer after layering, and filter the organic layer to remove sulfate ester precipitates , retain the filtrate. Immediately after, activated carbon was added to the filtrate and stirred for 1.5 hours. After the stirring is completed, potassium permanganate is added for oxidation treatment to remove impurities containing double bonds such as acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 10. After the o...

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Abstract

The invention discloses a purification method of acetonitrile for a liquid chromatography-mass spectrometer. The method is characterized in that impurities in a raw material acetonitrile are removed through processes such as modified activated carbon adsorption and the like so as to obtain acetonitrile for a liquid chromatography-mass spectrometer. By the purification method of acetonitrile for a liquid chromatography-mass spectrometer, acetonitrile with its purity being greater than or equal to 99.99 wt% can be obtained, thus meeting the high-purity requirement of a liquid chromatography-mass spectrometer. The acetonitrile obtained after purification can be applied in the field of liquid chromatography-mass spectrometers, and the application range of acetonitrile is broadened.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying acetonitrile for liquid chromatography-mass spectrometry. Background technique [0002] The online coupling of chromatography-mass spectrometry combines the separation ability of chromatography with the qualitative function of mass spectrometry to achieve more accurate quantitative and qualitative analysis of complex mixtures. It also simplifies the pretreatment process of the sample and makes the sample analysis easier. Chromatography-mass spectrometry includes gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry. Liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry complement each other to analyze compounds of different properties. [0003] Liquid Chromatography Mass Spectrometer (LC-MS for short) is a high-end instrument in the organic analysis market. Liquid chromatography (LC) can effectively...

Claims

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Application Information

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IPC IPC(8): C07C255/03C07C253/34
Inventor 范文林张群星王洪魏丽
Owner 上海星可高纯溶剂有限公司
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