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Purification method of n-hexane for liquid chromatography-mass spectrometry

A technology of liquid chromatography and purification method, which is applied in the field of purification of n-hexane for liquid chromatography-mass spectrometry, can solve the problems of high-purity n-hexane dependence on imports, complicated production process, low yield, etc. Cost required, simple production process, effect of expanding the scope of application

Active Publication Date: 2018-03-06
上海星可高纯溶剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If precision distillation and special distillation process are adopted, there are disadvantages such as high energy consumption, high production cost, low yield and complicated production process, which also leads to my country's dependence on imports of high-purity n-hexane
At present, there are few domestic reports about obtaining high-purity n-hexane through adsorption and purification. The patent application number 200910068762.4 discloses a method for purifying n-hexane by zeolite adsorption. The purified n-hexane has a purity of ≥98% (wt), which is still not To meet the high purity requirements of industrial use, the purification method needs to be further improved

Method used

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  • Purification method of n-hexane for liquid chromatography-mass spectrometry
  • Purification method of n-hexane for liquid chromatography-mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The method for purifying n-hexane for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0025] a. Take n-hexane as a raw material, add activated carbon, stir for 1 hour, add potassium permanganate to it for oxidation treatment, and remove unsaturated hydrocarbons in n-hexane as a raw material. 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 refluxing for 1 hour, n-hexane was quickly distilled off.

[0026] b. the above-mentioned n-hexane distilled out is passed into the adsorbent column that particle diameter is 50 order 3A molecular sieves with the speed of 0.5 column volume / hour, further removes the moisture in the organic layer; After adsorption, the n-hexane water content is controlled at ≤0.03%; in this step, molecular sieves are used to remove the moisture i...

Embodiment 2

[0033] The method for purifying n-hexane for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0034] a. Take n-hexane as a raw material, add zeolite, stir for 2 hours, add potassium permanganate to it for oxidation treatment, and remove unsaturated hydrocarbons in n-hexane as a raw material. 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 14. After refluxing for 3 hours, n-hexane was quickly distilled off.

[0035] B. the above-mentioned n-hexane distilled out is passed into the adsorbent column that particle diameter is 20 order 3A molecular sieves with the speed of 30 column volumes / hour, further removes the moisture in the organic layer; After adsorption, the n-hexane water content is controlled at ≤0.03%; in this step, molecular sieves are used to remove the moisture in the ...

Embodiment 3

[0042] The method for purifying n-hexane for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0043] a. Take n-hexane as a raw material, add molecular sieves, stir for 1.5 hours, add potassium permanganate to it for oxidation treatment, and remove unsaturated hydrocarbons in n-hexane as a raw material. 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 refluxing for 0.5 hour, n-hexane was quickly distilled off.

[0044] b. Pass the n-hexane distilled above into an adsorbent column with a particle size of 100 mesh molecular sieves at a rate of 15 column volumes / hour to further remove moisture in the organic layer; after adsorption, the water content of n-hexane is controlled at ≤ 0.03%; in this step, molecular sieves are used to remove the moisture in the extracted n-hexan...

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Abstract

The invention discloses a method for purifying n-hexane used in liquid chromatography-mass spectrometry, which is characterized in that impurities in the raw material n-hexane are removed through processes such as modified activated carbon adsorption to obtain liquid chromatography-mass spectrometry Use n-hexane. The method for purifying n-hexane used in liquid chromatography-mass spectrometry provided by the invention can obtain n-hexane with a purity ≥ 99.99% (wt), which meets the high-purity requirements of liquid chromatography-mass spectrometry and makes the purified n-Hexane can be applied to the field of liquid chromatography-mass spectrometry, expanding the scope of application.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying n-hexane used in 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 Chromatograph 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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Patent Type & Authority Patents(China)
IPC IPC(8): C07C9/15C07C7/00C07C7/12C07C7/148C07C7/13
Inventor 范文林张群星张怡陈建辉
Owner 上海星可高纯溶剂有限公司
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