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Method for solid-phase extraction of nitrogen-containing compounds in diesel oil

A nitrogen compound, solid-phase extraction column technology, applied in instruments, measuring devices, scientific instruments, etc., can solve the problems of long processing time and large solvent consumption, and achieve the effect of improving work efficiency

Active Publication Date: 2018-11-16
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention can solve the problems of long processing time and large amount of solvent used in the separation and enrichment of nitrogen-containing compounds in diesel oil by column chromatography

Method used

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  • Method for solid-phase extraction of nitrogen-containing compounds in diesel oil
  • Method for solid-phase extraction of nitrogen-containing compounds in diesel oil
  • Method for solid-phase extraction of nitrogen-containing compounds in diesel oil

Examples

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preparation example Construction

[0049]The invention provides a method for preparing a solid-phase extraction column for separating nitrogen-containing compounds in diesel oil. The stationary phase of the solid phase extraction column used in the present invention is a mixture of silica gel, aluminum oxide and basic compound, wherein the content of aluminum oxide is 5-40wt%, and the content of basic compound is 1-15wt%. Silica gel and alumina need to undergo activation treatment at a certain temperature and time, mix well and set aside. The basic compound solid can be mixed evenly with silica gel and alumina and then loaded into the solid phase extraction column, or it can be packed on the top of the mixture of silica gel and alumina. Preferably, the basic compound solid is loaded on top of the mixture of silica gel and alumina. The solid-phase extraction column described in this patent can effectively separate and enrich different types of nitrogen-containing compounds in diesel samples while reducing the a...

Embodiment 1

[0059] 4 g of silica gel-alumina-potassium hydroxide stationary phase with an alumina content of 40 wt % and a potassium hydroxide content of 15 wt % were filled in the solid-phase extraction column, and were wetted with 2 mL of the first eluent (n-pentane). The activation temperature of silica gel is 80°C, and the activation time is 6 hours; the activation temperature of alumina is 550°C, and the activation time is 3 hours.

[0060] Use a pipette gun to take 6mL of Qingyang Petrochemical FCC diesel oil into a 25mL test tube, add 0.7g of potassium hydroxide solid, shake for 1min and then let it stand for 30min.

[0061] Use a pipette gun to take 2 mL of the above-mentioned treated diesel sample, add it to the upper part of the wetted solid phase extraction column and be completely absorbed by the stationary phase. The SPE cartridge was flushed with 6 mL of the first eluent (n-pentane) to obtain saturated hydrocarbons (component 1). Rinse the solid-phase extraction column with...

Embodiment 2

[0077] 4 g of silica gel-alumina-sodium hydroxide stationary phase with an alumina content of 30 wt % and a sodium hydroxide content of 10 wt % were filled in the solid phase extraction column, and were wetted with 2 mL of the first eluent (n-hexane). The activation temperature of silica gel is 100°C, and the activation time is 5 hours; the activation temperature of alumina is 500°C, and the activation time is 4 hours.

[0078] Take 6mL of Karamay Petrochemical Coked Diesel Oil into a 25mL test tube with a pipette gun, add 6mL of potassium hydroxide solution with a mass concentration of 30wt%, shake for 1min and then let stand for 20min.

[0079] Take 1mL of the above-mentioned treated diesel sample with a pipette gun, add it to the upper part of the wetted solid phase extraction column and be completely absorbed by the stationary phase. Rinse the solid-phase extraction column with 5 mL of the first eluent (n-hexane) to obtain saturated hydrocarbons (component 1). Rinse the S...

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Abstract

A method for solid phase extraction of nitrogen-containing compounds from diesel oil comprises the following steps: 1, adding an alkali metal compound or an alkali earth metal compound or an alkali metal compound solution or an alkali earth metal compound solution into a diesel oil sample, and uniformly mixing to obtain a preprocessed diesel oil sample; 2, producing a solid phase extraction column, wherein the stationary phase of the solid phase extraction column is a silica gel, alumina and alkaline compound mixture; and 3, eluting: wetting the solid phase extraction column by a first eluent, adding the preprocessed diesel oil sample from the upper portion of the solid phase extraction column, flushing the solid phase extraction column with the first eluent to obtain saturated hydrocarbons, flushing the solid phase extraction column with a second eluent to obtain aromatic hydrocarbons, flushing the solid phase extraction column with a third eluent to obtain neutral nitrogen-containing compounds, and flushing the solid phase extraction column with a fourth eluent to obtain alkaline nitrogen-containing compounds.

Description

technical field [0001] The invention relates to the field of petrochemical industry, in particular to a method for separating and enriching neutral nitrogen-containing compounds and basic nitrogen-containing compounds in a diesel sample by using a single-column solid-phase extraction method. Background technique [0002] The nitrogen-containing compounds in diesel can be divided into neutral nitrogen-containing compounds and basic nitrogen-containing compounds. Due to the low content of nitrogen-containing compounds in diesel oil, when conducting qualitative or quantitative research on nitrogen-containing compounds, it is often necessary to enrich the nitrogen-containing compounds in diesel oil first, and then perform qualitative or quantitative analysis on the enriched substances. [0003] Commonly used methods for separating and enriching nitrogen-containing compounds include acid extraction, ion exchange chromatography, and column chromatography, among which column chroma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08
Inventor 史得军肖占敏薛慧峰王春燕曹青霍明辰徐华许蔷梁迎春汪艳
Owner PETROCHINA CO LTD
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