Process for determining hydrocarbon composition of vacuum gas oil by combination of solid phase extraction and mass spectrum

A technology of reduced pressure gas oil and family composition, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of long time, large sample volume, unsuitable for batch and rapid analysis of VGO samples, etc. The effect of shortening analysis time

Active Publication Date: 2005-11-02
CHINA PETROLEUM & CHEM CORP +1
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AI Technical Summary

Problems solved by technology

Although this method is accurate, it uses a large amount of samples, many steps in the separation process, a large amount of extraction solvent, slow separation speed, and a long time to determine the content of saturated hydrocarbons and aromatic hydrocarbons.
Therefore, it is not suitable for batch and rapid analysis of VGO samples

Method used

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  • Process for determining hydrocarbon composition of vacuum gas oil by combination of solid phase extraction and mass spectrum
  • Process for determining hydrocarbon composition of vacuum gas oil by combination of solid phase extraction and mass spectrum
  • Process for determining hydrocarbon composition of vacuum gas oil by combination of solid phase extraction and mass spectrum

Examples

Experimental program
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Effect test

example 1

[0043] The applicability of the internal standard method GC-FID of the present invention to determine the relative content of saturated hydrocarbons and aromatic hydrocarbons in VGO samples was investigated.

[0044] in such as figure 1 The shown SPE column with a height of 60 mm and an internal diameter of 7.0 mm is packed with 1.8 g of activated silica and has a specific surface area of ​​600 m 2 / g, the pores with a pore volume of 0.45 ml / g and a pore diameter of 290-330 nm accounted for 60% of the total pore volume.

[0045] According to the method of ASTM D2549, take 2 grams of VGO samples, separate the saturated hydrocarbons, aromatics and colloids, and prepare 4 samples with different contents of saturated hydrocarbons and aromatics after weighing each, and take 0.10 grams of prepared samples Dropped into the solid phase extraction column, the sample is completely absorbed by the stationary phase silica. Then add 2.5 milliliters of n-pentane to the solid-phase extract...

example 2

[0050] The VGO sample was analyzed according to the method of Example 1, except that the VGO sample was dropped into the solid-phase extraction column to extract saturated hydrocarbons, aromatic hydrocarbons and colloids therein. Dry the obtained saturated hydrocarbon and aromatic hydrocarbon extracts in a water bath at 50-60°C for 30 minutes, weigh them at room temperature, then dry them at this temperature for 10 minutes, and weigh them again. Repeat the drying and weighing steps until The solvent in the extract is completely volatilized, and the difference between the two weighing results is no more than 10 mg, which is regarded as a constant weight. Record the mass of saturated hydrocarbons and aromatic hydrocarbons obtained after weighing constant weight, then dry the colloidal solution obtained by extraction in a water bath at 80-90°C in the same way, weigh until the solvent is completely volatilized, and record the mass after weighing constant weight The resulting gum m...

example 3

[0053] The VGO sample was analyzed according to the method of Example 1, except that the VGO sample was dropped into the solid-phase extraction column to extract saturated hydrocarbons, aromatic hydrocarbons and colloids therein. Take 0.5 μL of the extracts of each component added with the internal standard, and pass it into the injection port of the GC-MS instrument, and send a part of the sample to the GC-FID detection system through the diverter valve for chromatographic analysis; the other part The sample is sent to the mass spectrometry detection system to determine the hydrocarbon group composition. Calculate the relative content of saturated hydrocarbons, aromatic hydrocarbons and colloids from the peak area of ​​the gas chromatogram, calculate the hydrocarbon group composition according to the method of ASTM D2425, and then calculate the saturated hydrocarbons and aromatic hydrocarbons in the total content of the two calculated by the GC-FID spectrum The relative conte...

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Abstract

A composition measurement method for hydrocarbon of vacuum gas oil by solid phase extraction combination mass spectrum comprises that separate the oil to three parts of saturated hydrocarbon, arene and gum by solid phase extraction, analyze their corresponding content by weighing or gas chromatography; detect makeup of saturated hydrocarbon and arene by mass spectrum; use normalization method to compute hydrocarbon composition of vacuum gas oil according to corresponding content of saturated hydrocarbon and arene; stationary phase of aforementioned solid phase extraction is silicon dioxide with specific surface is 450~750m2g, pore volume is 0.35~0.55ml / g, and pore with aperture 290~350nm takes up 50~70% of total pore volume. The method need less oil sample, and is quick and accurate.

Description

technical field [0001] The invention relates to a method for determining the hydrocarbon group composition of vacuum gas oil by mass spectrometry, specifically, a method for determining the hydrocarbon group composition of vacuum gas oil by using solid phase extraction and mass spectrometry. Background technique [0002] The hydrocarbon composition distribution of vacuum gas oil (VGO) directly affects the performance of catalytic cracking and lubricating base oil products, and is also an important basis for choosing a reasonable processing plan. Therefore, it is necessary to establish a fast and accurate analysis method for the hydrocarbon group composition of VGO samples. [0003] At present, the methods for analyzing the hydrocarbon composition of VGO mainly include classical liquid chromatography, high performance liquid chromatography, supercritical fluid chromatography, thin layer chromatography-flame ionization detection (TLC-FID) and ultraviolet spectroscopy. These me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 胡健刘泽龙田松柏
Owner CHINA PETROLEUM & CHEM CORP
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