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Method for qualitatively and quantitatively analyzing hydrocarbon components in aromatics extraction solvent sulfolane

An aromatic hydrocarbon extraction and hydrocarbon component technology, which is applied in the field of analytical chemistry, can solve the problems of inability to guide production in time, unable to measure the content of aromatic hydrocarbons, and the operation is not simple enough, and achieves the effects of shortening time consumption, simple operation and good accuracy.

Active Publication Date: 2014-01-22
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method overcomes the shortcoming that the direct distillation method is easy to cause environmental pollution, the sensitivity is also improved; but the detection limit is only 100 μg / g, and the lower content of C cannot be detected. 9 Aromatics
Moreover, the instrument analysis time of a sample is as long as 40 minutes, which cannot guide the production in time and meet the actual needs
In addition, when this method is used to determine the sample content, it is necessary to first dissolve the homogeneously mixed sulfolane and the internal standard - n-heptane in CS 2 In the solution, use an ultrasonic oscillator to vibrate for 10 minutes, and the sample can only be injected after mixing evenly. The operation is not easy enough

Method used

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  • Method for qualitatively and quantitatively analyzing hydrocarbon components in aromatics extraction solvent sulfolane
  • Method for qualitatively and quantitatively analyzing hydrocarbon components in aromatics extraction solvent sulfolane
  • Method for qualitatively and quantitatively analyzing hydrocarbon components in aromatics extraction solvent sulfolane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 Qualitative analysis of the hydrocarbon components in the aromatics extraction solvent sulfolane by GC / MS

[0042] The chromatographic conditions are:

[0043] Chromatographic column: non-polar capillary column, 30m×0.25mm,

[0044] Carrier gas: high purity helium,

[0045] Head pressure: 90-100kPa,

[0046] Injection port temperature: 220-250°C,

[0047] Column temperature: the initial temperature is 35°C, the temperature is raised to 50-60°C at 2-4°C / min, and then the temperature is raised to 200-250°C at 35-40°C / min, and kept for 2-5min.

[0048] Injection volume: 0.2-1μL.

[0049] Mass Spectrometry Conditions:

[0050] Interface temperature: 230-250°C,

[0051] Ionization method: electron ionization (EI),

[0052] Electron energy: 70eV,

[0053] Detector voltage: 1.5-1.8kV.

[0054] Direct sample analysis on GC / MS instrument, figure 1 It is a typical sulfolane solvent SCAN analysis total ion chromatogram, according to No. 1 peak, No. 2 peak, No. ...

Embodiment 2

[0055] The mensuration of each hydrocarbon component relative volume correction factor in embodiment 2 sulfolane

[0056] Chromatographic conditions and mass spectrometry conditions are the same as in Example 1.

[0057]In a 10mL volumetric flask, add 4 μL each of toluene, n-octane, ethylbenzene, o-xylene, cumene, n-propylbenzene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene, m- 2 μL each of xylene and p-xylene, dilute to 10 mL with analytical grade acetone, and prepare a standard solution, including toluene, n-octane, ethylbenzene, o-xylene, cumene, n-propylbenzene, 1, 3, 5 - The concentrations of trimethylbenzene and 1,2,4-trimethylbenzene are 400 μL / L, and the concentrations of m-xylene and p-xylene are 200 μL / L. The standard solution was directly injected on the GC / MS instrument and repeated 6 times. The SCAN analysis total ion chromatogram of this standard solution is shown in figure 2 . Among them, peak No. 1 is toluene, peak No. 2 is n-octane, peak No. 3 is ethyl...

Embodiment 3

[0064] Example 3 investigates the precision and accuracy of the inventive method to measure the content of each hydrocarbon component in the aromatics extraction solvent sulfolane

[0065] Chromatographic conditions and mass spectrometry conditions are the same as in Example 1.

[0066] Preparation of mother liquor: In a 10mL volumetric flask, add 10μL each of toluene, ethylbenzene, o-xylene, cumene, n-propylbenzene, 1,3,5-trimethylbenzene, and 1,2,4-trimethylbenzene, Then add 5 μL each of m-xylene and p-xylene, and dilute to 10 mL with acetone. The volume concentration of toluene, ethylbenzene, o-xylene, isopropylbenzene, n-propylbenzene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene is 1000 μL / L, m-xylene, p-xylene The volume concentration was 500 μL / L.

[0067] Preparation of samples with low hydrocarbon concentration: Add 0.5mL of mother liquor to a 10mL volumetric flask, and dilute to 10mL with sulfolane solvent from the No. 2 joint production site of Jiujiang Branch C...

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Abstract

The invention discloses a method for qualitatively and quantitatively analyzing hydrocarbon components in aromatics extraction solvent sulfolane by adopting the gas chromatography / mass spectrometry coupling technology. In the method, the qualitative method is as follows: adopting the scanning mode to analyze the hydrocarbon components in the sample and determining the structures of the hydrocarbon components in accordance with the obtained mass spectrogram, in combination with the standard mass spectral library search and in contrast to the retention time of the guide samples of the hydrocarbon components; and the quantitative method is as follows: adopting the scanning mode, taking normal heptane or normal octane as an internal standard substance and obtaining the contents of the hydrocarbon components according to the relative volume correction factors and peak areas of the hydrocarbon components and the peak area of the internal standard substance. The method has the beneficial effects of high accuracy, low limit of detection, no interference with quantitative analysis, short analysis time, no need for pretreatment of the sample to be detected and simpleness and convenience in operation.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a qualitative and quantitative analysis method for hydrocarbon components in sulfolane, an aromatic hydrocarbon extraction solvent. Background technique [0002] Sulfolane solvent has high solubility to aromatic hydrocarbons, good selectivity, high thermal stability, and no corrosion to equipment. Therefore, the aromatics extraction device in petrochemical enterprises uses sulfolane as a solvent, and the aromatic-rich sulfolane solvent passes through the distillation tower, and the sulfolane is separated from the aromatic components, thereby recovering high-purity benzene, toluene, xylene and C 9 For the above aromatics, the obtained sulfolane solvent is recycled. The impurity content in sulfolane directly affects the extraction effect of sulfolane solvent, and is an important control index for aromatics extraction equipment. Therefore, it is necessary to analyze the hydrocar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72
Inventor 赵惠菊刘明清王忠罗光汪昌华万义芳贾咏梅
Owner CHINA PETROLEUM & CHEM CORP
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