Determination of c in gasoline or micro-reaction products by gas chromatography 6 The following methods for oxygenated compounds

A technology of micro-reaction products and gas chromatography, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex composition of gasoline, difficulty in separating oxygen-containing compounds from hydrocarbon components, and low content

Active Publication Date: 2016-11-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Due to the complex composition of gasoline, the content of oxygenated compounds that may be contained in it is very low, as low as several μg / g, it is difficult to separate trace oxygenated compounds from hydrocarbon components by conventional chromatographic analysis methods
At present, for the determination of methanol and other oxygenated compounds in gasoline, the double-column method of SH / T0663 or the gas chromatography / oxygen selective detector method of SH / T0720 are mostly used. The lower limit of the determination of the mass fraction of a single component is about 0.1%. Cannot meet the requirements of microanalysis

Method used

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  • Determination of c in gasoline or micro-reaction products by gas chromatography <sub>6</sub> The following methods for oxygenated compounds
  • Determination of c in gasoline or micro-reaction products by gas chromatography <sub>6</sub> The following methods for oxygenated compounds
  • Determination of c in gasoline or micro-reaction products by gas chromatography <sub>6</sub> The following methods for oxygenated compounds

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0050] The retention time of each oxygen-containing compound is determined according to the method of the present invention.

[0051] Using the Agilent 7890 gas chromatograph from Agilent, press figure 1 Connect the chromatographic column as shown, set the inlet temperature to 250°C, the inlet pressure to 72.26kPa in the steady pressure mode, the split ratio to 10:1, and the injection volume to be 1μL; nitrogen is used as the carrier gas, and flow1 and flow2 are controlled. The two pressures are 68.95kPa and 29.51kPa respectively; the initial temperature of the chromatographic column used is 100°C, keep it for 5 minutes, the heating rate is 5°C / min, and the final temperature is 210°C, keep it for 8 minutes; the solenoid valve 16 is set to ON state; The detector adopts double FID, the temperature is 280°C, the flow rate of hydrogen is 30mL / min, the flow rate of air is 350mL / min, and the flow rate of nitrogen (compensation gas) is 25mL / min. Precut column 1 is HP-5 (2m×0.32mm×0....

example 2

[0056] Prepare standard samples with a mass fraction of 2.0 μg / g for each component, analyze and measure under the same conditions as in Example 1, gradually dilute the standard sample concentration with n-heptane, and inject samples to determine the detection limit of each component. When the signal-to-noise ratio is 3, the determined detection limits of each component are shown in Table 2.

[0057] As can be seen from Table 2, due to C 1 ~C 3 Alcohol has a strong polarity and has a certain adsorption effect. Its detection limit is relatively high, ranging from 1.0 μg / g to 2.0 μg / g. The detection limits of acetaldehyde and propionaldehyde are 2.0 μg / g and 1.0 μg / g, respectively. The detection limit of oxygen-containing compound components is 0.5 μg / g.

[0058] Table 1

[0059]

[0060] Table 2

[0061]

example 3

[0063] The Agilent7890 gas chromatograph of Agilent Company was used, equipped with an autosampler, a heart-cutting assembly, a backflushing assembly, and a double FID detector. according to figure 1 Connect the column as shown. Chromatographic columns include: pre-cut column 1, HP-5 (2m×0.32mm×0.25μm), non-polar chromatographic column 2, DB-1 (30m×0.32mm×1.0μm), strong polar chromatographic column 4 , is OxyPLOT (10m×0.53mm×40μm), and the damping column is an elastic quartz column tube. The chromatographic conditions are: inlet temperature 250°C, inlet pressure 72.26kPa in steady pressure mode, split ratio 10:1, injection volume 1μL; nitrogen as carrier gas, hold for 0.7min, at a rate of 700kPa / min Decrease to 56kPa and keep it until the end of the analysis; the pressures of flow1 and flow2 carrier gases are 68.95kPa and 29.51kPa respectively, the initial temperature of the chromatographic column used is 100°C, keep for 5min, the heating rate is 5°C / min, and the final tempe...

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Abstract

The invention discloses a method for determining oxygenated compound of C6 in gasoline or a micro-reaction product by gas chromatography. The method comprises the following steps: introducing a determined sample to a sampling opening of a gas chromatography and enabling the determined sample to enter a nonpolar chromatographic column after the determined sample enters a pretruncating column, back-flushing heavy components with boiling point greater than that of n-undecane out of the gas chromatography by changing the pressure program of the chromatographic column after the components with boiling point being not greater than that of the n-undecane flow out from the pretruncating column, regulating the connection position of an electromagnetic valve, detecting through a flame ionization detector after the components separated from the nonpolar chromatographic column enter the strongly polar chromatographic column, changing the position of the electromagnetic valve after 2-hexanone flows out from the nonpolar chromatographic column and enters the strongly polar chromatographic column, so as to enable the carrier gas flowing by the nonpolar chromatographic column to flow to a damping column and the components with boiling point higher than that of 2-hexanone to directly enter another flame ionization detector for detection. According to the method, the lower detection limit of the oxygenated compounds can be reduced.

Description

technical field [0001] The present invention is a method for measuring the content of oxygen-containing compounds in hydrocarbon mixtures by gas chromatography, specifically, a method for measuring the content of C in gasoline or micro-reaction products by gas chromatography. 6 The oxygenate method below. Background technique [0002] Trace oxygenates in gasoline fractions are a very important non-hydrocarbon impurity contained in gasoline, and their content will have an important impact on process research and product quality, especially in the process research of catalytic cracking to produce more propylene. The demand for the determination of oxygenates in products is more urgent. As a basic chemical raw material, the demand for propylene continues to rise. It is difficult to meet the market demand only by the traditional steam cracking process. The process of catalytic cracking to produce more propylene is a new way to produce propylene. Since the raw materials of the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 李长秀
Owner CHINA PETROLEUM & CHEM CORP
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