Method for detecting the structure and/or content of polar substances in non-polar matrices

A polar substance, non-polar technology, applied in the field of detection, can solve the problems of hydrocarbon interference and lack of availability, and achieve the effects of simple operation, good repeatability and short analysis time

Active Publication Date: 2022-03-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if SPME is directly used to extract sulfur compounds in gasoline, accurate results will not be obtained due to hydrocarbon interference. Currently, SPME is only used to analyze volatile organic compounds in aqueous solutions and solid samples.

Method used

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  • Method for detecting the structure and/or content of polar substances in non-polar matrices
  • Method for detecting the structure and/or content of polar substances in non-polar matrices
  • Method for detecting the structure and/or content of polar substances in non-polar matrices

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0042] Determination of standard curves for three sulfur-containing compounds in gasoline (there are three types of sulfur-containing compounds in gasoline, namely mercaptans, sulfides and thiophenes).

[0043] Accurately weigh 7.6mg of isopropyl mercaptan, 7.6mg of methyl ethyl sulfide, and 8.4mg of thiophene in a 500mL volumetric flask, add petroleum ether solution (90°C-120°C) and set the volume to 500mL to make the petroleum ether solution The concentration of sulfur in the above three compounds is 6.4mg / L.

[0044] Use 2ml of N-methylpyrrolidone to extract 5ml of the above three samples respectively, and then perform headspace extraction on the obtained polar extracts respectively. The extraction probe is a 100 μm PDMS probe, and the volume of the headspace bottle is 20mL. The volume is 2 mL, the headspace extraction time is 20 min, and the extraction temperature is 40°C. The extraction probes after headspace extraction were desorbed at the inlet of gas chromatography-su...

example 2

[0048] This example illustrates a repeatability experiment of the method.

[0049] N-methylpyrrolidone (2mL) was used for liquid-liquid extraction of sulfur-containing compounds in gasoline samples (5mL), and then the volatile sulfur-containing compounds in N-methylpyrrolidone polar extracts were enriched through the headspace of a 100 μm PDMS probe. The extraction probe is a 100 μm PDMS probe, the volume of the headspace bottle is 20 mL, the volume of the extraction solution is 2 mL, the headspace extraction time is 20 min, and the extraction temperature is 40 °C. The injection port is used for desorption, the desorption time is 1min, the desorption temperature is 280°C, and the desorbed product enters the GC-SCD analysis system for analysis.

[0050] The experimental conditions are: the chromatographic separation column is a PONA column (50m×0.2mm×0.5μm, Agilent Company). It is preferable to control the inlet temperature of the chromatograph at 280°C, the pressure of the in...

example 3

[0056] An Agilent 7890 gas chromatograph equipped with an autosampler and a sulfur chemiluminescence detector was used. The conditions of GC-SCD are as follows: the separation column is a PONA column (50m×0.2mm×0.5μm, Agilent Company). Column temperature: the initial temperature is 35°C, raised to 170°C at a rate of 2°C / min, and kept for 10 minutes. The carrier gas was high-purity nitrogen (purity 99.999%), and the sample was injected in constant flow mode with a flow rate of 0.6 mL / min. The injection volume was 1.0 μL, and the split ratio was 50:1. SCD condition: the temperature of the burner is 800°C. Hydrogen and air are purified with a sulfur purifier. The flow rate of hydrogen was 40 mL / min, and the flow rate of air was 55 mL / min. The pressure of the detector is 0.8kPa. The data acquisition rate is 20Hz.

[0057] Weigh 0.9885g of a finished gasoline sample in a chromatographic vial with a cover to make a test sample. After the condition of the instrument is stable,...

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Abstract

The present invention proposes a method for detecting the structure and / or content of polar substances in nonpolar substrates. The method for detecting the structure and / or content of polar substances in non-polar substrates of the present invention includes: 1) using a polar solvent to extract the non-polar substrates; 2) extracting the polar extracts obtained through step 1) Carry out the headspace extraction operation to obtain the carrier containing the enrichment; 3) send the carrier containing the enrichment obtained through step 2) into the analytical tester, and determine the structure and / or structure of the polar substance in the non-polar matrix to be tested or content. The method of the invention can overcome the interference of a large number of non-polar substances in complex non-polar matrices, can enrich trace polar compounds in complex non-polar matrices with high selectivity, and is especially suitable for separation, enrichment, and detection of gas Trace amounts of polar substances such as sulfides and nitrides in the complex matrix of diesel oil.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for detecting the structure and / or content of polar substances from non-polar substrates. Background technique [0002] With the increasingly stringent requirements of environmental protection departments for trace pollutants in non-polar matrices such as gasoline and diesel, it is urgent to establish a simple and sensitive analysis method to analyze the distribution and content of various trace pollutants in fuel oil fractions. . [0003] However, when the content of polar impurities in complex non-polar matrix samples such as gasoline and diesel is very low, due to the limitation of detector sensitivity, direct chromatographic analysis of the original sample often fails to detect the polar compounds contained therein. At present, it is still a difficult problem to analyze trace polar impurities (especially when the content is less than 10mg / Kg) in complex non-polar matrices such ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 钱钦王征李长秀
Owner CHINA PETROLEUM & CHEM CORP
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