Gas chromatography-mass spectrometry detection method for methylaniline compound

A technology of methylaniline and gas chromatography is applied in the field of gas chromatography-mass spectrometry detection of methylaniline compounds, which can solve the problems of high cost and achieve the effects of high accuracy, high extraction efficiency and easy operation

Inactive Publication Date: 2012-09-26
SHENZHEN ACAD OF METROLOGY & QUALITY INSPECTION
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Problems solved by technology

Some studies use different detectors for detection. Such methods ne

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  • Gas chromatography-mass spectrometry detection method for methylaniline compound
  • Gas chromatography-mass spectrometry detection method for methylaniline compound
  • Gas chromatography-mass spectrometry detection method for methylaniline compound

Examples

Experimental program
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Embodiment 1

[0023] Example 1 Extraction of samples.

[0024] Accurately measure 100mL gasoline sample, add 10mL 10% (v / v) hydrochloric acid solution to extract methylaniline compounds in gasoline according to the ratio of oil to volume ratio of 10:1, separate and obtain hydrochloric acid liquid phase extraction solution, add sodium hydroxide solution to the hydrochloric acid liquid-phase extraction solution to adjust the pH to neutral, add 40 mL of dichloromethane 2 times the volume of the neutral extraction solution to back-extract the methylaniline compounds, and set the volume to 100 mL. Obtain gasoline sample detection solution. It is also possible to measure 100mL crude oil sample or diesel oil sample, and follow the above operation to obtain crude oil sample detection solution or diesel oil sample detection solution respectively.

Embodiment 2

[0025] The detection of embodiment dimethyl aniline compound.

[0026] Gas chromatography conditions: inlet temperature 200 °C, injection volume 1 μL, split injection, split ratio 20:1; temperature program, initial temperature 60 °C for 40 min, 40 °C / min to 200 °C, keep 3 min, the carrier gas is helium, the carrier gas flow rate: 0.9 mL / min; mass spectrometry conditions: Perkinelmer Clarus600 quadrupole mass spectrometer, ionization mode EI, electron energy 70 eV, ion source temperature 200 ℃, solvent cut-off time 0 ~3.0 min, scan ion range m / z 40~m / z 200; scan rate 0.5 times / s, full scan mode (SCAN) qualitative, selected ion detection mode (SIM) external standard quantitative analysis.

[0027] Five kinds of methylaniline compounds (N-methylaniline, o-methylaniline, m-methylaniline, p-methylaniline and N,N-dimethylaniline) were mixed with dichloromethane to make 10mg / L, 20 mg / L, 50 mg / L, 100 mg / L, 200 mg / L, 500 mg / L serial concentrations of the standard mixed solution were...

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Abstract

The invention provides a gas chromatography-mass spectrometry detection method for a methylaniline compound. The method comprises the following steps of: A) extraction of a sample, namely adding an acid into the sample to extract the methylaniline compound into an acid liquor phase, adding alkaline into acid liquor phase extract to regulate pH to be neutral, adding methylene chloride to reextract the methylaniline compound in the neutral extract into the methylene chloride, and performing volume fixing to obtain a sample detection solution; and B) detection of the sample, namely separating the obtained sample detection solution by using a DB-1MS fused silica capillary column, and performing gas chromatography-mass spectrometry detection. The quantitative detection of the methylaniline compound is realized; the method is high in accuracy, low in detection limit, high in extraction efficiency and easy to operate, and can be widely applied to the detection of the methylaniline compound in a crude oil sample, a gasoline sample, a diesel sample and the like; the interference of other compounds in an extraction process can be eliminated; and powerful support can be provided for the environmental performance evaluation and monitoring of the sample.

Description

technical field [0001] The invention relates to a detection method for methylaniline compounds, in particular to a gas chromatography-mass spectrometry detection method for methylaniline compounds. Background technique [0002] At present, none of the relevant detection research provides a specific detection method for methylaniline additive compounds. The research mainly focuses on the synthesis of methylaniline compounds and the detection of similar compounds in air and diesel matrices. The detection methods include gas chromatography, liquid chromatography and gas chromatography-mass spectrometry (GC-MS). These detection methods have the disadvantages of high quantitative detection limit, long and complicated concentration and separation steps, narrow application range of equipment, and high test cost. The method of concentration, separation and analysis of nitrogen-containing compounds in petroleum products has been studied. The concentration and separation methods main...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 赵彦徐董育周永生黄开胜黄伟林李思源张世元陈晓燕陈丽琼
Owner SHENZHEN ACAD OF METROLOGY & QUALITY INSPECTION
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