A method for detecting nitrogen and sulfur compounds in tar by comprehensive two-dimensional gas chromatography-mass spectrometry
A gas chromatography spectrometer and sulfur compound technology, applied in the field of tar analysis, can solve the problems of complex structure, large number of isomers, low peak intensity, etc.
Active Publication Date: 2022-02-08
TAIYUAN UNIV OF TECH
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Problems solved by technology
However, GC×GC has strong resolving power, and due to the comprehensive two-dimensional modulation function, its detection limit is greatly reduced. Therefore, the use of comprehensive two-dimensional analysis will generate a large amount of mass spectrometry data, which is about 25 times that of traditional one-dimensional GC. , it will be a heavy task to manually perform one-to-one matching analysis of mass spectral library for each chromatographic peak in complex samples
In addition, the structure of N and S heteroatom compounds in tar is complex, the number of isomers is large and the content is low, resulting in scattered distribution of N and S heteroatom compounds in the comprehensive two-dimensional spectrum, and low peak intensity , not easy to find
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Embodiment 1
[0050] 1 Instruments and samples
[0051] The GC×GC-MS system is composed of 7890B-5977A GC-MS of Agilent Company of the United States, equipped with a ZX10542 thermal modulator of ZOEX Company of the United States. Chromatographic column system: the first dimension column is DB-1 (15m×0.25mm×0.25μm), and the second dimension column is BPX-50 (2.75m×0.1mm×0.1μm). Dichloromethane, anhydrous sodium sulfate (analytical grade, Aladdin Reagent (Shanghai) Co., Ltd.). The tar samples are the tars produced by two different Yunnan lignites in fixed bed low temperature pyrolysis (600°C), and the numbers are A and B respectively.
[0052] 2 Experimental conditions
[0053] Injection conditions: Weigh 1g of tar sample and dissolve it in 25mLCH 2 Cl 2 In the solution, add 5g of anhydrous sodium sulfate, stir, to remove the moisture contained in the tar. Filter the solution through a filter cloth of 200 mesh (0.075 mm), and use CH 2 Cl 2 Wash the filter residue several times. The fi...
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The invention provides a method for detecting nitrogen and sulfur compounds in tar by using a comprehensive two-dimensional mass spectrometer, belonging to the field of tar analysis. The invention realizes rapid detection of nitrogen and sulfur compounds in tar by pre-editing computer language. N-containing compounds in tar mainly include pyridine, quinoline, indole, carbazole, benzoquinoline, benzocarbazole and alkyl substitutes of various types of compounds; S-containing compounds mainly include thiophene, benzothiophene, di Benzothiophene and alkyl substituents of various types of compounds, because the isomers of the same type of compounds have the same or similar mass spectrum data, by analogy, based on the mass spectrum data of different N and S-containing compounds, pre-edited Computer language, describe its mass spectrum characteristics, and then use this language to find out the preset N and S-containing compounds in the comprehensive two-dimensional chromatogram. Moreover, this language can be continuously supplemented and improved to achieve a more complete identification and analysis of N and S compounds in tar oil.
Description
technical field [0001] The invention relates to the technical field of tar analysis, in particular to a method for detecting nitrogen and sulfur compounds in tar by using a comprehensive two-dimensional mass spectrometer. Background technique [0002] Coal tar is a liquid product obtained in the process of carbonization and gasification of coal. According to the difference in carbonization temperature, coal tar can be roughly divided into: low-temperature coal tar (450-550°C), medium-temperature coal tar (600-800°C) and high-temperature coal tar Tar (1000°C). There are as many as tens of thousands of species in coal tar, and the compounds that have been characterized are mainly aromatic hydrocarbon compounds with 1-8 rings and a small amount of polycyclic compounds containing nitrogen, sulfur, and oxygen heteroatoms. [0003] Although the content of N and S heteroatom compounds in coal tar is relatively low (1.5-2wt%), their existence has a great impact on the properties an...
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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 黄伟刘建伟张乾梁丽彤
Owner TAIYUAN UNIV OF TECH