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Detection method of nitrogen-containing compound from rock extract

A nitrogen compound and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inaccurate qualitative and quantitative results, large differences, limited qualitative and quantitative nitrogen compounds, etc., and achieve accurate and reliable qualitative and quantitative results Effect

Inactive Publication Date: 2014-11-26
CHINA UNIV OF GEOSCIENCES (WUHAN)
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Problems solved by technology

However, when analyzing actual samples, due to the great difference in geological conditions, the content of carbazole compounds in many samples is extremely low, and the interference of aromatic hydrocarbon compounds and other polar components is unavoidable, resulting in inaccurate qualitative and quantitative results
At present, the qualitative number of nitrogen-containing compounds is very limited, only carbazole, methylcarbazole, dimethylcarbazole and benzocarbazole have been qualified, and the detection of other nitrogen-containing compounds needs to be further studied

Method used

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  • Detection method of nitrogen-containing compound from rock extract
  • Detection method of nitrogen-containing compound from rock extract
  • Detection method of nitrogen-containing compound from rock extract

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Embodiment

[0032] A method for detecting nitrogenous compounds in rock extracts, comprising the steps of:

[0033](1) Pretreatment: Knock the rock sample into small pieces, select the clean pieces on the surface and enter the crushing machine for fine crushing, pass through a 100-mesh sieve, and mix evenly; take the 200g rock sample after sieving, and place it in a Soxhlet pump Extraction in the extractor for 48 hours, Soxhlet extraction using 300ml of binary mixed reagent of chloroform and methanol with a volume ratio of 98:2, then the resulting extract was concentrated to 3mL on a rotary evaporator, and evaporated to dryness at 40°C. Store in a desiccator for later use;

[0034] (2) Separation of group components: dissolve the rock extract with 0.5ml chloroform, then add 10ml n-hexane, and let stand overnight. Fill the chromatographic column with neutral alumina and hydrated silicic acid respectively, and keep the column wet. After adding the asphaltene-removed sample, use 40ml of n-h...

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Abstract

The invention relates to a detection method of a nitrogen-containing compound from a rock extract. The detection method comprises the following steps of (1) pre-treating a rock sample to obtain the rock extract; (2) carrying out family component separation on the rock extract, separating and collecting of nitrogen-containing compound fraction, and concentrating the nitrogen-containing compound fraction to use as a to-be-detected sample; (3) preparing a carbazole standard solution and 9-phenyl-carbazole standard solution, measuring a mass chromatogram by using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry to obtain standard curves of the both; and (4) detecting the to-be-detected sample by using the comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry, qualitatively analyzing the nitrogen-containing compound in the to-be-detected sample according to a retention time and characteristic ions, and quantitatively analyzing the nitrogen-containing compound in the to-be-detected sample. The comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry analysis method of the nitrogen-containing compound in the rock extract overcomes the interference problems of overlapping peaks in conventional GC / MS chromatogram; and the qualitative and quantitative results are accurate and reliable.

Description

technical field [0001] The invention belongs to the field of chemical composition analysis and research of petroleum samples, and relates to a detection method for nitrogen-containing compounds in rock extracts. Background technique [0002] In the process of oil and gas exploration, the high-sensitivity detection of nitrogen-containing compounds has important guiding significance. Especially carbazole nitrogen-containing compounds (including carbazole, methylcarbazole series, dimethylcarbazole series, trimethylcarbazole series and other compounds), because of their special molecular structure, they have significant oil and gas migration fractionation effect, which can be used as an important tracer indicator of oil and gas migration. In recent years, the application of nitrogen-containing compounds to study the primary and secondary migration of petroleum has become a hot topic at home and abroad. [0003] However, due to the extremely low content of nitrogen-containing c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 朱书奎代威高儇博童婷张万峰常振阳何生
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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