CN108020523A - The Fourier infrared spectrum analytical method of quick test crude maturity - Google Patents

The Fourier infrared spectrum analytical method of quick test crude maturity Download PDF

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Publication number
CN108020523A
CN108020523A CN201610942622.5A CN201610942622A CN108020523A CN 108020523 A CN108020523 A CN 108020523A CN 201610942622 A CN201610942622 A CN 201610942622A CN 108020523 A CN108020523 A CN 108020523A
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CN
China
Prior art keywords
maturity
infrared spectrum
analytical method
crude oil
fourier infrared
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201610942622.5A
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Chinese (zh)
Inventor
林晶
黎萍
刘会平
李钜源
刘庆
张学军
徐大庆
韩冬梅
刘军
鲍燕
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China Petroleum and Chemical Corp
Exploration and Development Research Institute of Sinopec Henan Oilfield Branch Co
Exploration and Development Research Institute of Sinopec Shengli Oilfield Co
Original Assignee
China Petroleum and Chemical Corp
Exploration and Development Research Institute of Sinopec Henan Oilfield Branch Co
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Publication date
Application filed by China Petroleum and Chemical Corp, Exploration and Development Research Institute of Sinopec Henan Oilfield Branch Co filed Critical China Petroleum and Chemical Corp
Priority to CN201610942622.5A priority Critical patent/CN108020523A/en
Publication of CN108020523A publication Critical patent/CN108020523A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The present invention provides a kind of Fourier infrared spectrum analytical method of quick test crude maturity, which includes:Step 1, crude oil is uniformly applied on thin slice, film-making is spare;Step 2, under freezing, light transmission mode, each experiment parameter is adjusted;Step 3, back end scanning is carried out with thin slice to experiment, and preserves background result;Step 4, face is carried out to crude oil selection area to sweep to obtain spectrogram;Step 5, spectrum analysis are carried out, calculate maturity indices CH2a/CH3a.The Fourier infrared spectrum analytical method of the quick test crude maturity quickly can carry out IR spectrum scanning to crude oil, avoid the oil component caused by long-time operation and change, improve maturity indices CH2a/CH3aAccuracy.

Description

The Fourier infrared spectrum analytical method of quick test crude maturity
Technical field
The present invention relates to oil field geologic Exploration Domain, especially relates to a kind of Fourier of quick test crude maturity Infrared spectrum analysis.
Background technology
Infrared spectrum is mainly the structure and chemical bond for studying molecule.Some groups or chemical bond in molecule are not assimilating Corresponding bands of a spectrum wave number is substantially fixed or only changes in small band in compound, therefore many organo-functional groups are such as: Methyl, methylene, carbonyl, hydroxyl, amido etc. have characteristic absorption in infrared spectrum.We are tested using infrared spectrometer Crude maturity is mainly to obtain methyl in spectrogram, methylene peak, utilizes methyl, methylene peak area ratio characterization crude oil The parameter of maturity, realizes and sentences knowledge to crude maturity.
Traditional crude oil examination of infrared spectrum method needs to carry out crude oil dehydration shakeout, it is necessary to be carried out with chloroform to sample Dissolving, takes longer;In sample analysis by the way of point is swept, the error of data is larger.Crude oil open-assembly time in atmosphere Longer, light component just has different degrees of change in crude oil, and we have invented a kind of quick test crude maturity for this Fourier infrared spectrum analytical method, solves above technical problem.
The content of the invention
The object of the present invention is to provide one kind can quickly test crude oil, improve crude maturity parameter CH2a/CH3a's The Fourier infrared spectrum analytical method of the quick test crude maturity of accuracy.
The purpose of the present invention can be achieved by the following technical measures:The fourier infrared light of quick test crude maturity Spectral analysis method, the Fourier infrared spectrum analytical method for quickly testing crude maturity include:Step 1, it is crude oil is uniform It is applied on thin slice, film-making is spare;Step 2, under freezing, light transmission mode, each experiment parameter is adjusted;Step 3, to testing with thin Piece carries out back end scanning, and preserves background result;Step 4, face is carried out to crude oil selection area to sweep to obtain spectrogram;Step 5, carry out Spectrum analysis, calculate maturity indices CH2a/CH3a
The purpose of the present invention can be also achieved by the following technical measures:
The Fourier infrared spectrum analytical method of the quick test crude maturity further includes, before step 1, by sample preparation The thin slice used, glass bar these articles for use are soaked with chloroform, cleaned, are dried for standby;Fourier micro ft-ir spectroscopy instrument is opened, and Liquid nitrogen is added in instrument, instrument stabilizer 15 minutes, then keeps holding state.
In step 1, film-making is carried out to crude oil, is uniformly applied to crude oil on thin slice during film-making;In Jing Xiaguan Sample is examined, crude oil smearing is chosen uniformly and region of the thickness less than 0.03mm is tested.
In step 2, tested under selection freezing, transmission optical mode, acquisition time selection 12s, scanning times 64 times, Resolution ratio 8cm-1, slit area is 150 × 150 μm2, analysis wave band is 600-4000cm-1, according to actual sample situation, adjustment Experiment parameter.
In step 4, after selecting Experimental Area, before testing crude oil, signal is optimized, when reflection light When the energy column value of transmitance is more than 5, energy column color is green, illustrates that the transmitance of light is good, carries out face to sample again at this time Sweep.
In steps of 5, maturity figure is calculated using Fourier infrared spectrum spectrogram, comprised the following steps:
A, the baseline of sample spectrogram is determined using segmentation base-line method;
B, divides the position of methylmethylene, 3000cm-1~2947cm-1Wave band is methyl CH3aAsymmetric stretching vibration is inhaled Receive area, 2947cm-1~2883cm-1Wave band is methylene CH2aAsymmetric stretching vibration uptake zone, calculates the peak of two wave bands respectively Area;
C, calculates methylene and methyl ratio C H2a/CH3a, to characterize the maturity of crude oil.
The Fourier infrared spectrum analytical method of quick test crude maturity in the present invention, can quickly to crude oil into Row IR spectrum scanning, can quickly test crude oil, avoid the oil component caused by long-time operation and change, improve original Oily maturity indices CH2a/CH3aAccuracy.
Brief description of the drawings
Fig. 1 is a specific embodiment of the Fourier infrared spectrum analytical method of the quick test crude maturity of the present invention Flow chart;
Fig. 2 is to utilize Fourier infrared spectrum spectrogram calculating maturity figure in the specific embodiment of the present invention.
Embodiment
For enable the present invention above and other objects, features and advantages become apparent, it is cited below particularly go out preferable implementation Example, and coordinate shown in attached drawing, it is described in detail below.
As shown in Figure 1, Fig. 1 is the stream of the Fourier infrared spectrum analytical method of the quick test crude maturity of the present invention Cheng Tu.
In step 101, instrument is opened, liquid nitrogen cooling is added in instrument, by instrument stabilizer 15 minutes, into standby shape State.In one embodiment, the articles for use such as thin slice sample preparation used, glass bar are soaked with chloroform, cleaned, are dried for standby;Open Fourier micro ft-ir spectroscopy instrument, and liquid nitrogen is added in instrument, instrument stabilizer 15 minutes, then keeps holding state.Flow Enter step 102.
In a step 102, crude oil is uniformly applied to the top layer of thin slice, during smearing cannot with hand contact thin slice and Crude oil.In Microscopic observation sample, choose crude oil smearing uniformly and region of the thickness less than 0.03mm is tested.Flow enters Step 103.
In step 103, tested under selection freezing, transmission optical mode.Recommended parameter value, acquisition time selection 12s, Scanning times 64 times, resolution ratio 8cm-1, slit area is 150 × 150 μm2, analysis wave band is 600-4000cm-1, can basis Actual sample situation, regulation experiment parameter.Flow enters step 104.
At step 104, background scans are carried out to thin slice, and preserves background result.Flow enters step 105.
In step 105, crude oil scanning area is selected, signal optimization is carried out to it, when the energy of the transmitance of reflection light When column value is more than 5, energy column color is green, illustrates that the transmitance of light is good, then carries out face to sample and sweep.Flow enters step 106。
In step 106, Sample Scan the data obtained is preserved into * .map forms.Flow enters step 107.
In step 107, gained spectrogram is handled using OMNIC Specta softwares, calculates methylene and methyl ratio Value CH2a/CH3a.Flow terminates.
Fig. 2 calculates maturity figure for the present invention using Fourier infrared spectrum spectrogram.One in the application present invention is specific In embodiment, comprise the following steps:
In step 1, the baseline of sample spectrogram is determined using segmentation base-line method.Flow enters step 2.
In step 2, the position of methylmethylene, 3000cm are divided-1~2947cm-1Wave band is mainly methyl (CH3a) no Symmetrical stretching vibration uptake zone, 2947cm-1~2883cm-1Wave band is mainly methylene (CH2a) asymmetric stretching vibration absorption Area, calculates the peak area of two wave bands respectively, and flow enters step 3.
In step 3, methylene and methyl ratio C H are calculated2a/CH3a, to characterize the maturity of crude oil.Flow terminates.

Claims (6)

1. quickly test crude maturity Fourier infrared spectrum analytical method, it is characterised in that this quickly test crude oil into The Fourier infrared spectrum analytical method of ripe degree includes:
Step 1, crude oil is uniformly applied on thin slice, film-making is spare;
Step 2, under freezing, light transmission mode, each experiment parameter is adjusted;
Step 3, back end scanning is carried out with thin slice to experiment, and preserves background result;
Step 4, face is carried out to crude oil selection area to sweep to obtain spectrogram;
Step 5, spectrum analysis are carried out, calculate maturity indices CH2a/CH3a
2. the Fourier infrared spectrum analytical method of quick test crude maturity according to claim 1, its feature exist In the Fourier infrared spectrum analytical method for quickly testing crude maturity further includes, and before step 1, sample preparation is used Thin slice, glass bar these articles for use soak with chloroform, cleaned, are dried for standby;Fourier micro ft-ir spectroscopy instrument is opened, and in instrument Liquid nitrogen is added in device, instrument stabilizer 15 minutes, then keeps holding state.
3. the Fourier infrared spectrum analytical method of quick test crude maturity according to claim 1, its feature exist In, in step 1, to crude oil carry out film-making, crude oil is uniformly applied on thin slice during film-making;In Microscopic observation sample Product, choose crude oil smearing uniformly and region of the thickness less than 0.03mm is tested.
4. the Fourier infrared spectrum analytical method of quick test crude maturity according to claim 1, its feature exist In in step 2, selection freezing, transmit and tested under optical mode, and acquisition time selection 12s, scanning times 64 times, are differentiated Rate 8cm-1, slit area is 150 × 150 μm2, analysis wave band is 600-4000cm-1, according to actual sample situation, regulation experiment Parameter.
5. the Fourier infrared spectrum analytical method of quick test crude maturity according to claim 1, its feature exist In, in step 4, select Experimental Area after, before testing crude oil, signal is optimized, when reflection light transmission When the energy column value of rate is more than 5, energy column color is green, illustrates that the transmitance of light is good, and carrying out face to sample again at this time sweeps.
6. the Fourier infrared spectrum analytical method of quick test crude maturity according to claim 1, its feature exist In, in steps of 5, using Fourier infrared spectrum spectrogram calculate maturity figure, comprise the following steps:
A, the baseline of sample spectrogram is determined using segmentation base-line method;
B, divides the position of methylmethylene, 3000cm-1~2947cm-1Wave band is methyl CH3aAsymmetric stretching vibration absorbs Area, 2947cm-1~2883cm-1Wave band is methylene CH2aAsymmetric stretching vibration uptake zone, calculates the peak face of two wave bands respectively Product;
C, calculates methylene and methyl ratio C H2a/CH3a, to characterize the maturity of crude oil.
CN201610942622.5A 2016-11-01 2016-11-01 The Fourier infrared spectrum analytical method of quick test crude maturity Pending CN108020523A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104678018A (en) * 2015-02-13 2015-06-03 中国石油天然气股份有限公司 Crude oil mass fracture maturity evaluation method
CN105572324A (en) * 2016-02-19 2016-05-11 西南石油大学 Analysis method of oil and gas geochemical characteristics

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104678018A (en) * 2015-02-13 2015-06-03 中国石油天然气股份有限公司 Crude oil mass fracture maturity evaluation method
CN105572324A (en) * 2016-02-19 2016-05-11 西南石油大学 Analysis method of oil and gas geochemical characteristics

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
伏美燕 等: "AHDEB油田白垩系油藏油气充注期次的流体包裹体证据", 《地球科学——中国地质大学学报》 *
申家年主编: "《石油地质实验原理及分析方法》", 30 August 2012, 哈尔滨工业大学出版社 *

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