CN113624743A - Method for dividing microscopic components by applying Raman spectrum parameters - Google Patents
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- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000004079 vitrinite Substances 0.000 claims abstract description 20
- 238000001069 Raman spectroscopy Methods 0.000 claims description 20
- 238000006073 displacement reaction Methods 0.000 claims description 15
- 238000002310 reflectometry Methods 0.000 claims description 14
- ZLHFONARZHCSET-UHFFFAOYSA-N 5-aminolevulinic acid hydrochloride Chemical compound Cl.NCC(=O)CCC(O)=O ZLHFONARZHCSET-UHFFFAOYSA-N 0.000 claims description 9
- 230000003595 spectral effect Effects 0.000 claims description 7
- 239000003245 coal Substances 0.000 claims description 6
- 239000004215 Carbon black (E152) Substances 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- 239000011435 rock Substances 0.000 claims description 5
- 238000013507 mapping Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000001228 spectrum Methods 0.000 description 5
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- 238000000386 microscopy Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
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Abstract
The invention discloses a method for dividing microscopic components by applying Raman spectrum parameters. The method realizes the description of different microscopic components by using organic laser Raman spectrum data and the parameters, and can effectively reflect the basic principle of the first-order vibration condition of carbon molecules based on the difference of the first-order vibration of the carbon molecules of different microscopic components. The method solves the problem that the microscopic components of the vitrinite and the inert material group are time-consuming and labor-consuming to distinguish; the laser Raman spectrum analysis has the advantages of small using amount, short analysis time and the like. The invention has good reliability, economy and universality, and has good application and popularization prospects.
Description
Technical Field
The invention relates to application of a laser Raman spectrum technology in the field of petroleum geology, in particular to a method for dividing microscopic components by applying Raman spectrum parameters.
Background
The micro-component classification has important significance for distinguishing the organic matter type of the hydrocarbon source rock and researching the pore space of the shale gas reservoir. In recent years, research means is developed from an optical microscope to a scanning electron microscope with higher resolution, organic microscopic component analysis is mainly identified by traditional manual analysis, and influence caused by human factors such as polished sheet polishing quality and researcher capability difference is larger. In recent years, ancient marine shale has become a research hotspot, most organic matters are in a high-over mature stage, optical properties of microscopic components gradually converge, and the traditional manual analysis method is easier to identify errors.
The Raman spectroscopy is a microstructure analysis technology, and can reflect the ordered degree and the structural defects of the structure in the thermal evolution process of the graphitized carbon substance, so that the Raman spectroscopy is widely used in oil-gas geological research in recent years. The chemical structures of different microscopic components in the coal have difference, and the carbon structure of the coal gradually becomes ordered along with the continuous deepening of the coalification effect. Therefore, the coal micro-components can be researched from the microstructure by using the Raman spectroscopy, the analysis errors caused by human factors are effectively reduced, and a reference is provided for the difference research of the shale micro-components.
Disclosure of Invention
The invention aims to provide a method for dividing micro-components by using Raman spectrum parameters, which can make up the defects of the existing method.
The method for dividing the microscopic components by applying the Raman spectrum parameters comprises the following steps:
s1, taking n hydrocarbon source rock samples as standard samples, and sequentially marking the samples as a standard sample 1, a standard sample 2 and a standard sample … …; n can be a natural number between 5 and 10;
s2, taking a standard sample 1, and selecting a microscopic component A1 on the standard sample 1; performing laser Raman scanning on one scanning point A1-1 of the microscopic component A1 to obtain a laser Raman spectrum of the scanning point A1-1 of the microscopic component A1 in the standard sample 1, subtracting the background to obtain a laser Raman spectrum of the scanning point A1-1 with the background subtracted, wherein the abscissa of the spectrum represents Raman shiftIn units of cm-1The ordinate represents the raman intensity, dimensionless; the spectrogram has two original peaks, wherein the peak with small displacement is a D peak, and the peak with large displacement is a G peak;
the laser raman scan can be performed under the following conditions:
determining laser wavelength and laser power according to the adopted laser Raman spectrometer, wherein the laser wavelength and the laser power are required to be kept consistent in the whole experimental process, for example, the laser wavelength is 532nm, the laser power is 10mW, the exposure time is 10-20 s, and the scanning range is 100-3500 cm-1。
The microscopic components can be selected by a microscope carried by a laser Raman spectrometer;
s3, performing 5-peak fitting on the laser Raman spectrum of the scanning point A1-1 after background subtraction by adopting a Mixed fitting mode of Lorentzian and Gaussian functions to obtain 5 fitting function peak curves of a D peak and a G peak in the laser Raman spectrum of the scanning point A1-1 after background subtraction, wherein the fitting function peak curve shifts are a D4 peak fitting function curve, a D1 peak fitting function curve, a D3 peak fitting function curve, a G peak fitting function curve and a D2 peak fitting function curve from small to large in sequence;
the peak intensities represented by the maximum ordinate of the D1 peak fitting function curve and the G peak fitting function curve are respectively denoted as IBiao 1-A1-1D1And ILabel 1-A1-1GThe peak displacement represented by the abscissa value corresponding to the maximum ordinate value is respectively recorded as WBiao 1-A1-1D1And WLabel 1-A1-1GThe full widths at half maximum indicated by the peak widths corresponding to one half of the maximum ordinate value are denoted as FWHM-D1Label 1-A1-1And FWHM-GLabel 1-A1-1；
The spectral peak area of the D1 peak fitting function curve and the G peak fitting function curve are respectively marked as ABiao 1-A1-1D1And ALabel 1-A1-1G；
Said IBiao 1-A1-1D1The said ILabel 1-A1-1GW is as describedBiao 1-A1-1D1W is as describedLabel 1-A1-1GThe FWHM-D1Label 1-A1-1The FWHM-GLabel 1-A1-1The above-mentioned ABiao 1-A1-1D1And said ALabel 1-A1-1GAs the D1 peakFitting a function curve and basic parameters of the G peak fitting function curve;
peak intensity ratio IBiao 1-A1-1D1/ILabel 1-A1-1GPeak displacement ratio WBiao 1-A1-1D1/WLabel 1-A1-1GSum peak area ratio ABiao 1-A1-1D1/ALabel 1-A1-1G(ii) as a derivative of said D1 peak-fitting function curve and said G peak-fitting function curve;
s4, determining a plurality of scanning points of the microscopic component A1, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum of the microscopic component A1 after background subtraction of different scanning points of the microscopic component A1 according to the steps S2-S3; preferably determining 5-10 scanning points;
s5, selecting other microscopic components on the standard sample 1, marking the microscopic components as microscopic components A2, A3 and … … Ai, respectively determining a plurality of scanning points of each microscopic component, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum of different scanning points of different microscopic components after background subtraction of the different scanning points according to the steps S2-S3; preferably determining 5-10 scanning points;
s6, measuring vitrinite reflectance R of the standard sample 1oIs denoted as Ro mark 1；
S7, repeating the steps S2-S5 to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram after background subtraction is carried out on different scanning points of different microscopic components on the rest standard samples;
s8, repeating the step S6 to obtain vitrinite reflectivities of different standards, and marking as Ro mark 2、Ro mark 3、……Ro denotes n；
S9, respectively mapping basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum spectrogram after background subtraction is carried out on the vitrinite reflectivity of different standard samples and different scanning points of different microscopic components on different standard samples to obtain Raman spectrum parameters with good correlation with vitrinite reflectivity on the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram;
s10, respectively drawing the vitrinite reflectivity of different standard samples and Raman spectrum parameters with good correlation with vitrinite reflectivity on a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram obtained in the step S9 to obtain Raman spectrum parameters and RoWhether the combined cross plot can classify microscopic components and thermal maturity Ro% of combined cross plots of every two Raman spectrum parameters with good correlation can be used for dividing organic microscopic components;
and S11, taking the intersection image of the parameter combinations which can divide the microscopic components and are obtained in the step S11 as a template, and taking the data point concentrated area, namely the distribution range of the microscopic components and the inert components.
In the method of the invention, the type III hydrocarbon source rock sample can be a coal sample or shale in a continental phase stratum, a marine phase stratum or a sea-land transition phase stratum.
The method mainly utilizes organic laser Raman spectrum data and the parameters to realize the description of different microscopic components, and is based on the basic principle that the first-order vibration of carbon molecules of different microscopic components is different, and the laser Raman spectrum can effectively reflect the first-order vibration condition of the carbon molecules. The method solves the problem that the microscopic components of the vitrinite and the inert material group are time-consuming and labor-consuming to distinguish; the laser Raman spectrum analysis has the advantages of small using amount, short analysis time and the like. The invention has good reliability, economy and universality, and has good application and popularization prospects.
Drawings
FIG. 1 shows the peak fitting results of Raman spectra.
Fig. 2 shows raman spectra of different organic micro-components (fig. 2a shows the original raman spectrum, and fig. 2b shows the raman spectrum after pretreatment).
FIG. 3 is a combination of Raman spectral parameters for the compartmentalized microscopy fractions.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The experimental instrument used in the following examples is an in Via type laser microscopy confocal Raman spectrometer with a laser wavelength of 532nm, a laser power of 10mW, an exposure time of 10s and a scanning range of 100-3500 cm-1The number of analysis spots per micro-component in each sample was 10.
The method for dividing the microscopic components by using the Raman spectrum parameters comprises the following steps:
taking 10 coal samples with different maturity at east edges of an Ordos basin as standard samples, numbering the 10 standard samples, and sequentially taking a standard sample 1, a standard sample 2, a standard sample … …, a standard sample 9 and a standard sample 10;
secondly, a standard sample 1 is taken, one scanning point of one micro component is selected on the standard sample 1 for laser Raman scanning, and a laser Raman spectrum of the scanning point of the micro component in the standard sample 1 is obtained, wherein the abscissa of the spectrum represents Raman displacement and the unit is cm-1The ordinate represents the raman intensity, dimensionless; the spectrogram has two original peaks, wherein the peak with small displacement is a D peak, and the peak with large displacement is a G peak;
deducting the background of the original Raman spectrum of the scanning points of the microscopic components in the standard sample 1 to obtain a laser Raman spectrum of the scanning points of the microscopic components in the standard sample 1 after deducting the background;
step four, adopting a Mixed fitting mode of Lorentzian and Gaussian functions to perform 5-peak fitting on the laser Raman spectrum of the standard sample 1 with the background subtracted from the scanning points of the microscopic components to obtain 5 fitting function peak curves of a D peak and a G peak in the laser Raman spectrum of the standard sample 1 with the background subtracted from the scanning points of the microscopic components, wherein the displacement is 1240cm from small to large-1Nearby 1350cm-1Nearby 1540cm-1About 1600cm-1Near, 1610cm-1Nearby, the displacement of the fitting function peak curve is sequentially a D4 peak fitting function curve, a D1 peak fitting function curve, a D3 peak fitting function curve, a G peak fitting function curve and a D2 peak fitting function curve from small to large (figure 1);
d1 peak simulation in laser Raman spectrum of micro component scanning point minus background in standard sample 1The peak intensities represented by the maximum ordinate of the resultant curve and the G-peak fitted function curve are respectively denoted as IBiao 1-1D1、ILabel 1-1G(ii) a The peak displacements represented by the abscissa values corresponding to the maximum ordinate values are respectively recorded as WBiao 1-1D1、WLabel 1-1G(ii) a The full widths at half maximum indicated by the peak widths corresponding to one half of the maximum vertical coordinate are denoted as FWHM-D1Tab 1-1、FWHM-GTab 1-1；
The spectral peak area of the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram obtained by subtracting the background from the scanning point of the microscopic component in the standard sample 1 are respectively marked as ABiao 1-1D1、ALabel 1-1G；
I in laser Raman spectrum spectrogram fitting curve of standard sample 1 with background subtracted from scanning point of micro-componentBiao 1-1D1、ILabel 1-1G、WBiao 1-1D1、WLabel 1-1G、FWHM-D1Tab 1-1、FWHM-GTab 1-1、ABiao 1-1D1、ALabel 1-1GFitting the basic parameters of the function curve for the D1 peak and the G peak; the derivative parameters of the D1 peak fitting function curve and the G peak fitting function curve have a peak intensity ratio IBiao 1-1D1/ILabel 1-1GPeak displacement ratio WBiao 1-1D1/WLabel 1-1GPeak area ratio ABiao 1-1D1/ALabel 1-1G；
Fifthly, re-determining 10 scanning points of the microscopic component on the standard sample 1 obtained in the second step, and operating each scanning point according to the second step to the fourth step to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum of the microscopic component after background subtraction of different scanning points;
step six, re-determining other microscopic components on the standard sample obtained in the step two, and classifying the microscopic components by taking a microscopic component and an inert component as classification standards; determining 10 scanning points for different microscopic components respectively, and operating each scanning point according to the steps from two to five; obtaining the laser Raman spectrum spectra (figure 2) of different scanning points of different microscopic components and the basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectra after background subtraction, wherein the Raman spectrum spectra of different microscopic components are different before and after treatment as can be seen from figure 2;
step seven, taking the standard sample 1 which completes the 6 steps as a measuring object, and measuring the reflectivity R of the vitriniteoIs denoted as Ro mark 1；
Eighthly, repeating the second step to the sixth step to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum after background subtraction is carried out on different scanning points of different microscopic components on different standard samples;
step nine, repeating the step seven to obtain the vitrinite reflectivity R on different standard sampleso mark 2、Ro mark 3、……Ro denotes n；
Step ten, obtaining vitrinite reflectivity R of different standard samples in step seven and step nineo mark 1、Ro mark 2、……Ro denotes nRespectively mapping basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum after background subtraction is carried out on different scanning points of different microscopic components on different standard samples obtained in the first to sixth steps and the ninth step to obtain Raman spectrum parameters with good correlation with the vitrinite reflectance on the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum;
step eleven, obtaining vitrinite reflectivity R of different standard samples in step seven and step nineo mark 1、Ro mark 2、……Ro denotes nAnd respectively mapping the D1 peak fitting function curve and the Raman spectrum parameters with good correlation with the vitrinite reflectance of the G peak fitting function curve in the laser Raman spectrum spectrogram obtained in the step ten to obtain the Raman spectrum parameters and the RoWhether the combined cross plot can classify microscopic components and thermal maturity Ro% good correlation of raman spectral parameters a merged picture of two-by-two combinations of spectral parameters can be used to classify organic microscopic components.
Specific results are shown in table 1. Wherein the difference in displacement RBS ═ WG-WD1Peak intensity ratio R1 ═ ID1/IG
Table 1 raman spectral parameter combinations for the fractioned microscopic components (Ro% ═ 0.55-1.88%)
Step twelve, taking the intersection image of the parameter combinations which can be used for dividing the microscopic components and is obtained in the step eleven as a template, and taking a part of the distribution image of the data point concentrated region, namely the distribution range of the microscopic components, the inert components and other large-class microscopic components as shown in the figure 3, so that the laser Raman spectrum parameters can well distinguish different microscopic components.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. A method for dividing microscopic components by using Raman spectrum parameters comprises the following steps:
s1, taking n hydrocarbon source rock samples as standard samples, and sequentially marking the samples as a standard sample 1, a standard sample 2 and a standard sample … …;
s2, taking a standard sample 1, and selecting a microscopic component A1 on the standard sample 1; performing laser Raman scanning on one scanning point A1-1 of the microscopic component A1 to obtain a laser Raman spectrum of the scanning point A1-1 of the microscopic component A1 in the standard sample 1, and subtracting the background to obtain a laser Raman spectrum of the scanning point A1-1 with the background subtracted;
s3, performing 5-peak fitting on the laser Raman spectrum of the scanning point A1-1 after background subtraction by adopting a Mixed fitting mode of Lorentzian and Gaussian functions to obtain 5 fitting function peak curves of a D peak and a G peak in the laser Raman spectrum of the scanning point A1-1 after background subtraction, wherein the fitting function peak curves are a D4 peak fitting function curve, a D1 peak fitting function curve, a D3 peak fitting function curve, a G peak fitting function curve and a D2 peak fitting function curve in sequence from small to large according to displacement;
the peak intensities represented by the maximum ordinate of the D1 peak fitting function curve and the G peak fitting function curve are respectively denoted as IBiao 1-A1-1D1And ILabel 1-A1-1GThe peak displacement represented by the abscissa value corresponding to the maximum ordinate value is respectively recorded as WBiao 1-A1-1D1And WLabel 1-A1-1GThe full widths at half maximum indicated by the peak widths corresponding to one half of the maximum ordinate value are denoted as FWHM-D1Label 1-A1-1And FWHM-GLabel 1-A1-1；
The spectral peak area of the D1 peak fitting function curve and the G peak fitting function curve are respectively marked as ABiao 1-A1-1D1And ALabel 1-A1-1G；
Said IBiao 1-A1-1D1The said ILabel 1-A1-1GW is as describedBiao 1-A1-1D1W is as describedLabel 1-A1-1GThe FWHM-D1Label 1-A1-1The FWHM-GLabel 1-A1-1The above-mentioned ABiao 1-A1-1D1And said ALabel 1-A1-1GAs basic parameters of the D1 peak-fitting function curve and the G peak-fitting function curve;
peak intensity ratio IBiao 1-A1-1D1/ILabel 1-A1-1GPeak displacement ratio WBiao 1-A1-1D1/WLabel 1-A1-1GSum peak area ratio ABiao 1-A1-1D1/ALabel 1-A1-1G(ii) as a derivative of said D1 peak-fitting function curve and said G peak-fitting function curve;
s4, determining a plurality of scanning points of the microscopic component A1, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum of the microscopic component A1 after background subtraction of different scanning points of the microscopic component A1 according to the steps S2-S3;
s5, selecting other microscopic components on the standard sample 1, marking the microscopic components as microscopic components A2, A3 and … … Ai, respectively determining a plurality of scanning points of each microscopic component, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum of different scanning points of different microscopic components after background subtraction of the different scanning points according to the steps S2-S3;
s6, measuring vitrinite reflectance R of the standard sample 1oIs denoted as Ro mark 1；
S7, repeating the steps S2-S5 to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram after background subtraction is carried out on different scanning points of different microscopic components on the rest standard samples;
s8, repeating the step S6 to obtain vitrinite reflectivities of different standards, and marking as Ro mark 2、Ro mark 3、……Ro denotes n；
S9, respectively mapping basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum spectrogram after background subtraction is carried out on the vitrinite reflectivity of different standard samples and different scanning points of different microscopic components on different standard samples to obtain Raman spectrum parameters with good correlation with vitrinite reflectivity on the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram;
s10, respectively drawing the vitrinite reflectivity of different standard samples and Raman spectrum parameters with good correlation with vitrinite reflectivity on a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram obtained in the step S9 to obtain Raman spectrum parameters and RoWhether the combined cross plot can classify microscopic components and thermal maturity Ro% of combined cross plots of every two Raman spectrum parameters with good correlation can be used for dividing organic microscopic components;
and S11, taking the intersection image of the parameter combinations which can divide the microscopic components and are obtained in the step S11 as a template, and taking the data point concentrated area, namely the distribution range of the microscopic components and the inert components.
2. The method of claim 1, wherein: the hydrocarbon source rock sample is a coal sample or shale in a continental phase stratum, a marine phase stratum or a sea-land transition phase stratum.
3. The method according to claim 1 or 2, characterized in that: n is a natural number between 5 and 10.
4. The method according to any one of claims 1-3, wherein: the laser raman scanning conditions were as follows:
the laser wavelength and the laser power are determined according to the adopted laser Raman spectrometer, the laser wavelength and the laser power are kept consistent in the whole experiment process, the exposure time is 10-20 s, and the scanning range is 100-3500 cm-1。
5. The method according to any one of claims 1-4, wherein: and selecting the microscopic components by using a microscope carried by a laser Raman spectrometer.
6. The method according to any one of claims 1-5, wherein: in steps S4 and S5, 5 to 10 scanning points are determined.
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| CN105044077A (en) * | 2015-06-24 | 2015-11-11 | 中国石油大学(华东) | Acquiring method of organic matter thermal maturity quantitative characterization function and application of function |
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