CN113959998B - Method for determining crude oil components and occurrence states thereof based on fluorescence lifetime - Google Patents
Method for determining crude oil components and occurrence states thereof based on fluorescence lifetime Download PDFInfo
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Abstract
The invention provides a method for determining crude oil components and occurrence states thereof based on fluorescence lifetime, which comprises the following steps: (1) preparing a sample to be tested comprising a standard component smear and a rock slice; (2) scanning a sample to be detected by using a fluorescence lifetime imaging mode to obtain fluorescence lifetime data of the sample to be detected; (3) selecting laser with the wavelength of 492nm as an excitation light source, selecting an xyz scanning mode, receiving a data body within the range of 520nm to 740nm, determining rock sample pores and transparent mineral distribution characteristics in a rock slice through transmitted light and reflected light, and obtaining a rock sample pore and transparent mineral distribution diagram; (4) comparing the fluorescence life data of the rock slice with the fluorescence life data of the standard components, determining the components in the rock slice according to the comparison result, and obtaining a raw oil component distribution map in the rock slice; (5) and (4) matching the raw oil component distribution diagram of the rock slice with the rock sample pore and transparent mineral distribution diagram obtained in the step (3) according to the coordinates of the measuring points to obtain the occurrence state of the raw oil components in the rock pore of the rock slice. The method has the characteristics of high accuracy, visualization and no damage.
Description
Technical Field
The invention relates to a method for determining crude oil components of shale and sandstone and occurrence states thereof.
Background
With the increasing energy demand and the continuous consumption of conventional oil and gas resources, the supply and demand of the oil and gas resources are short, unconventional oil and gas gradually become the successive field of oil and gas growth, wherein the unconventional oil and gas such as shale oil and gas is one of the most practical successive fields, and the occurrence characteristics of different components of crude oil in a reservoir have important significance for oil and gas exploration and development and recovery ratio improvement. Previous researches on components in crude oil generally adopt a column chromatography method to separate the components from the crude oil and measure the content of the components, and the column chromatography method has three limitations: firstly, the method needs to leach crude oil from rocks and dry the crude oil by an extraction method, and a large amount of components are escaped due to extraction temperature and drying temperature in the process; secondly, the separation limit between the components in the method has obvious measurement error due to different solvent dosage and experimental operation; thirdly, the method cannot directly quantitatively characterize the three-dimensional occurrence state characteristics of the rock in the rock, and cannot determine the relationship between different components and pore characteristics.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a method for determining crude oil components and occurrence states thereof based on fluorescence lifetime, which is a feasible and reliable method for representing the content of the crude oil family components, the three-dimensional space distribution state, the distribution relation of the family components, pores and transparent minerals in a rock sample by observing the three-dimensional distribution characteristics of the crude oil family components in mudstone by using a laser confocal fluorescence lifetime imaging mode under the condition of keeping the original state of the rock sample.
The technical scheme of the invention is as follows: the method for determining the components and occurrence states of crude oil based on fluorescence lifetime comprises the following steps:
preparing a sample to be tested comprising a standard component smear and a rock slice;
secondly, scanning a sample to be detected by using a fluorescence life imaging mode of a fluorescence life confocal microscope to obtain a fluorescence life data body of the sample to be detected;
selecting pulse laser with the wavelength of 492nm as an excitation light source, selecting an xyz scanning mode, receiving a data body within the range of 520nm to 740nm, determining rock sample pores and transparent mineral distribution characteristics in the rock slice through transmitted light and reflected light, and obtaining a rock sample pore and transparent mineral distribution diagram;
Comparing the fluorescence life data of the rock slice with the fluorescence life data of the standard components, determining the components in the rock slice according to the comparison result, and obtaining a distribution map of the raw oil components in the rock slice;
and fifthly, matching the distribution diagram of the crude oil components in the rock slice with the rock sample pores and the transparent mineral distribution diagram obtained in the third step according to coordinates of the measuring points to obtain the occurrence state of the crude oil components in the rock pores in the rock slice.
Preferably, in the first step, the standard component smear sample to be tested is prepared by uniformly smearing the components separated from the crude oil on a glass slide to prepare the standard component smear sample to be tested, and the rock slice sample to be tested is prepared by using a freezing flaking method to prepare the rock slice sample to be tested under the condition that the crude oil in the rock slice is kept unchanged in an original state.
Preferably, in the second step, the rock slice to be detected is scanned, and the data volume with the fluorescence lifetime of 0.6-2.5ns is received to obtain a fluorescence lifetime image.
And the fourth step is carried out according to the following path, namely if the fluorescence life data of the rock slice and the sample to be tested of the standard component are compared, the average value of the fluorescence life of the sample to be tested of the rock slice is within the fluorescence life confidence interval [ mu-sigma, mu + sigma ] of a certain component in the sample to be tested of the standard component, mu is the average value, sigma is the standard deviation, and the confidence level is 0.683, and the component in the crude oil in the sample to be tested of which the point substance is the standard component can be determined.
The analysis of the fluorescence lifetime data of the obtained standard component smear shows that the fluorescence lifetime of the standard component obeys normal distributionX~N(μ,σ2) Where μ is the mean, σ is the standard deviation, and the confidence interval is [ μ - σ, μ + σ ]]The confidence level was 0.683.
The μ value and the σ value of the standard component are determined by fitting the fluorescence lifetime distribution of the standard substance.
Selecting fluorescence lifetime data of more than 1000 measuring points, taking the maximum value and the minimum value of the fluorescence lifetime as a statistical interval, equally dividing the statistical interval into 100 small intervals, counting the number of the fluorescence lifetime data of 1000 measuring points in the 100 small intervals of the statistical interval, and dividing the number of each small interval by 1000 to obtain the frequency with the small interval.
Carrying out distribution function curve fitting on the frequencies of the 100 small intervals and the corresponding fluorescence life, and selecting R after fitting2(correlation coefficient, i.e., degree of agreement between test data and fitting function) of the maximum distribution function, and the fitting distribution function in the experiment is a normal distribution function having the maximum correlation coefficient (R)2>0.999), see formula (1).
In the formula: y-frequency,%;
x-fluorescence lifetime, ns;
μ -mean fluorescence lifetime, ns;
σ — standard deviation, ns.
And thirdly, determining the mu value and the sigma value of the standard component according to the mu value and the sigma value in the fitted distribution function.
After each component of the crude oil in the sample to be detected of the rock slice is determined through the fluorescence lifetime, the distribution characteristics of each component in the scanning space are determined by utilizing the relation between each component and the scanning space, and thus the crude oil component distribution map in the sample to be detected of the rock slice is obtained.
And in the fifth step, matching the distribution diagram of the crude oil components in the rock slice with the distribution diagram of the rock sample pores and the transparent minerals obtained in the step (3) according to the coordinates of the measuring points, namely superposing the distribution characteristic data of the rock pores and the transparent minerals of the same measuring point coordinates and the distribution characteristic data of the crude oil components in the pores, and recovering the content of the crude oil group components in the rock sample to be measured, the three-dimensional space distribution state and the distribution relation between each group of components and the pores and the transparent minerals.
The invention has the following beneficial effects:
in unconventional oil and gas exploitation, the research on the components of the oil family has important significance for the planning of oil exploitation schemes. The method can reliably characterize the content of crude oil group components, the three-dimensional space distribution state, and the distribution relation of each group of components, pores and transparent minerals in the rock sample under the condition of keeping the original state of the rock sample, and has the advantages of visualization, accuracy, no damage and the like.
Description of the drawings:
FIG. 1 is a schematic diagram of the determination of a component in crude oil based on fluorescence lifetime distribution.
FIG. 2 is fluorescence lifetime data for components in crude oil. Wherein, (a) a saturated hydrocarbon; (B) aromatic hydrocarbons; (C) asphaltenes.
FIG. 3 is a graph of rock sample fluorescence lifetime imaging. In (a) plan view, and (b) perspective view, in an actually generated color picture, red: a saturated hydrocarbon; green: aromatic hydrocarbons; blue color: asphaltenes.
Figure 4 is an imaging view of a rock sample mineral. Wherein, (a) plan view, (b) perspective view, in the actually generated color picture, gray: and (4) minerals.
FIG. 5 is a diagram showing the types of component occurrence states, wherein, left: actually measuring data; and (3) right: theoretical models and mathematical models. Wherein, (a) free state, (b) adsorbed state, in the actually generated color picture, red: a saturated hydrocarbon; green: aromatic hydrocarbons; blue color: asphaltenes; off-white: and (4) minerals.
FIG. 6 is a superposition of a rock sample transmitted and reflected light imaging data volume and a rock sample fluorescence lifetime imaging data volume. In the color picture actually generated, the color image is red: a saturated hydrocarbon; green: aromatic hydrocarbons; blue color: asphaltenes; off-white: and (4) minerals.
The specific implementation mode is as follows:
the invention will be further described with reference to the accompanying drawings in which:
fluorescence lifetime refers to the average residence time of a molecule after excitation by a light pulse before returning to the ground state. The fluorescence lifetime is an inherent property of a fluorescent substance, and the structure of the fluorescent substance is a dominant factor for determining the fluorescence lifetime, so that the components in the crude oil can be determined by the fluorescence lifetime of the components of the crude oil.
One particular embodiment of the invention is given below, with samples from the Songliaowan. An experimental instrument: Leica-STELLARIS, fluorescence lifetime confocal microscope. Detection conditions are as follows: the lens is a 10-time lens, the digital amplification is 0.75 time, the pixel size is 541.58nm multiplied by 541.58nm, the scanning frequency is 400Hz, the acquisition condition is Line Average denoising for 4 times, and the Frame Average denoising for 2 times.
The specific implementation process comprises the following steps:
1. sample preparation
(1) Preparation of Standard component smears
The components in the crude oil are separated into three components of saturated hydrocarbon, aromatic hydrocarbon and asphaltene through a chromatography method. The components were smeared evenly onto glass slides to make standard component smears, i.e., saturates, aromatics and asphaltene smears, with numbering marks.
(2) Preparation of rock slice to be tested by using freezing flaking method
In connection with issued patents, patent names: hand-held type oil-containing sandstone refrigeration abrasive disc device. The patent number is as follows: ZL201310173697.8, taking out the pressure maintaining rock sample frozen in liquid nitrogen, grinding into rock slices of 25mm × 25mm × 2mm in low temperature freezing environment to ensure that the crude oil in the rock slices is in solid state and the original state of the crude oil in the pores is kept unchanged.
2. Scanning standard material using fluorescence lifetime imaging mode
And (3) inversely placing the crude oil group component standard sample slice on an object stage of a microscope, selecting pulse laser as an excitation light source, selecting an xyz scanning mode, respectively scanning the standard component smear prepared in the step (1), and receiving a data volume of the fluorescence lifetime.
The fluorescence lifetime data of the standard component smear obtained is analyzed, and the fluorescence lifetime of the standard component is subject to normal distributionX~N(μ,σ2) Where μ is the mean, σ is the standard deviation, and the confidence interval is [ μ - σ, μ + σ ]]The confidence level was 0.683, see fig. 1.
The μ value and the σ value of the standard component were determined by fitting to the fluorescence lifetime distribution of the standard substance.
Selecting fluorescence lifetime data of more than 1000 measuring points, taking the maximum value and the minimum value of the fluorescence lifetime as a statistical interval, equally dividing the statistical interval into 100 small intervals, counting the number of the fluorescence lifetime data of 1000 measuring points in the 100 small intervals of the statistical interval, and dividing the number of each small interval by 1000 to obtain the frequency with the small interval.
Carrying out distribution function curve fitting on the frequencies of the 100 small intervals and the corresponding fluorescence life, and selecting R after fitting2(correlation coefficient, i.e. degree of agreement between test data and fitting function) maximum distribution function, distribution of fit in experimentThe function is a normal distribution function with the maximum correlation coefficient (R)2>0.999), see formula (1).
In the formula: y-frequency,%;
x-fluorescence lifetime, ns;
μ -mean fluorescence lifetime, ns;
σ — standard deviation, ns.
And thirdly, determining the mu value and the sigma value of the standard component according to the mu value and the sigma value in the fitted distribution function.
The fluorescence lifetime data of the standard component smear obtained by the experiment are shown in FIG. 2, and according to the analysis of the data results, the following data can be obtained:
(1) saturated hydrocarbons: the fluorescence lifetime data of the received saturated hydrocarbon is normally distributedX~N(1.83402，0.399362) Confidence interval at a confidence level of 0.683 is [1.43466, 2.23338 ]]If the fluorescence lifetime of the measuring point is in the range of 1.43466ns-2.23338ns, the measuring point substance can be determined as saturated hydrocarbon and is displayed as red in a color image, and the color image is shown in figure 2A.
(2) Aromatic hydrocarbons: the fluorescence lifetime data of the received aromatic hydrocarbon is normally distributedX~N(0.99509，0.099852) Confidence interval at a confidence level of 0.683 is [0.89524, 1.09494 ] ]If the fluorescence lifetime of the measuring point is in the range of 0.89524ns-1.09494ns, the measuring point substance can be determined as aromatic hydrocarbon and is displayed as green in a color image, and the color image is shown in figure 2B.
(3) Asphaltenes: the fluorescence lifetime data of the received asphaltenes is normally distributedX~N(0.69472，0.100112) Confidence interval at confidence level 0.683 [0.59461, 0.79483 ]]If the fluorescence lifetime of the measuring point is in the range of 0.59461ns-0.79483ns, the measuring point substance can be determined as asphaltene, which is displayed as blue in a color image, as shown in figure 2C.
3. Scanning rock slice to be measured by utilizing fluorescence lifetime imaging mode
The rock slice to be detected is placed on an object stage of a microscope in an inverted mode, pulse laser is selected as an excitation light source, an xyz scanning mode is selected, the rock slice to be detected is scanned, and a data volume with the fluorescence lifetime of 0.6-2.5ns is received to obtain a fluorescence lifetime image, which is shown in figure 3.
4. Rock pore and mineral analysis
The rock sample slice to be detected is placed on an object stage of an optical microscope in an inverted mode, laser with the wavelength of 492nm is selected as an excitation light source, an xyz scanning mode is selected, a data body in the range of 520nm to 740nm is received, rock sample pores and transparent minerals in the sample to be detected are determined through transmitted light and reflected light, the distribution characteristics of the rock sample pores and the transparent minerals in a scanning space are determined by utilizing the relationship between the rock sample pores and the transparent minerals and the scanning space, and therefore a distribution diagram of the rock sample pores and the transparent minerals is obtained, and the diagram is shown in figure 4.
5. Determination of components in a sample to be tested
Judging and analyzing the fluorescence lifetime data of the sample to be tested measured in the step 3 and the fluorescence lifetime data of the standard component measured in the step 2:
if the average value of the fluorescence life of the sample to be measured is within a saturated hydrocarbon fluorescence life confidence interval [1.43466, 2.23338] (the confidence level is 0.683), determining that a measured point substance is a saturated hydrocarbon component and representing the saturated hydrocarbon component by red;
determining that the measured point substance is an aromatic hydrocarbon component if the average value of the fluorescence life of the sample to be measured is within the aromatic hydrocarbon fluorescence life confidence interval (0.89524, 1.09494) (the confidence level is 0.683), and representing the measured point substance by green;
and thirdly, if the average value of the fluorescence lifetime of the sample to be detected is within the asphaltene fluorescence lifetime confidence interval (0.59461, 0.79483) (the confidence level is 0.683), determining that the substance at the detected point is the asphaltene component and representing the substance by blue.
And determining the components of the crude oil in the sample to be detected through the fluorescence lifetime, and determining the distribution characteristics of the components in the scanning space by using the relationship between the components and the scanning space, thereby obtaining the crude oil component distribution map in the rock sample.
6. Analysis of occurrence state of crude oil component in rock
And (4) matching the distribution diagram of the crude oil components in the rock sample to be detected, which is determined in the step (5), with the distribution diagram of the rock sample pores and the transparent minerals, which is measured in the step (4), according to the measuring point coordinates, namely superposing the distribution characteristic data of the rock pores and the transparent minerals and the distribution characteristic data of the crude oil components in the pores, and recovering the content of the crude oil group components, the three-dimensional space distribution state and the distribution relation of each group of components, the pores and the transparent minerals in the rock sample to be detected, so as to obtain the occurrence state of the crude oil components in the rock pores.
The existing state of the crude oil component in the pore space can be divided into a free state and an adsorption state, and the position relationship between the fluorescence lifetime distribution diagram and the mineral distribution diagram of the component is determined. According to the type of the occurrence state of the components (figure 5), the intersection of the fluorescence lifetime distribution diagram of the saturated hydrocarbon and the rock mineral distribution diagram is an empty set, and the saturated hydrocarbon is in a free state (figure 5 a); the intersection of the fluorescence lifetime map of the aromatics with the rock mineral map is non-empty and the aromatics are in the adsorbed state (fig. 5 b).
According to the occurrence state of the crude oil components in the rock pores, the following can be obtained: the rock is differentially enriched with saturated hydrocarbons, aromatic hydrocarbons and asphaltene, wherein the saturated hydrocarbons are distributed in interparticle gaps and corrosion pores in a strip shape, the aromatic hydrocarbons are distributed in pores in an isolated shape, and the content of the asphaltene is less than that of the saturated hydrocarbons and the aromatic hydrocarbons; the presence of the transparent minerals provides enriched pore space for each component, mainly inter-granular pores, and a small part of the minerals are corroded to generate corrosion pores. Saturated and aromatic hydrocarbons in the crude oil component are distributed in the pores mainly in a free state, and asphaltenes are adsorbed on the surfaces of the mineral particles in an adsorption state, as shown in fig. 6.
Claims (4)
1. A method for determining crude oil components and occurrence states thereof based on fluorescence lifetime comprises the following steps:
The method comprises the steps of firstly, preparing a sample to be tested comprising a standard component smear and a rock slice;
secondly, scanning a sample to be detected by using a fluorescence life imaging mode of a fluorescence life confocal microscope to obtain a fluorescence life data body of the sample to be detected;
selecting pulse laser with the wavelength of 492nm as an excitation light source, selecting an xyz scanning mode, receiving a data body within the range of 520nm to 740nm, determining rock sample pores and transparent mineral distribution characteristics in the rock slice through transmitted light and reflected light, and obtaining a rock sample pore and transparent mineral distribution diagram;
comparing the fluorescence life data of the rock slice with the standard components, determining the components in the rock slice according to the comparison result, and obtaining the raw oil component distribution diagram in the rock slice;
the fourth step is carried out according to the following path, namely, if the fluorescence life data of the rock slice and the sample to be detected of the standard component are compared, the average value of the fluorescence life of the sample to be detected of the rock slice is within the fluorescence life confidence interval [ mu-sigma, mu + sigma ] of a certain component in the sample to be detected of the standard component, mu is the average value, sigma is the standard deviation, and the confidence level is 0.683, the component in the crude oil in the sample to be detected of which the measuring point substance is the standard component can be determined;
In this step, the determination of the μ value and the σ value is determined by fitting the fluorescence lifetime distribution of the standard substance, that is, the fluorescence lifetime distribution of the measurement points in a certain range of the standard substance is obtained as a histogram, wherein the number of the measurement points>1000, the abscissa is the fluorescence lifetime and the ordinate is the frequency, and a distribution function curve fitting is performed, selecting R after fitting2Maximum distribution function, and directly determining mu value and sigma value by fitting distribution function2Is the correlation coefficient, i.e. the degree of agreement between the test data and the fitting function;
determining each component of crude oil in a sample to be detected of the rock slice through the fluorescence life, and determining the distribution characteristics of each component in a scanning space by utilizing the relationship between each component and the scanning space so as to obtain a crude oil component distribution map in the sample to be detected of the rock slice;
and fifthly, matching the distribution diagram of the crude oil components in the rock slice with the rock sample pores and the transparent mineral distribution diagram obtained in the third step according to coordinates of the measuring points to obtain the occurrence state of the crude oil components in the rock pores in the rock slice.
2. The method of claim 1 for determining crude oil composition and its occurrence based on fluorescence lifetime, wherein: in the first step, the preparation of the standard component smear sample to be tested is to evenly smear the components separated from the crude oil on a glass slide to prepare the standard component smear sample to be tested, and the preparation of the rock slice sample to be tested is to prepare the rock slice sample to be tested by utilizing a freezing flaking method under the condition that the crude oil in the rock slice is ensured to be unchanged in the original state.
3. The method for determining crude oil components and occurrence states thereof based on fluorescence lifetime as claimed in claim 1 or 2, wherein: and in the second step, scanning the rock slice to be detected, and receiving a data body with the fluorescence life of 0.6-2.5ns to obtain a fluorescence life image.
4. The method of claim 1 for determining crude oil components and their occurrence based on fluorescence lifetime, wherein: and in the fifth step, matching the distribution diagram of the crude oil components in the rock slice with the distribution diagram of the rock sample pores and the transparent minerals obtained in the step (3) according to the coordinates of the measuring points, namely superposing the distribution characteristic data of the rock pores and the transparent minerals and the distribution characteristic data of the crude oil components in the pores at the same measuring point coordinates, and recovering the content of the crude oil group components in the rock sample to be measured, the three-dimensional space distribution state and the distribution relation of the group components with the pores and the transparent minerals.
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