CN108709770B - Single-period secondary oil inclusion group component sampling system and method - Google Patents

Single-period secondary oil inclusion group component sampling system and method Download PDF

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CN108709770B
CN108709770B CN201810731774.XA CN201810731774A CN108709770B CN 108709770 B CN108709770 B CN 108709770B CN 201810731774 A CN201810731774 A CN 201810731774A CN 108709770 B CN108709770 B CN 108709770B
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silica gel
gel separation
separation bag
objective table
mineral particles
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CN108709770A (en
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平宏伟
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China University of Geosciences
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China University of Geosciences
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/10Devices for withdrawing samples in the liquid or fluent state

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  • Hydrology & Water Resources (AREA)
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Abstract

The invention relates to a single-stage secondary oil inclusion group component sampling system and a single-stage secondary oil inclusion group component sampling method, which are characterized in that a rock sample which is determined to contain oil inclusion in the early stage is ground into a rock slice, fluorescence and transmission light observation are carried out on the rock slice, a silica gel separation bag is used for separating a surrounding mineral from a single-stage secondary oil inclusion region, a dichloromethane solution is filled in the silica gel separation bag, mineral particles on the surface of the rock slice are cleaned, the dichloromethane solution is added in the cleaning process for soaking the mineral particles, a final dichloromethane cleaning solution is reserved, gas chromatography and mass spectrometry are carried out until no residual hydrocarbon exists on the surface of the sample in the separation region of the silica gel separation bag, then the dichloromethane solution is filled in the silica gel separation bag again, the mineral particles containing the oil inclusion are drilled, oil in the inclusion is released and extracted into the dichloromethane solution, and finally the dichloromethane solution in the silica gel separation bag is subjected to chromatography and mass spectrometry analysis to obtain single-stage secondary oil inclusion component data.

Description

Single-period secondary oil inclusion group component sampling system and method
Technical Field
The invention relates to the technical field of various machines and engineering, including but not limited to the fields of automobile machines, textile machines, agricultural machines, engineering machines, construction engineering and the like, in particular to a single-period secondary oil inclusion group component sampling system.
Background
Oil inclusion component analysis has long been applied to oil and gas reservoir research, and can directly study the composition, heat maturity and whether secondary transformation is experienced by obtaining the molecular components of the group oil inclusions in the rock sample. Analysis of oil inclusion group composition is therefore important in hydrocarbon reservoir research.
Oil inclusion component analysis includes group inclusion component analysis and individual inclusion component analysis. The analysis of the composition of the crowd-sourced inclusion is aimed at a certain amount of rock particles containing the oil inclusion, and the crowd-sourced oil inclusion group is released and collected through breaking the rock particlesAnd (5) performing component analysis. Component analysis of individual oil inclusions for component analysis of individual oil inclusions, laser ablation methods are generally used to open the inclusions. Group oil inclusion component analysis can acquire component data of all hydrocarbons in oil, and single oil inclusion component analysis can only analyze C due to extremely low oil content in single inclusion and technical limitation 10 -C 30 Normal paraffins and partial aromatics are not able to analyze macromolecular standards. Furthermore, the equipment required for this method is expensive and not universally applicable. Group inclusion component analysis requires rock particles of a mass of several to several tens of grams, and the analysis process is very complex and time-consuming, and the oil component analyzed may be a mixture of multi-stage oils, so that its practical application is also very limited.
Therefore, if a group of oil inclusions of a single period can be found, the analysis of the group oil inclusion components of the oil inclusions of the single period can better solve the problems faced by the two methods. The greatest problem in the analysis of the composition of the single-stage oil-coated body is how to extract the oil in the single-stage oil-coated body.
Disclosure of Invention
In view of the above, the invention discloses a single-period secondary oil inclusion group component sampling system, which is characterized in that for a single sheet, firstly, a single-period secondary oil inclusion is identified, then the single-period secondary oil inclusion is physically isolated from other minerals and oil inclusions by a tool, then the single-period secondary oil inclusion component is released and acquired by a micro-region micro-drilling system, and finally, different-period secondary oil inclusion components in a sample can be acquired.
First aspect:
the invention provides a single-period secondary oil inclusion group component sampling system which comprises a positioning device, a cleaning device and a micro-drilling device, wherein the positioning device is used for positioning a secondary oil inclusion group component;
the locating device comprises a microscope and a fluorescence spectrometer, the microscope is provided with an objective table for fixing a sample, a fluorescence emitter for emitting fluorescence to the sample is arranged on the microscope above the objective table, the input end of the fluorescence spectrometer is positioned on the microscope above the objective table and used for obtaining a fluorescence spectrum of an oil inclusion after fluorescence excitation, the cleaning device and the micro-drilling device are movably arranged on the objective table on two sides of the sample, the cleaning device can clean the surface of mineral particles on the surface of the sample in the sampling process, and the micro-drilling device can break up the cleaned mineral particles containing the oil inclusion, so that release and collection of the oil components of the inclusion in the mineral particles are realized.
Further, the microscope still includes the base, vertically installs support on the base and installs eyepiece, objective on the support with the objective table, the objective table middle part is equipped with a light hole, the objective table below be equipped with the transmission light irradiator on the base, the transmission light irradiator can be followed the objective table bottom and passed through the light hole is sample irradiation transmission light, be equipped with in the support of objective table top the fluorescence emitter, the fluorescence emitter can be followed the objective table oblique top and is sample emission fluorescence on the objective table with certain angle.
Further, the cleaning device comprises a silica gel separation bag and an electric brush, wherein the silica gel separation bag can be adsorbed on the surface of a sample, an organic solvent suction pipeline and an organic solvent suction pipeline are inserted in the opening at the top of the silica gel separation bag, the electric brush is movably arranged on the objective table through a translation bracket, the translation bracket can drive the electric brush to extend into the silica gel separation bag, so that the surface of mineral particles of the rock slice is cleaned in the cleaning process, and the electric brush is driven to move out of the silica gel separation bag after the cleaning is finished;
the micro-drilling device is movably mounted on the objective table through a translation bracket, the translation bracket can drive the micro-drilling device to extend into the silica gel separation bag, drill mineral particles containing single-period secondary oil inclusion, and drive the micro-drilling device to move out of the silica gel separation bag after the punching drilling is completed.
Further, the silica gel separation bag is a sucking disc type silica gel separation bag, the diameter of the silica gel separation bag is 1-3mm, and the electric hairbrush is a 0.4mm electric hairbrush.
Further, the micro-drilling device comprises a set of small motor and a micro drill, and the diameter of the micro drill is 0.01-0.05mm.
Second aspect:
the invention discloses a method for sampling components of a single-period secondary oil coating population, which comprises the following implementation steps of,
step one: grinding a rock sample which is determined to contain oil inclusion in the early stage into a rock slice with double-sided polishing, and fixing the rock slice on a stage of a fluorescence microscope;
step two: turning on the microscope, performing fluorescence and transmitted light observation and fluorescence spectrum testing, and determining as many areas as possible containing single-period oil wraps;
step three: isolating as much of the area determined to contain the single-phase secondary oil coating as possible in step two from surrounding minerals by means of a silica gel separation capsule;
step four: filling dichloromethane solution into the silica gel separation bag, opening an electric brush to clean mineral particles on the surface of the rock slice, adding dichlorohexane solution at any time in the cleaning process to soak the mineral particles, and sucking out the organic solution after suspending for 10min after cleaning for 30 min; then adding dichloromethane solution again, and repeating the method for cleaning for 10 times;
step five: the dichloromethane solution finally sucked out in the step four is reserved, gas chromatography and mass spectrometry analysis are carried out, whether residual hydrocarbon exists in the dichloromethane solution is further analyzed, and if residual hydrocarbon exists, the step four operation is continuously repeated;
step six: filling dichloromethane solution into the silica gel separation bag again, and crushing mineral particles by using a micro drill;
step seven: collecting the dichloromethane solution, observing whether the ungrilled mineral particles exist, if so, combining the collected dichloromethane solution with the dichloromethane solution collected before to be used as a finally obtained single-period oil-coated sample, and continuing the step six; if there are no non-drilled mineral particles, the sampling is ended.
In the fourth step, when the silica gel separation bag is filled with the dichloromethane solution, whether the solution leaks or not is observed, and if the solution leaks, the silica gel separation bag needs to be fixed again.
Further, the silica gel separation bag is a sucking disc type silica gel separation bag, and the diameter of the silica gel separation bag is 1-3mm.
Further, the micro-drilling device comprises a set of small motor and a micro drill, the diameter of the micro drill is 0.01-0.05mm, and the electric hairbrush is a 0.4mm electric hairbrush.
Further, the methylene chloride solution is added into the silica gel separation capsule through an organic solvent suction line, and is discharged from the silica gel separation capsule through an organic solvent suction line.
The technical scheme provided by the invention has the beneficial effects that: firstly, identifying a single-period secondary oil inclusion body through a microscope, further physically isolating the single-period secondary oil inclusion body from other minerals and oil inclusion bodies through a sucking disc type silica gel separation bag, and then releasing and acquiring single-period secondary oil inclusion body components through a micro-drilling device.
Drawings
FIG. 1 is a block diagram of a single phase secondary oil inclusion group component sampling system of the present invention;
FIG. 2 is a block diagram of a stage of a single phase oil inclusion group component sampling system according to the present invention;
FIG. 3 is a flow chart of a method of sampling a single phase secondary oil coated population component of the present invention.
In the figure: 1. microscope 2, fluorescence spectrometer 3, objective table 4, fluorescence emitter 5, transmission light irradiator 6, silica gel separation bag 7, electric brush 8, organic solvent suction line 9, organic solvent suction line 10, translation support 11, micro-drilling device 12, base 13, support 14, eyepiece 15, objective.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, an embodiment of the present invention discloses a single-period secondary oil inclusion group component sampling system, wherein a single-period secondary oil inclusion refers to an oil inclusion captured in the same period, and the oil inclusions have similar occurrence and fluorescence spectrum characteristics. The group component sampling system consists of a positioning device for positioning the single-period secondary oil coating, a cleaning device for cleaning the surfaces of mineral particles and a micro-drilling device.
In this example, a rock sample which has been determined to contain oil inclusions is used as a sampling object, and the rock sample is ground into a double-sided polished rock sheet, the thickness of which is not too thin, and which can be slightly thicker, for example, about 0.5mm, and both sides of the rock sheet are not adhered with glass sheets.
The positioning device comprises a set of transmission light fluorescence dual-channel microscope 1, the microscope 1 is connected with a fluorescence spectrometer 2 and is used for analyzing fluorescence spectrum characteristics of oil inclusion to determine whether the oil inclusion is oil inclusion in the same period, the transmission light fluorescence dual-channel microscope 1 comprises a base 12, a support 13 vertically arranged on the base, an ocular 14 arranged on the support, an objective 15 and an objective table 3, the rock flake with double-sided light splitting is fixed on the objective table 3, the rock flake is kept to be fixed under the objective 15, a transmission light irradiator 5 is arranged on the base 12 below the objective table 3, the transmission light irradiator 5 can irradiate transmission light from the rock flake with double-sided light splitting at the bottom of the objective table 3, a fluorescence emitter 4 is further arranged in the support 13 above the objective table 3, fluorescence can be emitted from the rock flake with double-sided light splitting at a certain angle above the objective table 3, and during an experiment, the single oil inclusion in the oil inclusion can be ensured by observing the single oil inclusion in the oil inclusion distribution through the cooperation of the ocular 14 and the objective 15 through the positioning device.
The cleaning device consists of a sucking disc type silica gel separation bag 6, a 0.4mm electric hairbrush 7, an organic solvent suction pipeline 8 and an organic solvent suction pipeline 9. The diameter of the sucking disc type silica gel separation bag 6 is about 1-3mm, and the sucking disc type silica gel separation bag is mainly determined according to the distribution range of single-period secondary oil inclusion, and is used for physically separating the determined single-period secondary oil inclusion distribution range from surrounding minerals and inclusion. The electric hairbrush 7 is fixed on the objective table 3 through a translation bracket 10, the translation bracket 10 can drive the electric hairbrush 7 to move in the horizontal and vertical directions, so that the electric hairbrush 7 can be inserted into and removed from the silica gel separation bag 6, and the electric hairbrush 7 can wash the surfaces of mineral particles of the rock slices in the cleaning process and is used for accelerating removal of adsorbed organic matters, thereby ensuring quick and effective cleaning of the surfaces of the particles.
The micro-drilling device 11 is fixed between the rock slice and the microscope objective 15 through a translation bracket 10, and can drive the micro-drilling device 11 to move horizontally and vertically, so as to insert and remove the micro-drilling device 11 into and from the silica gel separation bag 6, the micro-drilling device 11 comprises a set of small motor and a micro drill bit, the diameter of the micro drill bit is about 0.01-0.05mm, and the micro drill bit is used for drilling out mineral particles containing single-period oil inclusion bodies and defined in the silica gel separation bag 6 and breaking the mineral particles, so that crude oil in the drilled oil inclusion bodies can be extracted by using an organic solvent.
A method for operating a single-period oil inclusion group component sampling system comprises the following implementation steps,
step one: grinding a rock sample which is determined to contain oil inclusions in the prior art into a double-sided polished rock slice, and fixing the rock slice on the objective table 3 of the fluorescence microscope 1;
step two: turning on the microscope 1, performing fluorescence and transmitted light observation by a fluorescence emitter and a transmitted light irradiator, and performing fluorescence spectrum test by connecting the fluorescence spectrometer 2, determining as many areas as possible containing single-period oil wraps;
step three: isolating as much of the area containing the single-phase secondary oil coating as possible determined in step two from the surrounding minerals by means of a suction cup type silica gel separation bag 6;
step four: filling dichloromethane solution into the silica gel separation bag 6 through an organic solvent suction pipeline 8, observing whether the solution leaks, if so, re-fixing the silica gel separation bag 6, if not, opening the electric hairbrush 7 to clean mineral particles on the surface of the rock slice, adding dichloromethane solution at any time in the cleaning process to soak the mineral particles, suspending for 10min after cleaning for 30min, and sucking out the organic solution through an organic solvent suction pipeline 9; subsequently, methylene chloride solution was added again through the organic solvent suction line 8, and the above-mentioned method was repeated for 10 times;
step five: the dichloromethane solution finally sucked out in the step four is reserved, gas chromatography and mass spectrometry analysis are carried out, whether residual hydrocarbon exists in the dichloromethane solution is further analyzed, and if residual hydrocarbon exists, the step four operation is continuously repeated;
step six: if no residual hydrocarbon exists, the silica gel separation bag 6 is filled with clean dichloromethane solution again, mineral particles are broken up by using a micro drill bit in the micro drill device 11, and the diameter of the micro drill bit is 0.01-0.05mm, so that oil inclusion in a single period is released and dissolved in dichloromethane;
step seven: collecting dichloromethane solution, observing whether untruncated mineral particles exist by using a fluorescence microscope 1, and if so, combining the collected dichloromethane solution with the dichloromethane solution collected before to serve as a single-period oil-coated sample finally obtained, and continuing the step six; if there are no non-drilled mineral particles, the sampling is ended.
Further, the silica gel separation bag 6 is a sucking disc type silica gel separation bag, and the diameter of the silica gel separation bag 6 is 1-3mm.
Further, the micro-drilling device 11 comprises a set of small motor and a micro drill, the diameter of the micro drill is 0.01-0.05mm, and the electric hairbrush 7 is a 0.4mm electric hairbrush.
The specific embodiments described herein are offered by way of illustration only. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
The embodiments described above and features of the embodiments herein may be combined with each other without conflict.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (6)

1. A single-period oil inclusion group component sampling system is characterized in that: comprises a positioning device, a cleaning device and a micro-drilling device;
the positioning device comprises a microscope and a fluorescence spectrometer, the microscope is provided with an objective table for fixing a sample, a fluorescence emitter for emitting fluorescence to the sample is arranged on the microscope above the objective table, the input end of the fluorescence spectrometer is positioned on the microscope above the objective table and is used for obtaining the fluorescence spectrum of an oil inclusion after fluorescence excitation, the cleaning device and the micro-drilling device are movably arranged on the objective table on two sides of the sample, the cleaning device cleans the surface of mineral particles on the surface of the sample before sampling, and the micro-drilling device drills the surface of the cleaned mineral particles to realize releasing the oil inclusion in the mineral particles and collecting the inclusion oil;
the microscope further comprises a base, a support vertically arranged on the base, an ocular, an objective lens and an objective table, wherein the ocular, the objective lens and the objective table are arranged on the support, a light passing hole is formed in the middle of the objective table, a transmission light irradiator is arranged on the base below the objective table, the transmission light irradiator irradiates transmission light for a sample from the bottom of the objective table through the light passing hole, a fluorescence emitter is arranged in the support above the objective table, and the fluorescence emitter emits fluorescence for the sample on the objective table from the obliquely upper side of the objective table at a certain angle;
the cleaning device comprises a silica gel separation bag and an electric brush, wherein the silica gel separation bag is adsorbed on the surface of a sample, an organic solvent suction pipeline and an organic solvent suction pipeline are inserted in the opening at the top of the silica gel separation bag, the electric brush is movably arranged on the objective table through a translation bracket, the translation bracket drives the electric brush to extend into the silica gel separation bag, so that the surface of mineral particles of the sample is washed in the cleaning process, and the electric brush is driven to move out of the silica gel separation bag after the cleaning is finished;
the silica gel separation bag is a sucking disc type silica gel separation bag, the diameter of the sucking disc type silica gel separation bag is 1-3mm, and the electric hairbrush is a 0.4mm electric hairbrush;
the micro-drilling device is movably mounted on the objective table through a translation bracket, the translation bracket drives the micro-drilling device to extend into the silica gel separation bag, mineral particles containing single-period oil inclusion are drilled, and the micro-drilling device is driven to move out of the silica gel separation bag after the punching drilling is completed;
the micro-drilling device comprises a set of small motor and a micro drill, wherein the diameter of the micro drill is 0.01-0.05mm.
2. A method for sampling components of a single-period secondary oil coating population is characterized by comprising the following implementation steps of,
step one: grinding a rock sample which is determined to contain oil inclusion in the early stage into a rock slice with double-sided polishing, and fixing the rock slice on a stage of a fluorescence microscope;
step two: turning on the microscope, performing fluorescence and transmitted light observation and fluorescence spectrum testing, and determining as many areas as possible containing single-period oil wraps;
step three: isolating as much of the area determined to contain the single-phase secondary oil coating as possible in step two from surrounding minerals by means of a silica gel separation capsule;
step four: filling a silica gel separation bag with a dichloromethane solution, opening an electric brush to clean mineral particles on the surface of a rock slice, adding the dichloromethane solution at any time in the cleaning process to soak the mineral particles, and sucking out the organic solution after suspending for 10min after cleaning for 30 min; then adding dichloromethane solution again, and repeating the method for cleaning for 10 times;
step five: the dichloromethane solution finally sucked out in the step four is reserved, gas chromatography and mass spectrometry analysis are carried out, whether residual hydrocarbon exists in the dichloromethane solution is further analyzed, and if residual hydrocarbon exists, the step four operation is continuously repeated;
step six: filling dichloromethane solution into the silica gel separation bag again, and crushing mineral particles by using a micro drill;
step seven: collecting the dichloromethane solution, observing whether the ungrilled mineral particles containing the oil inclusion exist or not, and if the ungrilled mineral particles exist, combining the collected dichloromethane solution with the dichloromethane solution collected before to be used as a finally obtained single-period oil inclusion sample, and continuing the operation of the step six; if there are no non-drilled mineral particles, the sampling is ended.
3. The single-phase secondary oil coated population component sampling method of claim 2, wherein: in the fourth step, when the silica gel separation bag is filled with the dichloromethane solution, whether the solution leaks or not is observed, and if the solution leaks, the silica gel separation bag needs to be fixed again.
4. The single-phase secondary oil coated population component sampling method of claim 2, wherein: the silica gel separation bag is a sucking disc type silica gel separation bag, and the diameter of the silica gel separation bag is 1-3mm.
5. The single-phase secondary oil coated population component sampling method of claim 2, wherein: the diameter of the micro drill is 0.01-0.05mm, and the electric hairbrush is 0.4 mm.
6. The single-phase secondary oil coated population component sampling method of claim 2, wherein: the methylene chloride solution is added into the silica gel separation bag through an organic solvent suction line, and is discharged from the silica gel separation bag through an organic solvent suction line.
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