阅读说明：本技术 一种泥页岩含油量与精细组分同步实验分析方法 (Synchronous experimental analysis method for oil content and fine components of shale ) 是由 张居和 冯子辉 霍秋立 曾花森 张博为 鄢仁勤 冯军 张琨 于 2020-05-30 设计创作，主要内容包括：本发明公开了一种泥页岩含油量与精细组分同步实验分析方法,利用泥页岩含油量与精细组分同步实验分析装置对泥页岩同步实验分析,得到含油量、精细组分组成实验数据及碳数范围、OEP、轻重比、甲基环己烷指数、环烷指数等多个饱和烃和轻烃参数,利用此参数达到对泥页岩油储层含油性和流动性评价的目的,满足泥页岩油勘探开发对地质实验技术的需求。本发明通过方法验证,提供了泥页岩储层不同粒径、放置时间、岩相样品的含油量和精细组分特征,评价了不同岩相及深度页岩的含油性和流动性特征,比如含油性青二三段纹层状页岩好于泥岩、青一段油页岩好于页岩且随埋深增加趋于变好,为泥页岩油“四性”评价、“甜点”优选等勘探生产提供了重要实验依据。(The invention discloses a synchronous experimental analysis method for oil content and fine components of shale, which is characterized in that a synchronous experimental analysis device for the oil content and the fine components of the shale is utilized to carry out synchronous experimental analysis on the shale, so that experimental data of the oil content and the fine components and a plurality of saturated hydrocarbon and light hydrocarbon parameters such as carbon number range, OEP, light-weight ratio, methylcyclohexane index and naphthenic index are obtained, the purpose of evaluating the oil content and the fluidity of a shale oil reservoir is achieved by utilizing the parameters, and the requirement of shale oil exploration and development on geological experimental technology is met. The invention provides characteristics of different particle sizes, placing time, oil content and fine components of a petrographic sample of a shale reservoir through method verification, and evaluates the characteristics of oil content and fluidity of shale with different lithofacies and depths, for example, the shale with the oil content of green two-three striations is better than that of shale, the shale with the green one-three striations is better than that of shale, and the shale tends to be better along with the increase of the burial depth, thereby providing important experimental basis for exploration and production of shale oil with ' four-character ' evaluation, dessert ' optimization and the like.)

1. A synchronous experimental analysis method for oil content and fine components of shale comprises the following steps:

1) collecting a shale oil exploration drilling coring rock sample, and performing freeze preservation to obtain a frozen shale sample;

2) turning on a carrier gas and a chemical workstation power switch of a synchronous experimental analysis device for oil content and fine components in shale, switching on air and hydrogen, and setting working and experimental analysis condition parameters;

3) when the device in the step 2) reaches the set values of working and experimental analysis parameters, accurately weighing the mudstone standard substance for experimental analysis to obtain synchronous experimental analysis data of oil content and fine components of the mudstone standard substance;

4) coarsely crushing the frozen shale sample in the step 1), weighing the sample, and analyzing according to the same working and experimental analysis condition parameters of the shale standard substance to obtain synchronous experimental analysis data of oil content and fine components of the shale;

5) carrying out external standard method quantification on the shale sample analysis data obtained in the step 4) by using the shale standard substance analysis data obtained in the step 3) to obtain main experimental analysis parameters of the shale;

6) and 5) evaluating the oil content and fine component characteristics of the shale reservoir, the oil content of the shale and the fluidity of the shale by using the experimental analysis parameters obtained in the step 5).

2. The method for synchronously analyzing oil content and fine components in shale according to claim 1, wherein the method comprises the following steps: the shale oil content and fine component synchronous experimental analysis device in the step 2) comprises four parts, namely an oil content detection unit (1), a trapping and heat releasing unit (2), a fine component detection unit (3) and an oil content and fine component synchronous analysis control unit (4);

the synchronous analysis control unit (4) comprises an analysis control and data processor and a chemical workstation (47), and the analysis control and data processor and the chemical workstation (47) are sequentially connected with a six-way valve controller b (46), an electromagnetic valve controller (45), a trapping and hot-trap controller (44), a six-way valve controller a (43), a negative pressure pump (42), a pyrolysis furnace controller (41) and a sample injection controller (40);

the oil content detection unit (1) comprises a sample injector (10), a pyrolysis furnace (11), a quantitative flow divider (12) and an FID detector a (13), wherein the sample injector (10), the pyrolysis furnace (11), the quantitative flow divider (12) and the FID detector a (13) are communicated through a pressure-resistant pipeline in sequence; one path of the FID detector (13) is connected with an electronic flowmeter a (14), a pressure stabilizing valve a (15) and an air pipeline through pressure-resistant pipelines, and the other path of the FID detector is connected with an electronic flowmeter b (16), a pressure stabilizing valve b (17) and a hydrogen pipeline; the sample inlet end of the sample injector (10) is connected with an electronic flowmeter c (18), a pressure stabilizing valve c (19) and a carrier gas pipeline;

one end of an electronic flowmeter d (26) used for trapping by the trapping and heat releasing unit (2) is connected with the quantitative flow divider (12) of the oil content detection unit (1) through a pressure-resistant pipeline, and the other end of the electronic flowmeter d (26) is connected with a six-way valve a (20), an electromagnetic valve (21), a trapping pipe (22), the six-way valve a (20), an electronic flowmeter e (27) and a negative pressure pump (42) of the synchronous analysis control unit (4) through a pressure-resistant pipeline; one end of an electronic flowmeter d (26) during heat release is connected with the quantitative flow divider (12) of the oil content detection unit (1) through a pressure-resistant pipeline, and the other end of the electronic flowmeter d is connected with the six-way valve a (20), the electromagnetic valve (21), the collecting pipe (22), the six-way valve a (20), the six-way valve b (25) and the analysis column (30) of the fine component detection unit (3) through the pressure-resistant pipeline;

the fine component detection unit (3) comprises an analysis column (30), the sample introduction end of the analysis column (30) is connected with a six-way valve b (25) of the trapping and heat release unit (2), and the outlet end of the analysis column is connected with a FID detector b (31); one path of the FID detector b (31) is connected with the electronic flowmeter f (32), the pressure stabilizing valve d (33) and the air pipeline through pressure-resistant pipelines, and the other path of the FID detector b (31) is connected with the electronic flowmeter g (34), the pressure stabilizing valve e (35) and the hydrogen pipeline.

3. The method for synchronously analyzing oil content and fine components in shale according to claim 1, wherein the method comprises the following steps: and 1) freezing and storing the shale sample by adopting liquid nitrogen.

4. The method for synchronously analyzing oil content and fine components in shale according to claim 1, wherein the method comprises the following steps: the parameters of the set working and experimental analysis conditions in the step 2) are mainly that the initial pyrolysis temperature of the pyrolysis furnace is 30 ℃, the heating rate is 25 ℃/min, the termination temperature is 300 ℃, the constant temperature is 3min, the freezing enrichment time is 15min, the heat release temperature is 300 ℃, the heat release time is 10min, the column temperature is 35 ℃, the constant temperature is 5min, the heating rate is 5 ℃/min, and the termination temperature is 300 ℃ and the constant temperature is 30 min.

5. The method for synchronously analyzing oil content and fine components in shale according to claim 1, wherein the method comprises the following steps: the sample weighing amount in the step 3) and the step 4) is 50g, and the frozen shale in the step 4) is coarsely crushed and a sample with the particle size of 1-3 mm is taken for analysis.

6. The method for synchronously analyzing oil content and fine components in shale according to claim 1, wherein the method comprises the following steps: the experimental analysis parameters in the step 5) mainly comprise oil content (mg/g), fine component content (mg/g,%), carbon number range, OEP, light-weight ratio, methylcyclohexane index (%), naphthene index I and the like.

7. The method for synchronously analyzing oil content and fine components in shale according to claim 1, wherein the method comprises the following steps: and 6) evaluating the oil content and the fine component characteristics of the shale reservoir according to different particle sizes, different placing times and different lithofacies, and evaluating the oil content and the fluidity of the shale according to different layers and different lithofacies.

Technical Field

The invention relates to the technical field of unconventional oil and gas exploration of oil fields, in particular to a synchronous experimental analysis method for oil content and fine components of shale.

Background

The scale development of unconventional oil and gas resources such as compact sand rock oil (compact oil for short), shale oil, compact conglomerate gas (compact gas for short), shale gas and the like is realized, and the global petroleum industry is promoted to enter a new stage of overlapping conventional and unconventional oil and gas resources. The shale oil reservoir 'quadric' (reservoir, oil-bearing, fluidity and compressibility) evaluation is important research content and basis of shale oil exploration and development, while the oil-bearing and fluidity evaluation is key of the exploration and development and has important significance for shale oil 'dessert' optimization, reserve and resource quantity evaluation and other exploration and development.

The evaluation method of the oil content of shale oil and compact oil reservoirs is reported in the literature, and is referred to as ' rock pyrolysis analysis ' such as Wu Li (Wu), Zhang Zheng Ling, Li bin and the like (national standard GB/T18602 one 2012 of the people's republic of China, 7 months and 1 day 2013); (2) "petroleum and deposited organic matter hydrocarbon gas chromatography analysis methods" of Shatingrong, Li, Zhang He, etc. (China's republic of China petroleum and gas industry standard SY/T5779 one-year 2008, 12 months and 1 day 2008); (3) "the control law of the material components of the depressed shale oil reservoir on the oil content" (oil and gas geology and recovery ratio, 1 st phase in 2019) such as Tenebin, Liuhuimin and Qiongwei; (4) nintendo, wenyi hua, zheng lei and the like "pre-stack inverted tight sandstone reservoir prediction and oil-gas bearing detection" (Tu ha oil gas, stage 1 of 2012); (5) the zhangjin "shale oil well logging evaluation method and its applications" (geophysical progress, 3 rd stage 2012); (6) plum blossom, Prunus mume, a "quantitative evaluation and prediction of oil content of Dongying depressed lithologic oil and gas reservoir" (oil and gas geology and recovery ratio, 3 rd stage 2006), and the like. The (1) adopts ROCK-EVAL 6 type produced by Wanqi France company or 'crude oil ROCK evaluation instrument' produced by domestic manufacturers to detect parameters such as ROCK pyrolysis S1, S2, Tmax and the like, and evaluates the oil content of the reservoir and shale; analyzing saturated hydrocarbon, aromatic hydrocarbon and crude oil full hydrocarbon components and parameters in the rock chloroform extract by adopting a gas chromatography, and evaluating the types, maturity, oil-containing characteristics and the like of crude oil and deposited organic matter matrixes; performing crude oil occurrence state and substance component analysis on shale oil reservoirs of upper sub-section of the four-depression-in-sand section and lower sub-section of the three-depression-in-sand section by adopting a petrology and geochemistry analysis means, wherein the analysis technology comprises shale oil fluorescent sheet characteristics and scanning electron microscope occurrence state analysis technology; the step (4) adopts the integrated technology of seismic data amplitude preservation processing and prestack inversion to predict the oil-gas content of the compact and shale reservoir, which is usually the oil-gas content evaluation on the macroscopic scale; the oil content evaluation of shale oil is carried out by utilizing the logging method, and because the storage space of a compact reservoir is small, the oil and gas information detected by the logging technology is weak, and the oil content evaluation difficulty is high; and (6) establishing a quantitative prediction model of the oil content of the lithologic trap by adopting a mathematical geology method of stepwise regression and variable elimination. Therefore, the domestic and foreign experimental instrument and the analysis method can only realize the analysis of the oil content or hydrocarbon components of the shale and the compact sandstone, but cannot realize the synchronous experimental analysis of the oil content and the fine hydrocarbon components thereof, and meanwhile, a shale sample needs to be crushed by 0.07-0.15 mm during the pyrolysis analysis of the rock, so that the loss of light hydrocarbon is serious, and the accurate evaluation of the oil content and the mobility of the compact reservoir is restricted.

Disclosure of Invention

The invention provides a synchronous experimental analysis method for oil content and fine components of shale, aiming at overcoming the problem that the prior experiment in the background art is lack of a synchronous experimental analysis method for oil content and fine components of shale. According to the shale oil content and fine component synchronous experimental analysis method, the shale synchronous experimental analysis is carried out to obtain the oil content, fine component composition experimental data and geological experimental parameters, so that the purpose of evaluating the oil content and the mobility of a shale oil reservoir is achieved, and the requirement of shale oil exploration and development on the geological experimental technology is met.

The invention can solve the problems by the following technical scheme: a synchronous experimental analysis method for oil content and fine components of shale comprises the following steps:

1) collecting a shale oil exploration drilling coring rock sample, and performing freeze preservation to obtain a frozen shale sample;

2) turning on a carrier gas and a chemical workstation power switch of a synchronous experimental analysis device for oil content and fine components in shale, switching on air and hydrogen, and setting working and experimental analysis condition parameters;

3) when the device in the step 2) reaches the set values of working and experimental analysis parameters, accurately weighing the mudstone standard substance for experimental analysis to obtain synchronous experimental analysis data of oil content and fine components of the mudstone standard substance;

4) coarsely crushing the frozen shale sample in the step 1), weighing the sample, and analyzing according to the same working and experimental analysis condition parameters of the shale standard substance to obtain synchronous experimental analysis data of oil content and fine components of the shale;

5) carrying out external standard method quantification on the shale sample analysis data obtained in the step 4) by using the shale standard substance analysis data obtained in the step 3) to obtain main experimental analysis parameters of the shale;

6) and 5) evaluating the oil content and fine component characteristics of the shale reservoir, the oil content of the shale and the fluidity of the shale by using the experimental analysis parameters obtained in the step 5).

And 1) freezing and storing the shale sample by adopting liquid nitrogen.

The parameters of the set working and experimental analysis conditions in the step 2) are mainly that the initial pyrolysis temperature of the pyrolysis furnace is 30 ℃, the heating rate is 25 ℃/min, the termination temperature is 300 ℃, the constant temperature is 3min, the freezing enrichment time is 15min, the heat release temperature is 300 ℃, the heat release time is 10min, the column temperature is 35 ℃, the constant temperature is 5min, the heating rate is 5 ℃/min, and the termination temperature is 300 ℃ and the constant temperature is 30 min.

The sample weighing amount in the step 3) and the step 4) is 50g, and the frozen shale in the step 4) is coarsely crushed and a sample with the particle size of 1-3 mm is taken for analysis.

The experimental analysis parameters in the step 5) mainly comprise oil content (mg/g), fine component content (mg/g,%), carbon number range, OEP, light-weight ratio, methylcyclohexane index (%), naphthene index I and the like.

And 6) evaluating the oil content and the fine component characteristics of the shale reservoir according to different particle sizes, different placing times and different lithofacies, and evaluating the oil content and the fluidity of the shale according to different layers and different lithofacies.

Compared with the background technology, the invention has the following beneficial effects: the invention provides a synchronous experimental analysis method for oil content and fine components of shale, which is characterized in that a synchronous experimental analysis device for the oil content and the fine components of the shale is utilized to analyze the shale, geological experimental parameters such as the oil content (mg/g), the fine component content (mg/g,%) and carbon number range, OEP, light-weight ratio, methylcyclohexane index (%), naphthene index and the like can be synchronously obtained, and the parameters are utilized to evaluate the oil content and the fine component characteristics of the shale with different particle sizes, the oil content and the fine component characteristics of the shale during different placing times, and the oil content and the fine component characteristics of the shale with different rock phases, so that the purpose of evaluating the oil content and the fluidity of a shale oil reservoir is achieved, and the requirements of exploration and development of the shale oil on geological experimental technology are met.

Description of the drawings:

FIG. 1 is a schematic diagram of an experimental analysis device for the oil content and fine component synchronization of shale in the invention;

FIG. 2 is a chart of fine component analysis of block and powder samples in a simultaneous experiment according to an embodiment of the present invention;

FIG. 3 is a graph illustrating the oil content change characteristics of shale synchronously analyzed at different placement times in the embodiment of the present invention;

FIG. 4 is a diagram illustrating synchronous analysis of fine component variation characteristics of shale at different placement times according to an embodiment of the present invention;

FIG. 5 is a diagram illustrating a fine component spectrum of shale of different lithofacies in accordance with an embodiment of the present invention;

FIG. 6 is a diagram illustrating the composition of fine components of shale in different lithofacies for simultaneous analysis in accordance with an embodiment of the present invention.

In the figure:

1-oil content detection unit, 10-sample injector, 11-pyrolysis furnace, 12-quantitative flow divider, 13-FID detector a, 14-electronic flow meter a, 16-electronic flow meter b, 18-electronic flow meter c, 15-pressure stabilizing valve a, 17-pressure stabilizing valve b, 19-pressure stabilizing valve c;

2-trapping and heat releasing unit, 20-six-way valve a, 25-six-way valve b, 21-electromagnetic valve, 22-trapping pipe, 23-cold trap, 24-heat releasing trap, 26-electronic flowmeter d, 27-electronic flowmeter e;

3-fine component detection unit, 30-analytical column, 31-FID detector b, 32-electronic flow meter f, 34-electronic flow meter g, 33-pressure maintaining valve d, 35-pressure maintaining valve e;

4-oil content and fine component synchronous analysis control unit, 40-sample injector controller, 41-pyrolysis furnace controller, 42-negative pressure pump, 43-six-way valve controller a, 46-six-way valve controller b, 44-trapping and hot-trap controller, 45-solenoid valve controller, 47-analysis control and data processor and chemical workstation.

The specific implementation mode is as follows:

the invention will be further described with reference to the following drawings and specific embodiments:

the invention mainly provides a synchronous experimental analysis method for oil content and fine components of shale, which mainly utilizes a synchronous experimental analysis device for the oil content and the fine components of the shale to carry out synchronous experimental analysis and evaluation on the oil content and the fine components of the shale, thereby achieving the purpose of evaluating the oil content and the mobility of a shale oil reservoir and meeting the requirements of shale oil exploration and development on geological experimental technology.

Synchronous experimental analysis device for oil content and fine components of shale

As shown in fig. 1, the shale oil content and fine component synchronous experimental analysis device comprises an oil content detection unit 1, a capture and heat release unit 2, a fine component detection unit 3, and an oil content and fine component synchronous analysis control unit 4;

the synchronous analysis control unit 4 comprises an analysis control and data processor and a chemical workstation 47, the analysis control and data processor and the chemical workstation 47 are connected with the fine component detection unit 3 through signal lines and communication interfaces, and the analysis control and data processor and the chemical workstation 47 are further connected with a six-way valve controller b46, an electromagnetic valve controller 45, a trapping and heat-trap controller 44, a six-way valve controller a43, a negative pressure pump 42, a pyrolysis furnace controller 41 and a sample injection controller 40 in sequence.

The oil content detection unit 1 mainly comprises a sample injector 10, a pyrolysis furnace 11, a quantitative flow divider 12 and an FID detector a13, wherein the sample injector 10, the pyrolysis furnace 11, the quantitative flow divider 12 and the FID detector a13 are sequentially communicated through a pressure-resistant pipeline; one path of the FID detector 13 is connected with an electronic flowmeter a14, a pressure stabilizing valve a15 and an air pipeline through pressure-resistant pipelines, and the other path of the FID detector is connected with an electronic flowmeter b16, a pressure stabilizing valve b17 and a hydrogen pipeline; the sample inlet end of the sample injector 10 is connected with an electronic flow meter c18, a pressure stabilizing valve c19 and a gas carrying pipeline; meanwhile, the sample injector 10 and the pyrolysis furnace 11 are respectively connected with a sample injection controller 40 and a pyrolysis furnace controller 41 of the synchronous analysis control unit 4 through signal lines and communication interfaces; the other outlet of the quantitative flow divider 12 is connected with an electronic flowmeter d26 of the trapping and heat releasing unit 2 through a pressure-resistant pipeline;

one end of an electronic flowmeter d26 used for trapping by the trapping and heat releasing unit 2 is connected with the quantitative flow divider 12 of the oil content detecting unit 1 through a pressure-resistant pipeline, and the other end is connected with a six-way valve a20, an electromagnetic valve 21, a trapping pipe 22, a six-way valve a20, an electronic flowmeter e27 and a negative pressure pump 42 of the synchronous analysis control unit 4 through a pressure-resistant pipeline; one end of an electronic flowmeter d26 during heat release is connected with the quantitative flow divider 12 of the oil content detection unit 1 through a pressure-resistant pipeline, and the other end is connected with the six-way valve a20, the electromagnetic valve 21, the collecting pipe 22, the six-way valve a20, the six-way valve b25 and the analysis column 30 of the fine component detection unit 3 through a pressure-resistant pipeline; meanwhile, the six-way valve a20, the electromagnetic valve 21, the cold trap 23, the heat release trap 24 and the six-way valve b25 are respectively connected with the six-way valve controller a43, the electromagnetic valve controller 45, the trapping and heat trap controller 44 and the six-way valve controller b46 of the synchronous analysis control unit 4 through signal lines and communication interfaces.

The fine component detection unit 3 comprises an analytical column 30, the sample inlet end of the analytical column 30 is connected with a six-way valve b25 of the trapping and heat releasing unit 2, and the outlet end is connected with a FID detector b 31; one path of the FID detector b31 is connected with an electronic flowmeter f32, a pressure stabilizing valve d33 and an air pipeline through pressure resisting pipelines, and the other path of the FID detector b31 is connected with an electronic flowmeter g34, a pressure stabilizing valve e35 and a hydrogen pipeline; meanwhile, the fine component detection unit 3 is connected to the analysis control and data processor of the synchronous analysis control unit 4 and the chemical workstation 47 through signal lines and a communication interface, respectively.

The oil content detection unit 1 is connected with an electronic flowmeter d26, a six-way valve a20, an electromagnetic valve 21, a collection pipe 22 and a six-way valve b25 of the collection and heat release unit 2 through a quantitative flow divider 12, and then is connected with an analysis column 30 and a FID detector b31 of a fine component detection unit 3; meanwhile, the analysis control and data processor and chemical workstation 47 of the synchronous analysis control unit 4 are connected with the fine component detection unit 3, the six-way valve controller a43, the six-way valve controller b46, the electromagnetic valve controller 45, the trapping and hot trap controller 44, the negative pressure pump 42, the trapping and heat release unit 2, the pyrolysis furnace controller 41, the sample injector controller 40 and the oil content detection unit 1, so that the automatic control of the synchronous detection process of the oil content and the fine component of the shale is realized.

The oil content detection unit 1 mainly comprises a sample injector 10, a pyrolysis furnace 11, a quantitative flow divider 12, an FID detector a13, an electronic flow meter a14, an electronic flow meter b16, an electronic flow meter c18, a pressure stabilizing valve a15, a pressure stabilizing valve b17 and a pressure stabilizing valve c19 which correspond to each other and are communicated through a pressure resisting pipeline; the injector 10 is automatically turned off or on the pyrolysis furnace and the sample is topped or backed off by the injector controller 40 upon instructions from the analysis control and data processor and chemical workstation 47; the pyrolysis furnace 11 automatically realizes the automatic control of the temperature of the pyrolysis furnace according to the instructions given by the analysis control and data processor and the chemical workstation 47 by the pyrolysis furnace controller 41, the maximum pyrolysis temperature is 800 ℃, and the temperature control precision is 0.1 ℃; the quantitative flow divider 12 automatically realizes the quantitative flow division of the shale oil component by the negative pressure pump 42 according to the instructions given by the analysis control and data processor and the chemical workstation 47; the FID detector a13 automatically detects the oil content of shale or any fractional fraction by instructions from the analysis control and data processor and chemical workstation 47.

The trapping and heat releasing unit 2 mainly comprises a six-way valve a20, a six-way valve b25, an electromagnetic valve 21, a trapping pipe 22, a cold trap 23, a heat releasing trap 24, an electronic flowmeter d26 and an electronic flowmeter e27 which correspond to each other and are communicated through pressure-resistant pipelines; the negative pressure pump 42, the six-way valve a20, the six-way valve controller a43, the electromagnetic valve controller 45 of the electromagnetic valve 21, the cold trap 23 and the trapping and heat releasing controller 44 automatically realize the enrichment of shale oil or any fraction component in the trapping pipe according to the instructions given by the analysis control and data processor and the chemical workstation 47, and the lowest freezing and trapping temperature is-196 ℃; the six-way valve a20 is composed of a six-way valve controller a43, an electromagnetic valve controller 45 of an electromagnetic valve 21, a heat release trap 24 is composed of a trapping and heat release controller 44, a six-way valve b25 is composed of a six-way valve controller b46, and heat release of shale oil or any fraction component in the trapping pipe is automatically realized according to instructions given by an analysis control and data processor and a chemical workstation 47, wherein the maximum heat release temperature is 800 ℃, and the temperature control precision is 0.1 ℃; the six-way valve a20 is composed of a six-way valve controller a43, an electromagnetic valve controller 45 of an electromagnetic valve 21, a heat release trap 24 is composed of a trapping and heat release controller 44, a six-way valve b25 is composed of a six-way valve controller b46, and according to instructions given by an analysis control and data processor and a chemical workstation 47, heating, purification and emptying of the trapping and heat release unit 2 are automatically realized; the six-way valve b25 and the carrier gas of the trapping and heat releasing unit 2 are automatically aged and purified by the analytical column 30 of the fine constituent detecting unit 3 by the six-way valve controller b46, the analytical column 30 and the FID detector b31 according to instructions given from the analytical control and data processor and the chemical workstation 47.

The fine component detection unit 3 mainly comprises an analysis column 30, an FID detector b31, an electronic flowmeter f32, an electronic flowmeter g34, a pressure stabilizing valve d33 and a pressure stabilizing valve e35 which are correspondingly communicated through a pressure resisting pipeline; the analysis column 30 and the FID detector b31 automatically realize the separation and detection of shale oil or any fraction fine molecular components according to the instructions given by the analysis control and data processor and the chemical workstation 47;

the synchronous analysis control unit 4 mainly comprises a sample injection controller 40, a pyrolysis furnace controller 41, a negative pressure pump 42, a six-way valve controller a43, a six-way valve controller b46, a trapping and hot trap controller 44, an electromagnetic valve controller 45, an analysis control and data processor and a chemical workstation 47, which correspond to each other and are connected through a signal line and a communication interface, so that the automatic control of synchronous experimental analysis of oil content and fine components of the shale is realized, and the detection data recording and data processing are realized.

When the device is used, a carrier gas, a power supply and a chemical workstation switch of the shale oil content and fine component synchronous experimental analysis device are turned on, air and hydrogen are switched on, working and analysis parameters of the device are respectively set, and all set working and analysis parameter values are reached; placing the enrichment tube 22 completely in the cold trap 23 liquid nitrogen, weighing milligram samples, and placing the milligram samples into the sample injector 10; the analysis is initiated, the sample is tested, and the control and data processor and chemical workstation 47 automatically controls and records the analytical data.

Second, synchronous experimental analysis method for oil content and fine components of shale

An apparatus for synchronously testing and analyzing the oil content and the fine components of the shale is adopted.

Oil content analysis conditions of shale

Main analysis conditions of oil content of shale: the initial pyrolysis temperature of the pyrolysis furnace is 30 ℃, the programmed heating rate is 25 ℃/min, the pyrolysis termination temperature of the pyrolysis furnace is 300 ℃, and the constant temperature is 3 min; the purity of carrier gas helium is 99.999%, and the working pressure is 0.90-1.00 MPa; the purity of the fuel gas hydrogen is 99.999 percent, and the working pressure is 0.20-0.30 MPa; the working pressure of combustion-supporting gas air is 0.50-0.60 MPa; crushing a sample with the particle size of 1-3 mm, and weighing the sample by 50 mg; quantification by external standard method.

Shale oil-containing enrichment and heat release conditions

The main enrichment conditions are as follows: adopting liquid nitrogen to freeze and enrich, completely submerging the collecting pipe by liquid nitrogen, and freezing and enriching for 15 min. The main conditions of heat release are as follows: the heat release temperature is 300 ℃, the temperature control precision is 0.1 ℃, and the heat release time is 10 min; the temperature of the trapping and heat releasing unit pipeline and the valve is 300 ℃.

Analysis condition for fine components of oil content in shale

The main conditions of the fine components are as follows: a temperature programming function, a control and data processor and a chemical workstation, an analytical column 50m × 0.20mm × 0.5 μm; the temperature of the FID detector is 320 ℃; column temperature: keeping the temperature at 35 ℃ for 5min, heating to 300 ℃ at the speed of 5 ℃/min, and keeping the temperature for 30 min; gas combustion: hydrogen with a flow rate of 45 ml/min; combustion-supporting gas: air flow rate of 450 ml/min.

Qualitative and quantitative determination: standard sample, retention time and literature qualification are carried out, and C in the shale can be obtained₁～C₄₀Hydrocarbon data, geological experimental parameters.

The synchronous experimental analysis method for the oil content and the fine components of the shale is completed according to the following steps:

1) collecting a shale oil exploration drilling coring rock sample, and freezing and storing the shale oil exploration drilling coring rock sample by using liquid nitrogen to obtain a shale sample;

2) opening a power switch of a carrier gas and a chemical workstation of a synchronous experimental analysis device for oil content and fine components of shale, switching on air and hydrogen, keeping the temperature constant at 30 ℃ and a temperature rise rate of 25 ℃/min and a termination temperature of 300 ℃ for 3min, freezing and enriching time of 15min, heat release temperature of 300 ℃ and heat release time of 10min, column temperature of 35 ℃ and constant temperature of 5min, a temperature rise rate of 5 ℃/min and a termination temperature of 300 ℃ for 30 min, and setting working and experimental analysis condition parameters;

3) when the device in the step 2) reaches the set values of working and experimental analysis parameters, accurately weighing 50g of mudstone standard substance for experimental analysis to obtain synchronous experimental analysis data of oil content and fine components of the mudstone standard substance;

4) coarsely crushing the shale sample obtained in the step 1), weighing 50g of a sample with the particle size of 1-3 mm, and analyzing according to the same working and experimental analysis condition parameters of a shale standard substance to obtain synchronous experimental analysis data of oil content and fine components of shale;

5) performing external standard method quantification on the shale sample analysis data obtained in the step 4) by using the shale standard substance analysis data obtained in the step 3) to obtain experimental analysis parameters such as shale oil content (mg/g), fine component content (mg/g), carbon number range, OEP, light-weight ratio, methylcyclohexane index, naphthene index I and the like;

6) and 5) evaluating the oil content and fine component characteristics of the shale reservoir, the oil content of the shale and the fluidity of the shale by using the experimental analysis parameters obtained in the step 5).