CN110412151B - Method for determining phase state of oil and gas reservoir - Google Patents

Method for determining phase state of oil and gas reservoir Download PDF

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CN110412151B
CN110412151B CN201910554319.1A CN201910554319A CN110412151B CN 110412151 B CN110412151 B CN 110412151B CN 201910554319 A CN201910554319 A CN 201910554319A CN 110412151 B CN110412151 B CN 110412151B
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reservoir
gas
ethyl
noradamantane
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CN110412151A (en
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朱光有
池林贤
王萌
张志遥
李婷婷
杨海军
韩剑发
孙崇浩
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Petrochina Co Ltd
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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Abstract

The invention discloses a method for determining a phase state of an oil and gas reservoir. The method comprises the following steps: s1, identifying and identifying the ethylnoradamantane series compounds in a plurality of crude oil samples by using a full two-dimensional gas chromatography-time-of-flight mass spectrometer GC x GC-TOFMS to obtain peak information of each compound; s2, carrying out quantitative analysis on the ethyl noradamantane series compounds to obtain the content of the ethyl noradamantane series compounds; s3, fitting a relational expression between the content of the ethyl noradamantane series compounds and the gas-oil ratio of the oil reservoir; s4, establishing a relation between the reservoir gas-oil ratio and the phase state of the oil-gas reservoir; and S5, determining the phase state of the oil and gas reservoir. The method determines the phase state of the oil and gas reservoir by utilizing the content of the ethyl noradamantane, provides a new index for determining the phase state of the deep oil and gas reservoir, and provides a new solution for evaluating oil and gas resources.

Description

Method for determining phase state of oil and gas reservoir
Technical Field
The invention belongs to the technical field of petroleum sample analysis, and particularly relates to a method for determining a phase state of an oil-gas reservoir.
Background
The determination of the hydrocarbon fluid phase is the basis of the exploration and evaluation of oil and gas resources and is the first problem to be solved in the oil and gas field development process. The complexity of the fluid phase is largely governed by the type of hydrocarbon-bearing matrix and the multistage nature of the thermal evolution. Meanwhile, the phase state of the hydrocarbon fluid is also influenced by the change of the external temperature and pressure. Determining the phase of the reservoir is to determine the original phase of the hydrocarbon, and the phase of the hydrocarbon fluid at the surface state cannot represent the original phase of the hydrocarbon. The PVT phase state analysis can recover the reservoir state of the hydrocarbon fluid under the formation condition, and is the most effective means for judging the oil-gas phase state at present. In addition, the type of the oil gas can be judged by a method such as a pseudo-ternary phase diagram discrimination method, a hydrocarbon component block diagram discrimination method and the like. However, the problems of high analysis cost, long period and the like generally exist.
Comprehensive two-dimensional gas chromatography (GC x GC) is a brand new analysis means which can effectively separate complex mixtures and has good response to low-content compounds. The qualitative and quantitative analysis of the compounds in the crude oil by using the full two-dimensional flight chromatography-mass spectrometry is already popularized and applied.
Ethyl noradamantane is a very thermally stable class of compounds currently found only in crude oil, of which ethylnoradamantane (C)12H18) And ethyl norbiadamantane (C)16H22) Is the two most stable configurations of all its isomers, and therefore its degree of enrichment can be an indication of the cracking alteration that the crude oil has undergone.
Disclosure of Invention
Based on the background technology, the invention provides a method for determining the phase state of an oil and gas reservoir, which determines the phase state of the oil and gas reservoir by utilizing the content of the ethyl noradamantane series compounds, provides a new index for determining the phase state of a deep oil and gas reservoir, and provides a new solution for evaluating oil and gas resources.
In order to achieve the above purpose, the invention adopts the following scheme:
a method of determining a reservoir phase, the method comprising the steps of:
s1, identifying and identifying the ethylnoradamantane series compounds in a plurality of crude oil samples by using a full two-dimensional gas chromatography-time-of-flight mass spectrometer GC x GC-TOFMS to obtain peak information of each compound;
s2, carrying out quantitative analysis on the ethyl noradamantane series compounds to obtain the content of the ethyl noradamantane series compounds;
s3, fitting a relational expression between the content of the ethyl noradamantane series compounds and the gas-oil ratio of the oil reservoir; the oil reservoir gas-oil ratio is obtained according to the actual production data of the oil reservoir, and is the ratio of the total output of natural gas and crude oil obtained after stable production at the initial stage of oil and gas production;
s4, establishing a relation between the reservoir gas-oil ratio and the phase state of the oil-gas reservoir;
and S5, determining the phase state of the oil and gas reservoir.
Preferably, S5 includes: establishing the relation between the content of the ethyl noradamantane series compounds in the crude oil and the phase state of the oil-gas reservoir, and then directly determining the phase state of the oil-gas reservoir according to the content of the ethyl noradamantane series compounds; so as to match with corresponding exploration and development measures to ensure efficient and rapid exploration and development of oil and gas fields.
More preferably, S5 further includes: a discrimination chart is established according to the relation between the content of the ethyl noradamantane series compounds in the crude oil and the phase state of the oil-gas reservoir, the type of the oil-gas reservoir can be visually discriminated according to the total amount of the ethyl noradamantane series compounds in the crude oil, and the phase state of the oil-gas reservoir can be determined.
Preferably, the crude oil sample is added with D16An adamantane (deuterated adamantane) standard and diluted to the desired concentration using a solvent. Preferably, the solvent is dichloromethane, n-hexane can also be used, and dichloromethane has less influence on the test result because the crude oil sample does not contain dichloromethane.
According to a particular embodiment of the invention, preferably, D is added to the crude oil sample16The step of preparing an adamantane standard sample and diluting it to the desired concentration using a solvent, in particular comprising:
taking 50-200mg crude oil sample, adding D of 0.25-0.75 μ g/μ L into the crude oil sample1630-50 μ L of adamantane, adding solvent to 1.0-2.0mL,mixing uniformly for later use.
For example, the processing procedure in the embodiment of the present invention includes: a200 mg sample of crude oil was placed in a 2mL autosampler vial and D (0.5. mu.g/. mu.L concentration in methylene chloride) was added1640 μ L of adamantane standard sample, mixed well, and dichloromethane added to 1.5 mL.
Preferably, the full-two-dimensional gas chromatography-time-of-flight mass spectrometer GC × GC-TOFMS in the embodiment S1 of the present invention is manufactured by Leco corporation, and the ethyl noramantane series compound is identified and identified by comparing the mass spectrum collected by the instrument with the standard mass spectrum, so as to obtain the peak information of each compound.
Preferably, S2 specifically includes:
analyzing a crude oil sample by using a full two-dimensional gas chromatography-hydrogen flame ionization detector GC x GC-FID to obtain a GC x GC-FID spectrogram of the ethyl noradamantane; then calculating the peak area of the spectrogram in GC-FID according to the peak information of the ethylnoradamantane compound provided by GC-TOFMS, and comparing the peak area with D16Comparing the peak areas of the adamantane standard samples to obtain the content of the ethyl noradamantane series compounds.
Preferably, the correlation coefficient R of the fit of the content of the ethyl noramantadine series compounds and the gas-oil ratio of the oil reservoir in S32And when the value is more than 0.9, establishing a fitting formula.
For example, in the embodiment of the present invention, the fitting formula of the content of the ethylnoradamantane series compound in the Tarim basin hydrocarbon reservoir and the gas-oil ratio of the reservoir in S3 is as follows (as shown in FIG. 1):
G＝5.2797E1.4587(R2＝0.9121)；
wherein G is the gas-oil ratio, and E is the ethyl noradamantane content in ppm.
Those skilled in the art will readily appreciate that the fit formula will vary for a particular other reservoir, but the method is the same.
Preferably, the oil and gas reservoir phases are divided into a condensate gas reservoir, a volatile oil reservoir and a normal oil reservoir in S4; for example, for the Ordovician carbonate reservoir in the platform basin region of the Tarim basin,the normal oil reservoir gas-oil ratio is generally less than 300m3/m3The volatile oil content is generally 200-1500 m3/m3Condensate reservoirs are typically greater than 1000m3/m3。
Preferably, the method further comprises the step of verifying the validity:
compared with conventional oil and gas reservoir judgment methods such as a pseudo-ternary phase diagram judgment method, a hydrocarbon component block diagram judgment method and the like, the validity of the method is verified.
Preferably, the crude oil sample includes normal oil, condensate oil, heavy crude oil, etc., but it is derived from the wellhead of the oil well.
Preferably, the one-dimensional chromatographic column of GC × GC-TOFMS is HP-PONA (50m × 0.2mm × 0.5 μm), and the temperature programming is set: initial temperature is 50 deg.C, holding for 1min, raising to 120 deg.C at 20 deg.C/min, raising to 310 deg.C at 3 deg.C/min, and holding for 25 min; the two-dimensional chromatographic column is Rx17HT (1.5 mm multiplied by 0.1 mu m), and the temperature programming temperature is higher than the one-dimensional chromatographic column by 10 ℃; the temperature of a sample inlet is 300 ℃, the sample is injected without shunting, the carrier gas is helium, and the flow rate is 1 mL/min; modulation period 6s, with 1.8s hot blow time; in the aspect of mass spectrometry, the temperatures of a transmission line and an ion source are respectively 300 ℃ and 240 ℃, the voltage of a detector is 1600V, the mass scanning range is 40-600 amu, the acquisition rate is 100 spectrogram/s, and the solvent delay time is 0 min.
Preferably, the GC-FID analysis method adopts the same chromatographic experimental conditions as GC-TOFMS, and the flow rates of the carrier gas, the hydrogen and the air are 23mL/min, 60mL/min and 400mL/min respectively; the temperature of the detector is 310 ℃, the acquisition frequency is 200 spectrogram/s, and the solvent delay time is 9 min.
The supporting software of the instrument used in the embodiment of the invention is Chroma TOF software, a GC multiplied by GC system consists of an Agilent 7890A gas chromatograph provided with a hydrogen Flame Ionization Detector (FID) and a double-nozzle cold-hot modulator, a workstation of a flight time mass spectrometer is Chroma TOF software, the structure of the adamantane compound can be automatically identified according to the software, and quantitative analysis is carried out through a standard sample to provide accurate quantitative data of the content of the adamantane compound.
The method for determining the phase state of the oil-gas reservoir provided by the invention only depends on one drop of crude oil sample, does not need a complicated pretreatment process, directly performs qualitative analysis and quantitative calculation on the ethyl noradamantane in the crude oil sample through analysis of a full two-dimensional instrument, and further determines the phase state of the oil-gas reservoir, so that related supporting equipment and schemes for exploration and development can be rapidly determined, and the oil-gas field can be efficiently and rapidly explored and developed.
Drawings
FIG. 1 is a graph of a fit between gas-oil ratio and ethyl noradamantane content.
FIG. 2a is a two-dimensional gas chromatography dot-matrix diagram of ancient 8-well ethylnoradamantane in a Tarim basin.
FIG. 2b is a two-dimensional gas chromatography dot-matrix diagram of ancient 5-well ethylnoradamantane in a Tarim basin.
FIG. 2c is a two-dimensional gas chromatography dot-matrix diagram of Tarim basin model 101 well ethylnoramantadine.
FIG. 2d is a two-dimensional gas chromatography dot-matrix diagram of Tarim basin ancient 11-well ethylnoradamantane.
FIG. 2e is a Tary basin ancient 701 well ethyl noradamantane full two-dimensional gas chromatography dot-matrix diagram.
FIG. 2f is a two-dimensional gas chromatography dot-matrix diagram of Tarim basin 7-5 well ethylnoradamantane.
FIG. 3a is a two-dimensional gas chromatography dot-matrix chart of Zhonggu 8-well ethylnoramantane provided by GC × GC-TOFMS.
FIG. 3b is a mass spectrum corresponding to 1 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3c is a mass spectrum corresponding to 2 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3d is a mass spectrum corresponding to 3 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3e is a mass spectrum corresponding to 4 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3f is a mass spectrum corresponding to 5 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3g provides a mass spectrum corresponding to 6 in FIG. 3a from GC × GC-TOFMS.
FIG. 3h shows the mass spectrum corresponding to 7 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3i is a mass spectrum corresponding to 8 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3j is a mass spectrum corresponding to 9 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3k is a mass spectrum corresponding to 10 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3l is a mass spectrum corresponding to 11 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3m is a mass spectrum corresponding to 12 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3n is a mass spectrum corresponding to 13 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3o is a mass spectrum corresponding to 14 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3p is a mass spectrum corresponding to 15 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3q is a mass spectrum corresponding to 16 in FIG. 3a, as provided by GC × GC-TOFMS.
FIG. 3r is D provided by GC × GC-TOFMS16-mass spectrum of adamantane.
FIG. 4 is a chart of the phase states and hydrocarbon components of an ethylnoradamantane discriminating reservoir established in the present invention.
FIG. 5 is a pseudo-ternary phase diagram discrimination chart for Zhonggu 26, Zhonggu 15-2 and Zhonggu 22.
FIG. 6 is a PVT phase diagram of Zhonggu 26.
FIG. 7 is a phase diagram of PVT of Zhonggu 15-2.
FIG. 8 is a phase diagram of PVT of Zhonggu 22.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The invention is illustrated by taking Tarim basin hydrocarbon reservoirs as examples:
1) a200 mg crude oil sample was placed in a 2mL autosampler vial and 0.5. mu.g/. mu.L of D was added1640 μ L of adamantane standard sample, mixed well, and dichloromethane added to 1.5 mL.
2) Utilizing Leco corporation of AmericaA produced full-two-dimensional gas chromatography-time-of-flight mass spectrometer (GC × GC-TOFMS) analyzes a crude oil sample, compares a mass spectrogram acquired by an instrument with a standard substance spectrogram, and identifies ethyl noradamantane series compounds to obtain peak information of each compound, for example, fig. 2a to fig. 2f are full-two-dimensional gas chromatography dot-matrix charts of ethyl noradamantane corresponding to each well, wherein the abscissa is 1D retention time(s) and the ordinate is 2D retention time(s); the ethyl noradamantane corresponding to each signal peak is marked in the figure, the dotted lines separate the ethyl noradamantane with different substituent numbers, the structural formula in the dotted line area represents the typical structural formula of the compound in the area, C1-represents a carbon atom in the substituent of the compound, C2-、C3And so on.
3 a-3 q are chromatogram-mass spectra of Zhonggu 8-well ethylnoramantane. Wherein, fig. 3a is a two-dimensional gas chromatography dot-matrix diagram of the Zhonggu 8-well ethyl noradamantane provided by GC × GC-TOFMS, the numbers in the diagram represent various ethyl noradamantane series compounds, and fig. 3 b-fig. 3q are mass spectrograms corresponding to the various compounds in fig. 3 a. FIG. 3r is D16-mass spectrum of adamantane standard.
3) And analyzing by using a full two-dimensional gas chromatography-hydrogen flame ionization detector GC x GC-FID to obtain a GC x GC-FID spectrogram of the ethyl noradamantane.
4) Calculating the peak area of the spectrogram in GC × GC-FID according to the peak information of the ethylnoradamantane compound provided by GC × GC-TOFMS, and comparing the peak area with D16Comparing the peak areas of the adamantane standard samples to obtain the content of the ethyl noradamantane series compounds.
Such as D16The peak area of adamantane was 54458, the total amount was 20 μ g, the content was 183.6mg/2 (diluted twice with dichloromethane) to 54.5ppm, and the area of the EA-1 peak (numbered 2 in fig. 3 a) in the ancient 8 well was 12241, the content was 12241 × 54.5ppm/54458 to 12.25 ppm.
5) Testing a plurality of groups of crude oil samples at different well positions by calculating the obtained ethyl noradamantane content (ppm) in the step 4) to obtain the data in the table 1:
TABLE 1 Talima basin gas-oil ratio and ethyl noramantadine content data sheet
Figure BDA0002106445100000061
Fitting a relational expression between the content of the ethyl noradamantane and the gas-oil ratio of the oil reservoir according to the data in the table 1, wherein the relational expression is represented by a correlation coefficient R2Above 0.9, the fitting formula is established (as shown in fig. 1):
G＝5.2797E1.4587(R2＝0.9121)；
wherein, G-gas-oil ratio, corresponds to y in the figure; E-Ethyl noradamantane content (ppm), corresponding to x in the figure.
6) And establishing the relation between the gas-oil ratio and the phase state of the oil-gas reservoir. The oil-gas reservoir phase state is divided into a condensate gas reservoir, a volatile oil reservoir and a normal oil reservoir. For Ordovician carbonate rock oil and gas reservoirs in platform basin areas of Tarim basin, the normal reservoir gas-oil ratio is generally less than 300m3/m3The volatile oil content is generally 200-1500 m3/m3Condensate reservoirs are typically greater than 1000m3/m3。
7) Compared with conventional oil and gas reservoir judgment methods such as a pseudo-ternary phase diagram judgment method, a hydrocarbon component block diagram judgment method and the like, the validity of the method is verified.
The pseudo-ternary phase diagram discrimination method (figure 5) uses three light hydrocarbon parameters as division basis and uses C7The light hydrocarbon content is the division basis, and less than 11% is a normal oil reservoir (the region marked with 3 in fig. 5), more than 11% and less than 32% are volatile oil regions (the region marked with 2 in fig. 5), and more than 32% are condensate oil regions (the region marked with 1 in fig. 5); as can be seen from FIG. 5, the middle ancient reservoir 26 is a normal reservoir, the middle ancient reservoir 15-2 is a volatile reservoir, and the middle ancient reservoir 22 is a condensate reservoir.
The PVT phase diagrams (fig. 6, 7 and 8) show that the middle ancient 26 is a normal reservoir, the middle ancient 15-2 is a volatile reservoir, and the middle ancient 22 is a condensate reservoir.
FIG. 4 is a block diagram of hydrocarbon composition discrimination, discriminating the reservoir phase by four parameter ratios of light hydrocarbons; wherein the central axis is the relationship between the gas-oil ratio and the ethyl noradamantane derived by the invention, the scale above the central axis is the content of the noradamantane, and the scale below is the gas-oil ratio; by the method, the phase state of the oil reservoir can be determined only by determining the content of the ethyl noradamantane and directly finding the corresponding point on the central axis.
As can be seen from fig. 4, in the hydrocarbon component block diagram, the four hydrocarbon component parameters of the central ancient model 26 are all located in the normal oil reservoir region, indicating that the oil reservoir is a normal oil reservoir, the central ancient model 15-2 is a volatile oil reservoir, and the central ancient model 22 is a condensate oil reservoir. As in the ancient 26-well oil sample, the pseudo-ternary phase diagram (fig. 5) indicates that the oil reservoir drilled by the pseudo-ternary phase diagram is a normal oil reservoir; in its PVT phase diagram (fig. 6), the critical temperature pressure conditions indicate that the reservoir is a normal reservoir; in the hydrocarbon component block diagram (fig. 4), the four hydrocarbon component parameters of the 26-well oil sample are all located in the normal oil reservoir area, indicating that the oil reservoir is a normal oil reservoir. The method is too complex, the experimental requirement is high, and the oil reservoir phase state can be directly determined by the content of the ethyl noradamantane by fitting the relation between the ethyl noradamantane and the gas-oil ratio of the oil reservoir. The content of ethyl noradamantane of the ancient 26-well is 14.22ppm, and the calculation shows that the gas-oil ratio of the oil reservoir is about 249, indicating that the oil reservoir is a normal oil reservoir. The judgment result is consistent with the prior art, which shows the reliability of the method of the invention; compared with the prior art, the invention is simpler, more convenient and more direct.
8) A new discrimination chart is established, as shown in figure 4, the type of the oil and gas reservoir can be visually discriminated according to the total amount of the ethyl noradamantane series compounds in the crude oil, the phase state of the oil and gas reservoir is determined, and corresponding exploration and development measures are matched, so that the oil and gas field can be efficiently and quickly explored and developed.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.

Claims (9)

1. A method of determining a phase of a hydrocarbon reservoir, the method comprising the steps of:
s1, identifying and identifying the ethylnoradamantane series compounds in a plurality of crude oil samples by using a full two-dimensional gas chromatography-time-of-flight mass spectrometer GC x GC-TOFMS to obtain peak information of each compound;
s2, carrying out quantitative analysis on the ethyl noradamantane series compounds to obtain the content of the ethyl noradamantane series compounds;
s3, fitting a relational expression between the content of the ethyl noradamantane series compounds and the gas-oil ratio of the oil reservoir;
correlation coefficient R of fitting of ethyl noradamantane series compound content and reservoir gas-oil ratio2When the value is more than 0.9, establishing a fitting formula;
s4, establishing a relation between the reservoir gas-oil ratio and the phase state of the oil-gas reservoir;
the oil and gas reservoir phase state is divided into a condensate gas reservoir, a volatile oil reservoir and a normal oil reservoir; the gas-oil ratio of the normal oil reservoir is less than 300m3/m3The gas-oil ratio of the volatile oil reservoir is 200-1500 m3/m3The gas-oil ratio of condensate gas reservoir is greater than 1000m3/m3；
S5, determining the phase state of the oil and gas reservoir;
s5 includes: establishing a relation between the content of the ethyl noradamantane series compounds in the crude oil and the phase state of the oil-gas reservoir, establishing a distinguishing plate according to the relation between the content of the ethyl noradamantane series compounds in the crude oil and the phase state of the oil-gas reservoir, and visually determining the phase state of the oil-gas reservoir according to the total amount of the ethyl noradamantane series compounds in the crude oil.
2. The method of determining the phase of a hydrocarbon reservoir of claim 1 wherein the crude oil sample has D added thereto16Adamantane standard samples and diluted to the desired concentration using a solvent.
3. The method of determining a phase of a hydrocarbon reservoir of claim 2, wherein the solvent is methylene chloride.
4. The method of determining the phase of a hydrocarbon reservoir as claimed in claim 2, wherein the crude oil sample has D added thereto16The step of preparing an adamantane standard sample and diluting it to the desired concentration using a solvent, in particular comprising:
taking 50-200mg crude oil sample, adding D of 0.25-0.75 μ g/μ L into the crude oil sample1630-50 mu L of adamantane, adding the solvent to 1.0-2.0mL, and uniformly mixing for later use.
5. The method for determining the phase of a hydrocarbon reservoir according to claim 1, wherein S2 specifically comprises:
analyzing a crude oil sample by using a full two-dimensional gas chromatography-hydrogen flame ionization detector GC x GC-FID to obtain a GC x GC-FID spectrogram of the ethyl noradamantane; then calculating the peak area of the spectrogram in GC-FID according to the peak information of the ethylnoradamantane compound provided by GC-TOFMS, and comparing the peak area with D16Comparing the peak areas of the adamantane standard samples to obtain the content of the ethyl noradamantane series compounds.
6. The method of determining a reservoir phase according to claim 1, further comprising the step of validating:
and comparing with a pseudo-ternary phase diagram discrimination method and/or a hydrocarbon component block diagram discrimination method to verify the effectiveness of the hydrocarbon component block diagram discrimination method.
7. The method of claim 1, wherein the desired crude oil sample comprises normal oil, condensate oil, or heavy crude oil, all from a wellhead of an oil well.
8. The method for determining the phase of a hydrocarbon reservoir according to claim 5, wherein the one-dimensional chromatographic column of the GC-TOFMS is HP-PONA, 50m x 0.2mm x 0.5 μm, and the temperature programming is set as follows: initial temperature is 50 deg.C, holding for 1min, raising to 120 deg.C at 20 deg.C/min, raising to 310 deg.C at 3 deg.C/min, and holding for 25 min; the two-dimensional chromatographic column is Rx17HT, 1.5m is multiplied by 0.1mm is multiplied by 0.1 mu m, and the temperature programming temperature is higher than the one-dimensional chromatographic column by 10 ℃; the temperature of a sample inlet is 300 ℃, the sample is injected without shunting, the carrier gas is helium, and the flow rate is 1 mL/min; modulation period 6s, with 1.8s hot blow time; in the aspect of mass spectrometry, the temperatures of a transmission line and an ion source are respectively 300 ℃ and 240 ℃, the voltage of a detector is 1600V, the mass scanning range is 40-600 amu, the acquisition rate is 100 spectrogram/s, and the solvent delay time is 0 min.
9. The method of claim 8, wherein the GC x GC-FID analysis method uses the same chromatographic conditions as the GC x GC-TOFMS, and the flow rates of the carrier gas, hydrogen gas, and air are 23mL/min, 60mL/min, and 400mL/min, respectively; the temperature of the detector is 310 ℃, the acquisition frequency is 200 spectrogram/s, and the solvent delay time is 9 min.
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