CN105510456B - A kind of high ripe condensate oil sources determines method - Google Patents
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides a kind of high ripe condensate oil sources to determine method, and this method includes：(1) analysis detection is carried out to oil sample, determines whether contain thio adamantane compound in oil sample；(2) enrichment of thio adamantane compound is carried out to the oil sample containing thio adamantane compound；(3) sulfur isotope test is carried out to the thio adamantane compound after enrichment, test result and the sulfur isotope data of known oil-generative assemblage sulfate contrasted, so that it is determined that the oil sources of oil sample.The ripe condensate oil sources of height provided by the invention determines method, pass through this method for determining unique sexual factor in high stage of ripeness condensate, specify the oil sources of high stage of ripeness condensate, the blank of high ripe condensate OIL SOURCE CORRELATION problem can not be determined by having filled up current petroleum industry, by clearly high ripe condensate oil sources, main hydrocarbon and determination exploration highest priority series of strata and resource potential are found out so as to objective.
Description
Technical field
The invention belongs to oil field prospecting field, and in particular to a kind of high ripe condensate oil sources determines method.
Background technology
Deep Oil And Gas Exploration is the major domain of following global Oil Gas exploration.Deep layer temperature is high, pressure is big, organic-inorganic phase interaction
With strong, cause Deep Oil And Gas Exploration maturity high, standard biologic marker compounds information is lost, and can not be sentenced and be known Deep Oil And Gas Exploration source,
It is international headache, constrains the evaluation of deep layer resource potential and oil-gas exploration.Particularly Tarim Basin, deep petroleum resource is very
Abundant, main force's series of strata for exploration Ordovician Oil And Gas property is extremely complex at present, and Oil-gas source has dispute always, and also lacking has efficacious prescriptions
Method and means carry out source problem to solve high stand oil, constrain Deep Oil And Gas Exploration exploration and evaluation.
The content of the invention
To overcome above mentioned problem, it is an object of the invention to provide a kind of high ripe condensate oil sources to determine method, this method
Thio adamantane compound is chosen as biomarker, and determine by the measure of separation and concentration and sulfur isotope
Oil sources.
To reach above-mentioned purpose, the invention provides a kind of high ripe condensate oil sources to determine method, and this method includes：
(1) analysis detection is carried out to oil sample, determines whether contain thio adamantane compound in oil sample；
(2) enrichment of thio adamantane compound is carried out to the oil sample containing thio adamantane compound, enrichment
Step includes：The sulfur-containing compound in oil sample is set to be changed into sulfonium salt using methylation reaction, step by step will wherein after isolating sulfonium salt
Thiophenes and thio-ether type compounds remove, you can the thio adamantane compound after being enriched with；
(3) sulfur isotope test is carried out to the thio adamantane compound after enrichment, by test result and known life
The sulfur isotope data of oil reservoir system sulfate are contrasted, so that it is determined that the oil sources of oil sample.
In high ripe condensate oil sources determines method, firstly, it is necessary to which choosing the high stage of ripeness has the life of heat endurance
Thing marker compounds, by being found after analyzing substantial oil, adamantane and thio adamantane compound are in high maturated oil
Middle generally existing, and there is high heat endurance, therefore it is elected to be the marker compounds of high maturated oil.Secondly, how will
Thio adamantane enrichment, the requirement for reaching isotope assay amount are a problems, and the scheme that the application provides is to be based on methyl
Change and the separation principle of demethylation, it is established that a kind of method for separating oil sample component, Selective Separation thio gold therein
Firm alkane series compound is simultaneously enriched with, and makes monomer sulfur-containing compound in measure crude oil34S isotopes become a reality.Again, with same position
(sulfur isotope mass spectrum can be respectively to thio for measure of the quality spectrometer to the thio adamantane compound progress sulfur isotope of enrichment
Thio adamantane monomer compound in adamantane compound is measured), because the sulphur in compound comes from source bed
It is the sulphur in sulfate, is transferred to by organic-inorganic interaction in thio adamantane.According to stable isotope fractionation principle,
The sulfur isotope of thio adamantane monomer compound approaches with the sulfur isotope in oil-generative assemblage sulfate, then is closed with relationship
System, gap is bigger, then in the absence of affiliation, this provides the scientific information of molecular water sane level for exploration deep-seated oil gas field, according to
This can determine oil sources.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that the thio adamantane compound includes sulphur
For single adamantane compound, thiobis adamantane compound and thio three Double diamantane hydrocarbons class compound.In high ripe condensation
, can be according to actual conditions in oil, the one or more chosen in thio adamantane compound carry out analysis test.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that step is determined whether containing thio Buddha's warrior attendant in (1)
During alkyl compound, comprehensive two dimensional gas chromatography-flight time mass spectrum (GC × GC-TOFMS) and/or complete two-dimentional gas phase color are used
Spectrum-flame ionization ditector (GC × GC-FID) is analyzed and compound test.It is further preferred that in above-mentioned progress
In analysis and compound test, characteristic ion peaks of the m/z=168,182 and 192 as thio single adamantane compound is chosen；
Choose characteristic ion peaks of the m/z=206 and 220 as thiobis adamantane compound；Choose m/z=258 and 272 and be used as sulphur
The characteristic ion peak of three adamantane compounds of generation；Choose m/z=136,135,149,163,177 and 191 and be used as single adamantane
The characteristic ion peak of class compound.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that methylation reaction described in step (2) is to use
Iodomethane and silver tetrafluoroborate are handled；It is further preferred that the step of being handled using iodomethane and silver tetrafluoroborate
Including：Oil sample is dissolved in dichloromethane, silver tetrafluoroborate and iodomethane reaction is added, after reaction terminates, is filtered to remove reaction
Silver iodide precipitation in liquid, then remove methylene chloride and obtain grease；N-hexane is added into grease, it is cold through shaking
But, isolated sulfonium salt precipitation.In above-mentioned methylation reaction, after grease adds n-hexane, the temperature of cooling is preferably 0
DEG C, Rotary Evaporators can be used when removing methylene chloride.In addition, during separation sulfonium salt precipitation, most handy n-hexane is to precipitation
Repeatedly washed, make to be free of unreacted oil phase in sulfonium salt as far as possible.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that wherein, thiophene-based chemical combination is removed in step (2)
It is that the sulfonium salt for making to isolate reacts with 7- azaindoles during thing, so as to which the thiophenes in sulfonium salt be removed；
It is further preferred that the sulfonium salt for making to isolate reacts with 7- azaindoles, so as to by the thiophene-based in sulfonium salt
The step of compound removes includes：Sulfonium salt is dissolved in acetonitrile, adds the reaction of 7- azaindoles, reaction is entered after terminating with n-hexane
Go and extract liquid separation, the thiophenes in sulfonium salt, which are dissolved in n-hexane, to be removed, and other sulfonium salts substances are retained in acetonitrile
Phase.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that when thio-ether type compounds are removed in step (2),
It is other sulfonium salts substances is reacted with DMAP, (is a demethylation mistake so as to remove thio-ether type compounds
Journey, the methyl on the sulfonium salt of thio adamantane compound are divested, so that thio adamantane compound and thioether class
Compound realizes separation)；
It is further preferred that other described sulfonium salt materials are made to be reacted with DMAP, so as to remove thioether class
The step of compound, includes：Other sulfonium salts substances are dissolved in acetonitrile, DMAP is added, is reacted under counterflow condition,
Reaction adds watery hydrochloric acid after terminating, then with n-hexane extraction liquid separation；Through extracting liquid separation, thio-ether type compounds are dissolved in n-hexane phase
It is removed, thio adamantane compound is remained in acetonitrile-water phase, and the solvent in acetonitrile-water phase is removed and is enriched with
Thio adamantane compound.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that this method also includes verifying thio adamantane
Compound whether the successful step of separation and concentration, the step includes：To isolate thiophenes and thio-ether type compounds,
The thio adamantane compound of enrichment is detected, and to demonstrate thio adamantane compound, whether separation and concentration is successful.
If thio adamantane compound is substantially free of in the thiophenes and thio-ether type compounds isolated, and the sulphur being enriched with
The firm alkyl compound of cash equivalent is confirmed that, then demonstrates thio adamantane compound separation and concentration success.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that verifying thio adamantane compound separation
In the successful step of enrichment, sulphur Mass Spectrometer Method (GC- is carried out respectively to the thiophenes and thio-ether type compounds isolated
SCD) and/or gas chromatography mass spectrometry (GC-MS) is analyzed；Positive ionization electrospray-Fourier is carried out to the thio adamantane compound of enrichment
Leaf transformation-Ion cyclotron Resonance Mass Spectrometry (ESI FT-ICR MS) is analyzed.
In the ripe condensate oil sources of above-mentioned height determines method, it is preferable that verifying thio adamantane compound separation
In the successful step of enrichment, it is additionally included in before analysis and post layer first is carried out to the thiophenes and thio-ether type compounds isolated
Analyse the operation isolated and purified.
The ripe condensate oil sources of height provided by the invention determines method, solves high stand oil OIL SOURCE CORRELATION, resource potential is commented
The problems such as valency, it may be determined that main hydrocarbon and exploration target zone.Scheme provided by the invention determines the high stage of ripeness by this
The method of unique sexual factor in condensate, specifies the oil sources of high stage of ripeness condensate, having filled up current petroleum industry can not be true
The blank of fixed high ripe condensate OIL SOURCE CORRELATION problem, by clearly high ripe condensate oil sources, so as to looking for for objective
Go out main hydrocarbon and determine exploration highest priority series of strata and resource potential.
Embodiment
In order to which technical characteristic, purpose and the beneficial effect of the present invention is more clearly understood, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
A kind of method for determining high ripe condensate oil sources is present embodiments provided, this method comprises the following steps：
Step 1: the high Matured oil sample in In The Central Tarim Area (ZS1C crude oil) is chosen, in complete two-dimentional gas phase color
Spectrum/flight time mass spectrum (GC × GC-TOFMS) and comprehensive two dimensional gas chromatography-flame ionization ditector (GC × GC-FID)
On analyzed and compound test, be thio single adamantane compound according to characteristic ion m/z=168,182,192, it is special
Levy ion m/z=206,220 be thiobis adamantane compound, selection ion m/z136,135,149,163,177,191 for
Single adamantane series compound；After tested, feature biomarker is contained in oil sample：Thio single adamantane compound and
Thiobis adamantane compound.
Step 2: the separation and enrichment (methylating and demethylation process) of thio adamantane compound
Oil sample (0.5g) is dissolved in 5mL dichloromethane, sequentially adds the silver tetrafluoroborate and 15mL iodine of 5mol equivalents
Methane, 24h reactions are carried out under the conditions of room temperature lucifuge, after reaction terminates, the silver iodide precipitation that is filtered to remove in reaction solution, by filtrate
In dichloromethane removed by rotary distillation instrument；10mL n-hexanes are added into remaining grease, 0 DEG C are cooled to after concussion, sulfonium
Salt is separated out under this condition, and sulfonium salt is gathered in into bottle bottom under centrifugal condition, is inclined to the n-hexane gone out dissolved with unreacted oil,
The sulfonium salt of isolated polarity；Being washed 5 times using n-hexane can ensure to be free of unreacted oil phase in sulfonium salt；
Sulfonium salt is dissolved in 5mL acetonitriles, adds the 7- azaindoles of 10mol equivalents；After progress 48h is stirred at room temperature in reaction,
With n-hexane (3 × 10mL) extraction and liquid separation；It is divided into the n-hexane phase and acetonitrile phase dissolved with thiophene compound；N-hexane is mutually extracted
Liquid is taken by silica gel chromatography (5g silica gel, eluent are 100mL n-hexanes) to obtain thiophenes after merging concentration；
The DMAP of 10mol equivalents is added to above-mentioned acetonitrile, after reacting 12h under resulting solution counterflow condition
It is cooled to room temperature；5mL diluted hydrochloric acid aqueous solutions (2mol/L) are added thereto, and resulting solution is extracted simultaneously with n-hexane (3 × 10mL)
Liquid separation, obtain the n-hexane phase and acetonitrile-water phase dissolved with thio-ether type compounds；To mutually it be used dissolved with the n-hexane of thio-ether type compounds
Rotary distillation instrument concentrates, and then obtains thioether class chemical combination with silica gel chromatography (5g silica gel, eluent are 100mL n-hexanes)
Thing；
After the above-mentioned mutually rotated distillation apparatus of acetonitrile-water removes solvent acetonitrile and water, enriched composition is obtained, by enriched composition weight
Newly it is dissolved in acetonitrile, and the concentration for being made into 0.005mg/mL is analyzed for cation ESI FT-ICR MS；To isolated thiophene
Class compound and thio-ether type compounds carry out GC-SCD and GC-MS analyses and compared with crude oil GC-SCD analyses respectively.Analysis
Test result is shown：Thio adamantane compound, and enrichment group are substantially free of in thiophenes and thio-ether type compounds
Mainly contain thio single adamantane compound and thiobis adamantane chemical combination in point, it follows that thio adamantane chemical combination
The success of thing separation and concentration.
Step 3: the monomer sulfur isotope test of thio adamantane compound and OIL SOURCE CORRELATION
Sulfur isotope is carried out respectively to each thio adamantane monomer compound in enriched composition with isotope mass spectrometer
Measure, isotope test result shows：The same position of sulphur of thio adamantane monomer compound sulfur isotope and Cambrian system sulfate
Element is close, and very remote with Ordovician system sulfur isotope gap, so that it is determined that it is Tarim Basin Cambrian system typical case end to go out tower Crude Oil
First oil.Wherein, in ZS1C crude oil thio adamantane monomer sulfur isotope：35-38 ‰, the same position of sulphur of Cambrian system sulfate
Element：31-37 ‰, it is average：34 ‰, the two is relatively.Thio adamantane is that C-2 carbon potentials are substituted by sulphur atom in adamantane molecule
Compound, be TSR mark, be that the sulphur in stratum is bonded in organic matter, formed organic compounds containing sulfur.Therefore, sulphur
The information of corresponding series of strata is represented substantially for the sulfur isotope of adamantane.Thus, it is possible to determine thio adamantane in ZS1C crude oil
Sulphur in class comes from Cambrian system Sulfates.And the sulfur isotope of Ordovician, tarim Basin sulfate：22-27 ‰, it is average：
25.8 ‰, it is clear that with the sulfur isotope (average 35 ‰) of ZS1C crude oil and the monomer sulfur isotope (35- of thio adamantane
38 is ‰) far apart, in the absence of affiliation.Therefore, thio adamantane monomer compound sulfur isotope and Cambrian system sulfate
Sulfur isotope approach, it is and very remote with Ordovician system sulfur isotope gap, trembled with fear so that it is determined that going out ZS1C well crude oil for Tarim Basin
Force is typical end member oil.
Claims (4)
1. a kind of high ripe condensate oil sources determines method, this method includes：
(1) analysis detection is carried out to oil sample, determines whether contain thio adamantane compound in oil sample；The thio adamantane
Class compound includes thio single adamantane compound, thiobis adamantane compound and thio three Double diamantane hydrocarbons class chemical combination
Thing；
(2) enrichment of thio adamantane compound is carried out to the oil sample containing thio adamantane compound, the step of enrichment
Including：The sulfur-containing compound in oil sample is set to be changed into sulfonium salt using methylation reaction, after isolating sulfonium salt, step by step by thiophene therein
Fen class compound and thio-ether type compounds remove, you can the thio adamantane compound after being enriched with；
(3) sulfur isotope test is carried out to the thio adamantane compound after enrichment, by test result and known source bed
It is that the sulfur isotope data of sulfate are contrasted, so that it is determined that the oil sources of oil sample；
Wherein, when determining whether in step (1) containing thio adamantane compound, during using comprehensive two dimensional gas chromatography-flight
Between mass spectrum and/or comprehensive two dimensional gas chromatography-flame ionization ditector carry out analysis detection；Analysis detection is carried out described
In, choose characteristic ion peaks of the m/z=168,182 and 192 as thio single adamantane compound；Choose m/z=206 and
The 220 characteristic ion peak as thiobis adamantane compound；Choose m/z=258 and 272 and be used as thio three adamantane
The characteristic ion peak of compound；Choose the feature of m/z=136,135,149,163,177 and 191 as single adamantane compound
Quasi-molecular ions；
Wherein, methylation reaction is handled using iodomethane and silver tetrafluoroborate described in step (2)；Specifically by oil sample
It is dissolved in dichloromethane, adds silver tetrafluoroborate and iodomethane reaction, reacts after terminating, the silver iodide being filtered to remove in reaction solution
Precipitation, then remove methylene chloride and obtain grease；N-hexane is added into grease, is cooled down through concussion, it is isolated
Sulfonium salt precipitates；
Wherein, it is that the sulfonium salt for making to isolate reacts with 7- azaindoles when thiophenes are removed in step (2), from
And the thiophenes in sulfonium salt are removed；Specifically sulfonium salt is dissolved in acetonitrile, adds the reaction of 7- azaindoles, reaction knot
Shu Houyong n-hexanes carry out extraction liquid separation, and the thiophenes in sulfonium salt, which are dissolved in n-hexane, to be removed, other sulfonium salt class things
Matter is retained in acetonitrile phase；
Wherein, it is to make described other sulfonium salts substances and DMAP anti-when thio-ether type compounds are removed in step (2)
Should, so as to remove thio-ether type compounds；Other sulfonium salts substances are specifically dissolved in acetonitrile, add DMAP,
Reacted under counterflow condition, reaction adds watery hydrochloric acid after terminating, then with n-hexane extraction liquid separation；Through extracting liquid separation, thioether class
Compound is dissolved in n-hexane and is mutually removed, and thio adamantane compound is remained in acetonitrile-water phase, will be molten in acetonitrile-water phase
Agent removes the thio adamantane compound being enriched with.
2. the ripe condensate oil sources of height according to claim 1 determines method, wherein, this method also includes verifying thio gold
Firm alkyl compound whether the successful step of separation and concentration, the step includes：
The thiophenes and thio-ether type compounds isolated, the thio adamantane compound of enrichment are detected, with
Verifying thio adamantane compound, whether separation and concentration is successful.
3. the ripe condensate oil sources of height according to claim 2 determines method, wherein, verifying thio adamantane chemical combination
In the successful step of thing separation and concentration：
Sulphur Mass Spectrometer Method and/or Gc-mss are carried out respectively to the thiophenes and thio-ether type compounds isolated；
Positive ionization electrospray-Fourier transform-Ion cyclotron Resonance Mass Spectrometry analysis is carried out to the thio adamantane compound of enrichment.
4. the ripe condensate oil sources of height according to claim 3 determines method, wherein, verifying thio adamantane chemical combination
In the successful step of thing separation and concentration, first the thiophenes and thio-ether type compounds isolated are entered before being additionally included in analysis
The operation of row column chromatographic isolation and purification.
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