CN105510456A - Determination method of oil sources of high-maturity condensate oil - Google Patents
Determination method of oil sources of high-maturity condensate oil Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The invention provides a determination method of oil sources of high-maturity condensate oil. The method comprises the following steps: (1) an oil sample undergoes analysis and detection so as to determine whether the oil sample contains a thioadamantane compound; (2) the oil sample containing the thioadamantane compound undergoes enrichment of the thioadamantane compound; and (3) the enriched thioadamantane compound undergoes sulfur isotope testing, and the test result is compared with known sulfur isotope data of source sequence sulfate so as to determine the oil source of the oil sample. By the determination method of oil sources of high-maturity condensate oil, oil sources of condensate oil at high maturity stage are determined by determining the unique factor in condensate oil at high maturity stage. Thus, the blank that oil sources of high-maturity condensate oil cannot be determined in the present petroleum industry is filled up. By determining oil sources of high-maturity condensate oil, major hydrocarbon source rocks can be truly and objectively found and key exploration target series of strata and resources potential are determined.
Description
Technical field
The invention belongs to oil field prospecting field, be specifically related to a kind of high ripe white oil oil sources defining method.
Background technology
Deep Oil And Gas Exploration is the major domain of following global Oil Gas exploration.Deep layer temperature is high, pressure large, and organic-inorganic interacts strong, causes Deep Oil And Gas Exploration degree of ripeness high, standard biologic marker compounds information dropout, cannot sentence and know Deep Oil And Gas Exploration source, be international headache, constrain the evaluation of deep layer resource potential and oil-gas exploration.Particularly Tarim Basin, deep petroleum resource is very abundant, and current main force series of strata for exploration Ordovician Oil And Gas character is very complicated, and Oil-gas source exists dispute always, also lack effective ways and means to solve high stand oil and carry out source problem, constrain Deep Oil And Gas Exploration exploitation and evaluation.
Summary of the invention
For overcoming the problems referred to above, the object of this invention is to provide a kind of high ripe white oil oil sources defining method, the method chooses sulfo-adamantane compound as biomarker, and determines oil sources by the mensuration of separation and concentration and sulfur isotope.
For achieving the above object, the invention provides a kind of high ripe white oil oil sources defining method, the method comprises:
(1) carry out analysis to oil sample to detect, whether determine in oil sample containing sulfo-adamantane compound;
(2) oil sample containing sulfo-adamantane compound is carried out to the enrichment of sulfo-adamantane compound, the step of enrichment comprises: utilize methylation reaction to make the sulfocompound in oil sample change sulfonium salt into, after isolating sulfonium salt, substep, by thiophenes wherein and thio-ether type compounds removing, can obtain the sulfo-adamantane compound after enrichment;
(3) sulfur isotope test is carried out to the sulfo-adamantane compound after enrichment, the sulfur isotope data of test result and known source sequence sulfate are contrasted, thus determines the oil sources of oil sample.
In height ripe white oil oil sources defining method, first, need to choose the biomarker that the high stage of ripeness has thermal stability, finding after to substantial oil analysis, diamantane and sulfo-adamantane compound ubiquity in high maturated oil, and there is high thermal stability, be therefore elected to be the marker compounds of high maturated oil.Secondly, how by the enrichment of sulfo-diamantane, its requirement reaching isotope assay amount is made to be a difficult problem, the scheme that the application provides is based on methylating and the separation principle of demethylation, establish a kind of method being separated oil sample component, Selective Separation sulfo-adamantane series compound wherein enrichment, make monomer sulfocompound in mensuration crude oil
34s isotope becomes a reality.Again, the sulfo-adamantane compound of isotope mass spectrometer to enrichment is used to carry out the mensuration (sulfur isotope mass spectrum can measure the sulfo-adamantane monomer compound in sulfo-adamantane compound respectively) of sulfur isotope, because the sulphur in compound comes from the sulphur in source sequence sulfate, interacted by organic-inorganic and transfer in sulfo-diamantane.According to stable isotope fractionation principle, sulfur isotope in the sulfur isotope of sulfo-adamantane monomer compound and source sequence sulfate is close, then there is sibship, gap is larger, then there is not sibship, this provides the scientific information of molecular water sane level for exploring deep-seated oil gas field, can determine oil sources accordingly.
In above-mentioned height ripe white oil oil sources defining method, preferably, described sulfo-adamantane compound comprises sulfo-list adamantane compound, thiobis adamantane compound and sulfo-three Double diamantane hydrocarbons compounds.In the ripe white oil of height, can according to actual conditions, one or more choosing in sulfo-adamantane compound carry out analytical test.
In above-mentioned height ripe white oil oil sources defining method, preferably, when determining whether in step (1) containing sulfo-adamantane compound, comprehensive two dimensional gas chromatography-flight time mass spectrum (GC × GC-TOFMS) and/or comprehensive two dimensional gas chromatography-flame ionization ditector (GC × GC-FID) is used to carry out analyzing and compound test.Further preferably, carry out in analysis and compound test above-mentioned, choose m/z=168,182 and 192 as the characteristic ion peak of sulfo-list adamantane compound; Choose the characteristic ion peak of m/z=206 and 220 as thiobis adamantane compound; Choose the characteristic ion peak of m/z=258 and 272 as sulfo-three adamantane compound; Choose m/z=136,135,149,163,177 and 191 as the characteristic ion peak of single adamantane compound.
In above-mentioned height ripe white oil oil sources defining method, preferably, methylation reaction described in step (2) uses iodomethane and silver tetrafluoroborate to process; Further preferably, the step using iodomethane and silver tetrafluoroborate to carry out processing comprises: be dissolved in by oil sample in methylene chloride, add silver tetrafluoroborate and iodomethane reaction, after reaction terminates, cross the silver iodide precipitation filtered in reactant liquor, then remove methylene chloride and obtain grease; In grease, add normal hexane, through concussion cooling, be separated and obtain sulfonium salt precipitation.In above-mentioned methylation reaction, after grease adds normal hexane, the temperature of cooling is preferably 0 DEG C, can use Rotary Evaporators during removing methylene chloride.In addition, when being separated sulfonium salt precipitation, the most handy normal hexane repeatedly washs precipitation, makes in sulfonium salt not containing unreacted oil phase as far as possible.
In above-mentioned height ripe white oil oil sources defining method, preferably, wherein, in step (2) during removing thiophenes, be that isolated sulfonium salt and 7-azaindole are reacted, thus by the thiophenes removing in sulfonium salt;
Further preferably, isolated sulfonium salt and 7-azaindole are reacted, thus the step of the thiophenes removing in sulfonium salt is comprised: sulfonium salt is dissolved in acetonitrile, add the reaction of 7-azaindole, reaction terminates rear normal hexane and carries out extraction separatory, thiophenes in sulfonium salt is dissolved in normal hexane and is removed, and other sulfonium salts substances are retained in acetonitrile phase.
In above-mentioned height ripe white oil oil sources defining method, preferably, in step (2) during removing thio-ether type compounds, that other sulfonium salts substances and DMAP are reacted, thus removing thio-ether type compounds (is a demethylation, methyl on the sulfonium salt of sulfo-adamantane compound is divested, thus makes sulfo-adamantane compound and thio-ether type compounds realize being separated);
Further preferably, other sulfonium salt materials described and DMAP are reacted, thus the step of removing thio-ether type compounds comprises: by other sulfonium salt class substance dissolves in acetonitrile, add DMAP, react under counterflow condition, add watery hydrochloric acid after reaction terminates, then use n-hexane extraction separatory; Through extraction separatory, thio-ether type compounds is dissolved in normal hexane and is removed mutually, sulfo-adamantane compound remain in acetonitrile-water mutually in, by acetonitrile-water mutually in solvent removing namely obtain the sulfo-adamantane compound of enrichment.
In above-mentioned height ripe white oil oil sources defining method, preferably, the method also comprises the checking sulfo-adamantane compound whether successful step of separation and concentration, this step comprises: detect the sulfo-adamantane compound of isolated thiophenes and thio-ether type compounds, enrichment, to demonstrate the whether separation and concentration success of sulfo-adamantane compound.If the not firm alkyl compound of sulfur-bearing cash equivalent substantially in isolated thiophenes and thio-ether type compounds, and the sulfo-adamantane compound of enrichment obtains confirmation, then demonstrate sulfo-adamantane compound separation enrichment success.
In above-mentioned height ripe white oil oil sources defining method, preferably, in the successful step of checking sulfo-adamantane compound separation enrichment, sulphur Mass Spectrometer Method (GC-SCD) and/or gas chromatography mass spectrometry (GC-MS) analysis are carried out respectively to isolated thiophenes and thio-ether type compounds; The analysis of positive ionization electrospray-Fourier transform-Ion cyclotron Resonance Mass Spectrometry (ESIFT-ICRMS) is carried out to the sulfo-adamantane compound of enrichment.
In above-mentioned height ripe white oil oil sources defining method, preferably, in the successful step of checking sulfo-adamantane compound separation enrichment, also comprise the operation first isolated thiophenes and thio-ether type compounds being carried out to column chromatographic isolation and purification before analysis.
Height provided by the invention ripe white oil oil sources defining method, solves the difficult problems such as high stand oil OIL SOURCE CORRELATION, resource potential evaluation, can determine main hydrocarbon and exploration zone of interest.Scheme provided by the invention is by this method determining uniqueness factor in high stage of ripeness white oil, specify the oil sources of high stage of ripeness white oil, fill up the blank that current petroleum industry cannot determine high ripe white oil OIL SOURCE CORRELATION problem, by clear and definite high ripe white oil oil sources, thus can the finding out main hydrocarbon and determine exploration highest priority series of strata and resource potential of objective.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
Present embodiments provide a kind of method determining high ripe white oil oil sources, the method comprises the following steps:
Step one, choose In The Central Tarim Area height Matured oil sample (ZS1C crude oil), comprehensive two dimensional gas chromatography/flight time mass spectrum (GC × GC-TOFMS) and comprehensive two dimensional gas chromatography-flame ionization ditector (GC × GC-FID) carry out analyzing and compound test, be sulfo-list adamantane compound according to characteristic ion m/z=168,182,192, characteristic ion m/z=206,220 is thiobis adamantane compound, and Selective ion mode m/z136,135,149,163,177,191 is single adamantane series compound; After tested, feature biomarker is contained in oil sample: sulfo-list adamantane compound and thiobis adamantane compound.
The separation of step 2, sulfo-adamantane compound and enrichment (methylating and demethylation process)
Oil sample (0.5g) is dissolved in the methylene chloride of 5mL, add silver tetrafluoroborate and the 15mL iodomethane of 5mol equivalent successively, 24h reaction is carried out under room temperature lucifuge condition, after reaction terminates, cross the silver iodide precipitation filtered in reactant liquor, the methylene chloride in filtrate is removed by rotary distillation instrument; In residue grease, add 10mL normal hexane, be chilled to 0 DEG C after concussion, sulfonium salt is separated out under this condition, under centrifugal condition, sulfonium salt is gathered in bottle bottom, inclines to the normal hexane going out to be dissolved with unreacted oil, is separated the sulfonium salt obtaining polarity; Use n-hexane can ensure for 5 times in sulfonium salt not containing unreacted oil phase;
Sulfonium salt is dissolved in 5mL acetonitrile, adds the 7-azaindole of 10mol equivalent; Reaction, after stirring at room temperature carries out 48h, extracts and separatory with normal hexane (3 × 10mL); Be divided into the normal hexane phase and acetonitrile phase that are dissolved with thiophene compound; Normal hexane phase extract is merged concentrated rear silica gel chromatography (5g silica gel, eluent is 100mL normal hexane) of passing through and obtain thiophenes;
Be added to the DMAP of 10mol equivalent to above-mentioned acetonitrile, after reacting 12h under gained solution return condition, be cooled to room temperature; Add 5mL diluted hydrochloric acid aqueous solution (2mol/L) wherein, gained solution normal hexane (3 × 10mL) extraction also separatory, obtains the normal hexane phase and the acetonitrile-water phase that are dissolved with thio-ether type compounds; The normal hexane being dissolved with thio-ether type compounds is concentrated with rotary distillation instrument mutually, then uses silica gel chromatography (5g silica gel, eluent is 100mL normal hexane) to obtain thio-ether type compounds;
Above-mentioned acetonitrile-water, after rotary distillation instrument removing solvent acetonitrile and water, obtains enriched composition, enriched composition is again dissolved in acetonitrile, and the concentration being made into 0.005mg/mL is analyzed for positive ion ESIFT-ICRMS; To be separated the thiophenes that obtains and thio-ether type compounds carry out respectively GC-SCD and GC-MS analyze and and crude oil GC-SCD analyze and compare.Analytical test result shows: the not firm alkyl compound of sulfur-bearing cash equivalent substantially in thiophenes and thio-ether type compounds, and it is main containing sulfo-list adamantane compound and thiobis adamantane chemical combination in enriched composition, it can thus be appreciated that, sulfo-adamantane compound separation enrichment success.
The free sulfur isotope test of step 3, sulfo-adamantane compound and OIL SOURCE CORRELATION
Isotope mass spectrometer is used each sulfo-adamantane monomer compound in enriched composition to be carried out respectively to the mensuration of sulfur isotope, isotope test result shows: the sulfur isotope of sulfo-adamantane monomer compound sulfur isotope and Cambrian system sulfate is close, and very far away with Ordovician system sulfur isotope gap, thus determine that tower Crude Oil is Tarim Basin Cambrian system typical case end member oil.Wherein, the sulfur isotope of sulfo-adamantane monomer: 35-38 ‰, the sulfur isotope of Cambrian system sulfate: 31-37 ‰ in ZS1C crude oil, average: 34 ‰, the two relatively.Sulfo-diamantane is the compound that in diamantane molecule, C-2 carbon potential is replaced by sulphur atom, is the mark of TSR, is that the sulfide linkage in stratum is incorporated in organism, forms organic compounds containing sulfur.Therefore, the sulfur isotope of sulfo-diamantane represents the information of corresponding series of strata substantially.Thus, can determine that the sulphur in ZS1C crude oil in sulfo-adamantane comes from Cambrian system Sulfates.And the sulfur isotope of Ordovician, tarim Basin sulfate: 22-27 ‰, average: 25.8 ‰, obviously and the sulfur isotope (average 35 ‰) of ZS1C crude oil and the free sulfur isotope (35-38 ‰) of sulfo-adamantane far apart, there is not sibship.Therefore, the sulfur isotope of sulfo-adamantane monomer compound sulfur isotope and Cambrian system sulfate is close, and very far away with Ordovician system sulfur isotope gap, thus determines that ZS1C well crude oil is Tarim Basin Cambrian system typical case end member oil.
Claims (10)
1. a high ripe white oil oil sources defining method, the method comprises:
(1) carry out analysis to oil sample to detect, whether determine in oil sample containing sulfo-adamantane compound;
(2) oil sample containing sulfo-adamantane compound is carried out to the enrichment of sulfo-adamantane compound, the step of enrichment comprises: utilize methylation reaction to make the sulfocompound in oil sample change sulfonium salt into, after isolating sulfonium salt, substep, by thiophenes wherein and thio-ether type compounds removing, can obtain the sulfo-adamantane compound after enrichment;
(3) sulfur isotope test is carried out to the sulfo-adamantane compound after enrichment, the sulfur isotope data of test result and known source sequence sulfate are contrasted, thus determines the oil sources of oil sample.
2. height according to claim 1 ripe white oil oil sources defining method, wherein, described sulfo-adamantane compound comprises sulfo-list adamantane compound, thiobis adamantane compound and sulfo-three Double diamantane hydrocarbons compounds.
3. height according to claim 1 ripe white oil oil sources defining method, wherein, when determining whether in step (1) containing sulfo-adamantane compound, use comprehensive two dimensional gas chromatography-flight time mass spectrum and/or comprehensive two dimensional gas chromatography-flame ionization ditector to carry out analysis and detect.
4. height according to claim 3 ripe white oil oil sources defining method, wherein, carries out in analysis and compound test described, chooses m/z=168,182 and 192 as the characteristic ion peak of sulfo-list adamantane compound; Choose the characteristic ion peak of m/z=206 and 220 as thiobis adamantane compound; Choose the characteristic ion peak of m/z=258 and 272 as sulfo-three adamantane compound; Choose m/z=136,135,149,163,177 and 191 as the characteristic ion peak of single adamantane compound.
5. height according to claim 1 ripe white oil oil sources defining method, wherein, methylation reaction described in step (2) uses iodomethane and silver tetrafluoroborate to process;
Preferably, the step using iodomethane and silver tetrafluoroborate to carry out processing comprises:
Oil sample is dissolved in methylene chloride, adds silver tetrafluoroborate and iodomethane reaction, after reaction terminates, cross the silver iodide precipitation filtered in reactant liquor, then remove methylene chloride and obtain grease; In grease, add normal hexane, through concussion cooling, be separated and obtain sulfonium salt precipitation.
6. height according to claim 1 ripe white oil oil sources defining method wherein, in step (2) during removing thiophenes, is that isolated sulfonium salt and 7-azaindole are reacted, thus by the thiophenes removing in sulfonium salt;
Preferably, isolated sulfonium salt and 7-azaindole are reacted, thus the step of the thiophenes removing in sulfonium salt are comprised:
Be dissolved in by sulfonium salt in acetonitrile, add the reaction of 7-azaindole, reaction terminates rear normal hexane and carries out extraction separatory, and the thiophenes in sulfonium salt is dissolved in normal hexane and is removed, and other sulfonium salts substances are retained in acetonitrile phase.
7. height according to claim 6 ripe white oil oil sources defining method, wherein, in step (2) during removing thio-ether type compounds, is that other sulfonium salts substances described and DMAP are reacted, thus removing thio-ether type compounds;
Preferably, other sulfonium salt materials and DMAP are reacted, thus the step of removing thio-ether type compounds comprises:
By other sulfonium salt class substance dissolves in acetonitrile, add DMAP, react under counterflow condition, add watery hydrochloric acid after reaction terminates, then use n-hexane extraction separatory; Through extraction separatory, thio-ether type compounds is dissolved in normal hexane and is removed mutually, sulfo-adamantane compound remain in acetonitrile-water mutually in, by acetonitrile-water mutually in solvent removing namely obtain the sulfo-adamantane compound of enrichment.
8. height according to claim 1-7 any one ripe white oil oil sources defining method, wherein, the method also comprises the checking sulfo-adamantane compound whether successful step of separation and concentration, and this step comprises:
The sulfo-adamantane compound of isolated thiophenes and thio-ether type compounds, enrichment is detected, to demonstrate the whether separation and concentration success of sulfo-adamantane compound.
9. height according to claim 8 ripe white oil oil sources defining method, wherein, in the successful step of checking sulfo-adamantane compound separation enrichment,
Respectively sulphur Mass Spectrometer Method and/or Gc-ms are carried out to isolated thiophenes and thio-ether type compounds; Positive ionization electrospray-Fourier transform-Ion cyclotron Resonance Mass Spectrometry analysis is carried out to the sulfo-adamantane compound of enrichment.
10. height according to claim 8 ripe white oil oil sources defining method, wherein, in the successful step of checking sulfo-adamantane compound separation enrichment, also comprise the operation first isolated thiophenes and thio-ether type compounds being carried out to column chromatographic isolation and purification before analysis.
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