CN102053125A - System and method for analyzing polycyclic terpane in petroleum geological sample - Google Patents
System and method for analyzing polycyclic terpane in petroleum geological sample Download PDFInfo
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Abstract
The invention discloses a system and a method for analyzing polycyclic terpane in a petroleum geological sample. The system comprises a central processing unit, a mass spectrograph and a chromatograph, wherein the central processing unit is connected with the chromatograph through the mass spectrograph; the chromatograph comprises a vaporizing chamber and two chromatographic columns with different polarities; the sample enters the two chromatographic columns in turn for separation after passing through the vaporizing chamber in the chromatograph; each separated component substance enters the mass spectrograph in turn to form fragment ions; and the central processing unit qualitatively and quantitatively analyzes the component according to the distribution characteristic of the fragment ions and forms a chromatographic mass spectrum image. In the system and the method, by preferably and effectively combining the two chromatographic columns with different polarities, tricyclic terpenoids, tetracyclic terpenoids and pentacyclic terpenoids in saturated hydrocarbon component of crude oil or rock extract are effectively separated and qualitatively and quantitatively analyzed on the basis of optimized modulation period and analysis conditions.
Description
Technical field
The invention belongs to the field of in the petroleum prospecting geology Earth Information being analyzed, relate in particular to a kind of system and method that separates material in crude oil or the rock sample of measuring.
Background technology
Terpenoid is to be distributed widely in the big class organic compound of one in plant, insect and the microbial body, and it is that (its general formula is (C for the oligomer of isoprene (hemiterpene)
5H
8) n, n=2-8) and their derivant.So far detected a large amount of biolipid based composition matter in sediment and the oil, from their formation and content distribution feature, its topmost type is a terpenoid, secondly is steroid.Terpenoid comprises monoterpenes, sesquiterpenoids and two, triterpenes etc., and wherein two cyclic terpenes and above terpene are referred to as many cyclic terpenoid compounds.
For the present comparatively common method of the analyzing and testing of terpenoid in the oil geology sample mainly is that the liquid chromatography of carrying out solvable organic matter is earlier separated, and then the saturated hydrocarbon fraction of enrichment carried out the chromatogram mass spectrum or the mass spectrophotometry of chromatogram mass spectrum detects, the detecting device that uses mainly is the MSD detecting device, and relatively Chang Yong technology generally all is to adopt the chromatograph mass spectrum analysis technology.Crude oil or rock sample are removed bituminous matter with polar solvent through depositing with normal hexane after the extracting earlier again, carry out column chromatography for separation after the filtration again, isolate stable hydrocarbon, aromatic hydrocarbons and non-hydrocarbon-fraction and collection respectively, to on the chromatogram mass spectrometer, analyzing behind the saturated hydrocarbon component solvent dilution, generally adopt the method for the mass chromatogram that extracts mass-to-charge ratio m/z191 to carry out qualitative and quantitative analysis for the analysis of many cyclic terpenoid compounds.
In the prior art, as shown in Figure 1, adopt general chromatogram mass-spectrometric technique method to carry out the analysis of many cyclic terpenoid compounds, terpenoids such as a lot of tricyclene compounds and five rings, Fourth Ring mix mutually in the mass chromatogram of the mass-to-charge ratio m/z191 of extraction.A lot of high carbon number tricyclene compounds (more than the C29) appearance times and four, five rings terpenoid overlaid, simultaneously again because its low-abundance cause, people are difficult to many cyclic terpenoid compounds are discerned and quantitative test exactly, many cyclic terpenes of part hydride compounds such as gammacerane are owing to can not separate fully, the quantitative test error is big, simultaneously, can not carry out accurately qualitatively, thereby can't obtain detailed geochemical information many cyclic terpenes of part alkane material because chromatogram flows out altogether.
Summary of the invention
The present invention is in order to solve the compartment analysis problem of many cyclic terpenoid compounds, and the inventor has adopted a kind of system and analytical approach thereof of analyzing many cyclic terpenes alkane in the oil geology sample through research for many years.Its two-dimentional stratographic analysis time mass spectrum technology on the basis of sample pre-treatments, by the configuration of chromatographic column and the optimization of analysis condition, has successfully realized the separation and the accurate qualitative and quantitative analysis of many cyclic terpenoid compounds.
Principle of the present invention adopts the comprehensive two dimensional gas chromatography isolation technics to adopt nonpolar (or low pole) capillary column (chromatographic column) to be in series by the capillary column (chromatographic column) of modulator and another root middle polarity (or polarity), modulator has freezing enrichment of secondary and analytical capabilities, when locating the first order and be in freezing state, its second level then is in pyrolysis and analyses state, and hocket, cooling time adds that the pyrolysis time of analysing is the general of modulation period.Crude oil sample enters modulator after through the separation of first post successively, in the general time of the modulation period that is provided with, analysed by freezing enrichment of one-level and one-level pyrolysis, entering freezing enrichment of secondary and secondary pyrolysis then in second half time analyses, enter next root capillary column at last and separate again, thereby fail the component of fine separation because the change of rear pillar post obtains good separating effect at front pillar like this.Because the front pillar component enters and is cut enrichment behind the modulator and enters rear pillar again and separate, thereby peak shape is sharp-pointed, the situation that the peak shape under the simply series connection condition broadens and trails can not occur, peak capacity is bigger, and the component after rear pillar separates enters time of-flight mass spectrometer successively and carries out Analysis and Identification.The mass analyzer of time of-flight mass spectrometer is an ion drift tube.By the fragmention of the isolated organic substance component of chromatographic column different mass-to-charge ratioes of generation under the ion gun bombardment, the ion of generation enters field-free drift tube after quickening, and flies to ion acceptor with constant speed.Mass of ion is big more, and it is long more to arrive the used time of receiver, and mass of ion is more little, and it is short more to arrive the used time of receiver, according to this principle, can separate the ion of different quality by m/z value size.The detectable molecular weight ranges of time of-flight mass spectrometer is big, and sweep velocity is fast, and apparatus structure is simple.For fear of the slightly difference of the ion with identical mass-to-charge ratio owing to zero energy when leaving ion gun, there is certain distribution the time that makes the ion with identical mass-to-charge ratio reach detecting device, cause resolution characteristic to descend, generally add one group of electrostatic field catoptron now in the linear detector front, roll back the ion in the free flight is counter, the ion that zero energy is big is because initial velocity is fast, enter the distance of electrostatic field catoptron, distance when returning is also just long, distance when the ion that zero energy is little returns is short, will focus at the certain position of backhaul like this, thereby improve the resolution characteristic of instrument.This time of-flight mass spectrometer that has the electrostatic field catoptron is called as reflection type flight time mass spectrometer.It is detected that the fragmention of different mass-to-charge ratioes focuses on the back, and CPU (central processing unit) is carried out same composition the merger processing again according to the mass spectrum qualification result, provides corresponding component area and 2D collection of illustrative plates and 3D rendering.
The present invention is in order to realize the foregoing invention purpose, and the technical scheme that is adopted is as follows,
A kind of system that analyzes many cyclic terpenes alkane in the oil geology sample, described system comprises CPU (central processing unit), mass spectrometer and chromatograph; Described CPU (central processing unit) is connected with chromatograph by described mass spectrometer; Described chromatograph comprises two chromatographic columns that vaporizer is different with polarity;
Sample separates through entering two chromatographic columns successively after the vaporizer vaporization in the described chromatograph; Separated each component materials enters described mass spectrometer successively, forms fragmention; Described CPU (central processing unit) is carried out qualitative and quantitative analysis according to the fragmention distribution characteristics to component, and forms chromatogram mass spectrogram picture.
Described chromatograph also comprises a modulator; Described modulator is arranged in the middle of the different chromatographic column of described two polarity; Described vaporizer is connected with chromatographic column A; Described modulator comprises freezing enriching apparatus and air thermal dissociation analysis apparatus, and sample enters in the described modulator successively the branch two-stage and hockets freezing and pyrolysis is analysed, and enters after the parsing among the chromatographic column B; Described chromatographic column A is nonpolar chromatographic column; Described chromatographic column B is the polarity chromatographic column.
Sample enters chromatographic column A successively after the vaporization of described vaporizer separates, and the back enters chromatographic column B by modulator separates once more, after enter described mass spectrometer.
Described mass spectrometer is time of-flight mass spectrometer or reflection type flight time mass spectrometer; Proton analyzer in the described time of-flight mass spectrometer is an ion drift tube; By the fragmention of the isolated organic substance component of described chromatographic column B different mass-to-charge ratioes of generation under the ion gun bombardment, the fragmention of generation enters ion drift tube after quickening, and flies to ion acceptor and measures.Chromatographic column B endpiece directly enters the mass spectrometer ionization chamber by transmission line in the chromatograph, be subjected to producing after the electron bombard of certain energy the different fragmentions of reflection self structure and content information at the mass spectrometer ionization chamber by the isolated organic substance of chromatographic column B, these ions obtain kinetic energy under accelerating potential V effect, its movement velocity v, mass of ion m and ion accelerating voltage V have following formula relation, i.e. E=eV=mv
2, v=(eV/m)
1/2If the length of ion drift tube is L, then be t the drift time of fragmention, t=L/v, t=L (m/eV)
1/2, t=km
1/2Under the condition of energy, drift tube length unanimity, k is a constant, and fragmention flight time t is only relevant with mass of ion.For the identical ion of energy, the quality of ion is big more, and the time that arrives ion acceptor is long more, and quality is more little, and the used time is short more, utilizes this principle, can be the ion of different quality separately; The organic matter of while different content, the number of ions that each that is produced after its ionization is relevant is also inequality, detected signal intensity is also just different on ion acceptor, therefore just can come organic substance is carried out qualitative and quantitative analysis according to ion characteristic and ionic strength.
At freezing enriching apparatus described in the concrete application is liquid nitrogen spray device for cooling;
Described chromatographic column A is 30m * 0.25mm * 0.25umHP5-MS post;
Described chromatographic column B is 2.5m * 0.10mm * 0.10umDB-17HT post.
The present invention, described sample carries out pre-service earlier before analysis: precipitation bitumens matter, column chromatography for separation, aromatics separation component and saturated hydrocarbon component process.
The present invention also comprises a kind of method of analyzing many cyclic terpenes alkane in the oil geology sample,
1.. the sample pretreatment step takes by weighing 20-40mg crude oil sample or rock extractable bitumen sample and carries out family's component separation, to obtain stable hydrocarbon and aromatic fraction;
Described sample pretreatment step comprises,
I. precipitation bitumens matter process,
The chromatographically pure methylene chloride of getting 1-2ml dissolves whole crude oil or extract, and the heavily steaming n-pentane of adding 25ml is with precipitation bitumens matter, be transferred to the 50ml round-bottomed flask with vacuum filtration, the suction filtration device is a glass fiber filter paper, clean sediment 2-3 time in the flask and suction filtration cleaning solvent with the 5ml n-pentane; Sediment with on the n-pentane cleaning filter paper is filtered to guarantee all n-pentane soluble substances; The filtrate rotary evaporation is extremely done;
Ii. column chromatography for separation aromatic component process,
The 28-200 order silica gel of percentage by weight 25% added 75% 80-200 order aluminium oxide 100 ℃ of following activation processing 24 hours, the sealing of cooling back preserves that to do inserts stand-by;
Handling back extract weight according to deasphalting matter needs the standard of 1g inserts to get quantitative silica gel and aluminium oxide mixing inserts by every 10mg deasphalting matter extract, after chromatographic column bottom is loaded onto the thick silica sand of the glass wool handled and one deck 1cm earlier, stir evenly filler and the pillar of packing into n-pentane again, pat shaft and drive bubble away and filler is enriched; Bleed off n-pentane in the pillar, just cover filler up to liquid level;
Iii. stable hydrocarbon detachment process
Carry out the separation of saturated hydrocarbon component: with the deasphalting quality sample with measured above very a spot of nC
5Dissolving, and pour in the chromatographic column; Use nC
5The cleaning flask is also poured in the post; Open the post switch, flow out all nC
5Just cover filler up to liquid level; Weighing was to be analyzed after effluent was accepted back low temperature solvent flashing.
Solvent wherein and consumption be,
Solvent is attached most importance to and is steamed n-pentane, methyl alcohol and methenyl choloride; Solvent load is decided according to filler weight, and its consumption standard is for being: 3.5ml heavily steams n-pentane (/g filler); The 4ml volume ratio is 1: 1 nC
5/ CH
2Cl
2(/g filler); 4ml heavily steams CH
3OH (/g filler); 4ml heavily steams CHCl
3(/g filler).
2.. the sample analysis step, get certain dilute sample with microsyringe and be injected in the described system in the chromatograph vaporizer, and start-up routine carries out two-dimentional chromatogram flying time mass spectrum analysis;
3.. sample result output, CPU (central processing unit) is carried out qualitative and quantitative analysis according to the fragmention distribution characteristics of time of-flight mass spectrometer output to component, and forms chromatogram mass spectrogram picture.What the qualitative and quantitative analysis of many cyclic terpenes alkane extracted is the characteristic ion peak of mass-to-charge ratio m/z=191.Qualitative analysis is declared knowledge according to mass spectrogram feature, standard substance and documents and materials, and quantitative Analysis is that peak area with the characteristic ion peak of mass-to-charge ratio m/z=191 is a basis, and component concentration and component peaks area have linear relationship.
The present invention adopts stratographic analysis time mass spectrum technology, on the basis of sample pre-treatments, by the configuration of chromatographic column and the optimization of analysis condition, has successfully realized the separation and the accurate qualitative and quantitative analysis of many cyclic terpenoid compounds.Fig. 4 analyzes to finish the mass of ion chromatogram that m/z191 is extracted in the back, and Fig. 5 is high many cyclic terpenes of carbon number alkane partial enlarged drawing.As can be seen by two-dimentional stratographic analysis, separated well on chromatographic column B in terpene substances that can not fine separation on the chromatographic column A, tricyclene, Fourth Ring terpene and five rings terpenoid are distributed in different zones, can on one dimension retention time and two-dimentional retention time, distinguish the different terpenoid of identification at an easy rate, the tricyclene of the above carbon number of C29 also is easy to identification and quantitative, gammacerane also separates fully with other terpene substances, thereby quantitative test accurately and reliably.
Description of drawings
Fig. 1 is that chromatograph mass spectrum analysis mass-to-charge ratio 191 is extracted mass of ion chromatogram and mass spectrogram in the prior art;
Fig. 2 is the modular construction synoptic diagram of the present invention system of analyzing many cyclic terpenes alkane in the oil geology sample;
Fig. 3 is a comprehensive two dimensional gas chromatography flight time mass spectrum mapping process of the present invention;
Fig. 4 utilizes many cyclic terpenes hydride compounds m/z191 ion two dimension mass chromatogram behind the system and method for the present invention;
Fig. 5 utilizes many cyclic terpenes hydride compounds m/z191 ion two dimension mass chromatogram partial enlarged drawing behind the system and method for the present invention
More than each width of cloth accompanying drawing specifically in conjunction with background technology, effect and embodiment are illustrated.
Wherein, each pictorial representation among Fig. 2: 201-chromatograph; The 202-vaporizer; 203-chromatographic column A; The 204-modulator; The 205-liquid nitrogen; The 206-hot-air; 207-two-dimensional columns case; 208-chromatographic column B; The 209-time of-flight mass spectrometer; 210 CPU (central processing unit).
Embodiment
The present invention's two dimension chromatogram flight time mass spectrum is made up of three parts, comprise chromatograph 201, time of-flight mass spectrometer 209 and CPU (central processing unit) 210, on chromatograph 201, disposed the chromatographic column 203 and 208 of sample introduction vaporizer 202 and two opposed polarities, and modulator 204, utility appliance has liquid nitrogen spray device for cooling 205 and air thermal dissociation analysis apparatus 206.203 chromatographic column A are nonpolar chromatographic column 30m * 0.25mm * 0.25umHP5-MS post, and 208 chromatographic column B are polar column 2.5m * 0.10mm * 0.10umDB-17HT post.Sample enters chromatographic column 203 after vaporizer 202 vaporizations separates, be provided with after modulation period chromatographic column 203 being separated enter in the modulator 204 component successively the branch two-stage carry out freezing and pyrolysis is analysed, every grade of cooling time and the pyrolysis time of analysing are the general of modulation period, when the first order is in freezing state, the second level then is in pyrolysis and analyses state, and hocket, component after secondary is resolved enters chromatographic column 208 again and carries out secondary separation, thereby the opposed polarity compound that flows out altogether in chromatographic column 203 is like this entering chromatographic column 208 backs because the change of post reaches the purpose of separating fully.Each component materials that flows out from chromatographic column 208 enters time of-flight mass spectrometer 209 successively, under the ion gun bombardment, become the fragmention of different characteristic, fragmention arrives ion acceptor by drift tube and detects, working software carries out qualitative and quantitative analysis according to the fragmention distribution characteristics to component, and provides the 3D chromatogram mass spectrogram picture of amalyzing substances at last.
In force, the parameter taked of above-mentioned each device is
Embodiment
This laboratory sample is a S41 well crude oil, through two-dimentional chromatographic resolution analysis, can carry out qualitative and quantitative analysis to many cyclic terpenoid compounds well, do interior mark with four deuteriums for cholestane, the mass chromatogram that extracts mass-to-charge ratio m/z221 obtains interior mark peak area, the mass chromatogram that extracts mass-to-charge ratio m/z191 obtains the peak area of each many cyclic terpenoid compounds, calculate each components contents by Cx=Cs * Ax/As, Cx is the content of many cyclic terpenes class material x, Ax is the peak area of material x, the interior mark concentration of Cs for adding, As is interior mark peak area, the mass chromatogram of many cyclic terpenes alkane m/z191 is seen Fig. 4.
In sum; for the person of ordinary skill of the art; can make other various corresponding changes and distortion according to technical scheme of the present invention and technical conceive, and all these changes and distortion all should belong to the protection domain of claim of the present invention.
Claims (9)
1. system that analyzes many cyclic terpenes alkane in the oil geology sample, described system comprises CPU (central processing unit), mass spectrometer and chromatograph; It is characterized in that described CPU (central processing unit) is connected with chromatograph by described mass spectrometer; Described chromatograph comprises two chromatographic columns that vaporizer is different with polarity;
Sample separates through entering two chromatographic columns successively after the vaporizer vaporization in the described chromatograph; Separated each component materials enters described mass spectrometer successively, forms fragmention; Described CPU (central processing unit) is carried out qualitative and quantitative analysis according to the fragmention distribution characteristics to component, and forms chromatogram mass spectrogram picture.
2. a kind of system that analyzes many cyclic terpenes alkane in the oil geology sample according to claim 1 is characterized in that,
Described chromatograph also comprises a modulator; Described modulator is arranged in the middle of the different chromatographic column of described two polarity; Described vaporizer is connected with chromatographic column A;
Sample enters chromatographic column A successively after the vaporization of described vaporizer separates, the back by modulator through two-stage freezing with enter chromatographic column B after pyrolysis is analysed and separate once more, after enter described mass spectrometer.
3. a kind of system that analyzes many cyclic terpenes alkane in the oil geology sample according to claim 2 is characterized in that,
Described modulator comprises freezing enriching apparatus and air thermal dissociation analysis apparatus, and sample enters and carries out the freezing and pyrolysis of two-stage in the described modulator successively and analyse, and enters after the parsing among the chromatographic column B;
Described chromatographic column A is nonpolar chromatographic column; Described chromatographic column B is the polarity chromatographic column.
4. a kind of system that analyzes many cyclic terpenes alkane in the oil geology sample according to claim 3 is characterized in that,
Described freezing enriching apparatus is a liquid nitrogen spray device for cooling;
Described chromatographic column A is 30m * 0.25mm * 0.25umHP5-MS post;
Described chromatographic column B is 2.5m * 0.10mm * 0.10umDB-17HT post.
5. a kind of system that analyzes many cyclic terpenes alkane in the oil geology sample according to claim 1 and 2 is characterized in that,
Described mass spectrometer is time of-flight mass spectrometer or reflection type flight time mass spectrometer; Proton analyzer in the described time of-flight mass spectrometer is an ion drift tube; By the fragmention of the isolated organic substance component of described chromatographic column B different mass-to-charge ratioes of generation under the ion gun bombardment, the fragmention of generation enters ion drift tube after quickening, and flies to ion acceptor and measures.
6. a kind of system that analyzes many cyclic terpenes alkane in the oil geology sample according to claim 1 and 2 is characterized in that,
Described sample carries out pre-service earlier before analysis: precipitation bitumens matter, column chromatography for separation, aromatics separation component and saturated hydrocarbon component process.
7. use method, it is characterized in that according to many cyclic terpenes alkane in the described systematic analysis oil geology of the claim 1-6 sample,
Described method comprises,
1.. the sample pretreatment step takes by weighing 20-40mg crude oil sample or rock extractable bitumen sample and carries out family's component separation, to obtain stable hydrocarbon and aromatic fraction;
2.. the sample analysis step, get certain dilute sample with microsyringe and be injected in the described system in the chromatograph vaporizer, and start-up routine carries out two-dimentional chromatogram flying time mass spectrum analysis;
3.. sample result output, CPU (central processing unit) is carried out qualitative and quantitative analysis according to the fragmention distribution characteristics of time of-flight mass spectrometer output to component, and forms chromatogram mass spectrogram picture; What the qualitative and quantitative analysis of many cyclic terpenes alkane extracted is the characteristic ion peak of mass-to-charge ratio m/z=191; Qualitative analysis is declared knowledge according to mass spectrogram feature, standard substance and documents and materials, and quantitative Analysis is that peak area with the characteristic ion peak of mass-to-charge ratio m/z=191 is a basis, and component concentration and component peaks area have linear relationship.
8. the method for many cyclic terpenes alkane is characterized in that in the analysis oil geology sample according to claim 7, and described sample pretreatment step comprises,
I. precipitation bitumens matter process,
The chromatographically pure methylene chloride of getting 1-2ml dissolves whole crude oil or extract, and the heavily steaming n-pentane of adding 25ml is with precipitation bitumens matter, be transferred to the 50ml round-bottomed flask with vacuum filtration, the suction filtration device is a glass fiber filter paper, clean sediment 2-3 time in the flask and suction filtration cleaning solvent with the n-pentane of 5ml; Sediment with on the n-pentane cleaning filter paper is filtered to guarantee all n-pentane soluble substances; The filtrate rotary evaporation is extremely done;
Ii. column chromatography for separation aromatic component process,
The 28-200 order silica gel of percentage by weight 25% added 75% 80-200 order aluminium oxide 100 ℃ of following activation processing 24 hours, the sealing of cooling back preserves that to do inserts stand-by;
Handling back extract weight according to deasphalting matter needs the standard of 1g inserts to get quantitative silica gel and aluminium oxide mixing inserts by every 10mg deasphalting matter extract, after chromatographic column bottom is loaded onto the thick silica sand of the glass wool handled and one deck 1cm earlier, stir evenly filler and the pillar of packing into n-pentane again, pat shaft and drive bubble away and filler is enriched; Bleed off n-pentane in the pillar, just cover filler up to liquid level;
Iii. stable hydrocarbon detachment process
Carry out the separation of saturated hydrocarbon component: with the deasphalting quality sample with measured above very a spot of nC
5Dissolving, and pour in the chromatographic column; Use nC
5The cleaning flask is also poured in the post; Open the post switch, flow out all nC
5Just cover filler up to liquid level; Weighing was to be analyzed after effluent was accepted back low temperature solvent flashing.
9. the method for many cyclic terpenes alkane is characterized in that in the analysis oil geology sample according to claim 8, and solvent wherein and consumption be,
Solvent is attached most importance to and is steamed n-pentane, methyl alcohol and methenyl choloride; Solvent load is decided according to filler weight, and its consumption standard is for being: 3.5ml heavily steams n-pentane (/g filler); The 4ml volume ratio is 1: 1 nC
5/ CH
2Cl
2(/g filler); 4ml heavily steams CH
3OH (/g filler); 4ml heavily steams CHCl
3(/g filler).
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