CN102455317A - Micro component laser ablation isotope analyzing device and method - Google Patents
Micro component laser ablation isotope analyzing device and method Download PDFInfo
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- CN102455317A CN102455317A CN201010521367XA CN201010521367A CN102455317A CN 102455317 A CN102455317 A CN 102455317A CN 201010521367X A CN201010521367X A CN 201010521367XA CN 201010521367 A CN201010521367 A CN 201010521367A CN 102455317 A CN102455317 A CN 102455317A
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Abstract
The invention provides a micro component laser ablation isotope analyzing device and a micro component laser ablation isotope analyzing method, and belongs to the field of analysis of organic components of measured rock samples. The device comprises a laser device, a microscope, a sample cell, a high-temperature oxidation furnace, a cold trap, an isotope mass spectrometer and the like. Organic micro components in the sample cell are observed and found under the microscope and gasified and released by laser ablation, the released organic components are oxidized into carbon dioxide and water through the high-temperature oxidation furnace, the carbon dioxide is enriched in the cold trap, the carrier gas carrying the carbon dioxide enters the isotope mass spectrometer and is detected and analyzed, and the isotope values of the micro components of various organic substances are determined. By using the device, mixing of different rock component isotopes is effectively avoided, the geologic interpretation precision is improved, more targeted organic geochemical information is provided, and the oil-gas geological exploration is better served.
Description
Technical field
The invention belongs to and measure rock sample organic principle analysis field, be specifically related to a kind of micropetrological unit laser ablation isotope analysis device and method.
Background technology
Organic composition is widely used in the research field of oil organic geochemistry in the rock sample; From analytic target, can be divided into three kinds: soluble fraction (extract), insoluble part (kerogen) and total rock analysis (like pyrolysis analysis, isotope analysis etc.), these organic geochemistry application analysis methods can provide the molecular composition data of organic fossil (for example coal, hydrocarbon source rock, resinous shale and kerogen etc.).Specific as follows:
1; The constituent analysis of rock soluble fraction is for extracting obtained bitumen A through polar solvent (like chloroform etc.) after the large rock mass sample was pulverized, and bitumen A can be passed through column chromatography (filler is generally silica gel/aluminium oxide) and is separated into and respectively organize cut (stable hydrocarbon, aromatic hydrocarbons, nonhydrocarbon and bituminous matter).The rock soluble fraction of analysis just formed to(for) the composition or the isotope analysis of stable hydrocarbon, aromatic hydrocarbons, nonhydrocarbon, bituminous matter and bitumen A;
2, the insoluble part of rock generally is meant kerogen, i.e. the organic solvent that is insoluble to that extracting residue later obtains after pickling can not be by that part of organism of inorganic acid solution.Generally it is mainly carried out isotope and ultimate analysis;
3, the total rock analysis is meant that the large rock mass sample directly carries out pyrolysis or isotope analysis after pulverizing mixes.
More than these analytical approachs all be the rock sample to bulk, its result can not explain these materials and micro-information relevant and/or that originate unusually, reflection be the mean value of different component wherein.It then is through different organic matter in the rock of microscope location that micro laser degrades analysis, through laser ablation and component enrichment, transmission system component is imported analyzer, realizes the constituent analysis of micropetrological unit.Utilize manual selecting to be used for the different component enrichment with physical separation method such as density gravity centrifuging.Yet the problem that this method exists is very big for difficult realization of the hand picking of organic micropetrological unit and labour intensity generally speaking, and the enriched composition that centrifugal separation method obtains, its composition is suspectable.
Through Chinese patent Information Network, United States Patent (USP) library searching net, World Intellectual Property Organization WIPO net and CNKI periodical net the apparatus and method of relevant organic matter and micropetrological unit analysis are retrieved; Retrieve 1 in related patent U.S. Patent No. device, 5 of analytical technologies; Be respectively: 1, application (patent) number is 200310122849 a kind of macerals change in fluorescence and application thereof; 2, FAMM (variation of polycomponent microscopic fluorescence) technology and progress of application thereof; 3, laser Raman spectroscopy is analyzed multiple micropetrological unit change in fluorescence and application thereof; 4, the simple analysis of different component hydrocarbon source rock stone hydrocarbon dynamics; 5, coal seam micropetrological unit alkane series compound Geochemical Characteristics in the thermal simulation experiment; 6, the research and development of maceral isolation technics and application thereof.Can find out that through comparative studies said apparatus and method all can't carry out isotopic mensuration of organic micropetrological unit and analysis.
Summary of the invention
The objective of the invention is to solve a difficult problem that exists in the above-mentioned prior art, a kind of micropetrological unit laser ablation isotope analysis device and method is provided, organic micropetrological units different in the rock sample is carried out the laser ablation isotope analysis respectively.
The present invention realizes through following technical scheme:
A kind of micropetrological unit laser ablation isotope analysis device is characterized in that: said micropetrological unit laser ablation isotope analysis device comprises that micro laser degrades system, oxidation enrichment system and analytic system;
The said micro laser system of degrading comprises laser instrument, microscope and sample cell; Said laser instrument and said microscope are assembled on the same table top, and the laser beam that said laser instrument produces is refracted on the microscopical sample stage through said microscopical light path adjustment refracting telescope; Said sample cell places on the said sample stage, and said sample cell is provided with air intake opening and exhausr port;
Said oxidation enrichment system comprise injector, enrichment with carrier gas device, oxidation unit, sample introduction with carrier gas device and enricher; Said enrichment comprises that with carrier gas device enrichment uses carrier gas source, and said enrichment is connected with the air intake opening of said sample cell through pipeline with carrier gas source; Said oxidation unit is the high-temperature oxydation stove, and the entrance point of said high-temperature oxydation stove is connected with the exhausr port of said sample cell through pipeline, and endpiece is connected with said injector; Said sample introduction comprises that with carrier gas device sample introduction uses carrier gas source, and said sample introduction is connected with said injector through pipeline with carrier gas source; Said enricher adopts cold-trap, and said cold-trap is connected with said injector;
Said analytic system adopts isotope mass spectrometer;
Said micro laser degrades system and is communicated with said oxidation enrichment system, and the oxidation enrichment system is communicated with isotope mass spectrometer again; Sample degrades in the system at said micro laser and is degraded; The gaseous state organic component that produces gets into the oxidation enrichment system; The carbon dioxide that after reaction, generates gets into and carries out on-line analysis in the isotope mass spectrometer, thereby confirms the isotope value of various organic micropetrological units.
Specifically, a flowrate control valve and a threeway are housed in said enrichment successively in the pipeline between the air intake opening of carrier gas source and sample cell; Said enrichment is adopted helium with carrier gas source and sample introduction with carrier gas source.
Said enricher comprises two cold-traps, is respectively one-level cold-trap and secondary cold-trap; The two ends of one-level cold-trap are connected with injector, and an end of secondary cold-trap is connected with injector, and the other end links to each other with isotope mass spectrometer.
Said injector adopts six-way valve, and its six interfaces communicate in twos; Five interfaces of said six-way valve are connected with carrier gas source with the endpiece of said high-temperature oxydation stove, the two ends of one-level cold-trap, an end and the sample introduction of secondary cold-trap respectively, and the 6th interface is gas discharge outlet; Said six-way valve has enrichment and sample introduction two states.
Said sample cell comprises the pond body and covers the cover plate at Chi Tishang;
On said cover plate, have vertical through-via (being used for printing opacity observes), on the body of said pond, have vertical pond body opening, said vertical through-via and said pond body opening connect, and sample is placed in the body opening of described pond; O type circle (sealing) is equipped with on the top of body opening in said pond, and quartz glass plate (let light transmission, can observation sample, quartzy material can let laser see through and sample effect) is housed above said O type circle; The edge of said quartz glass plate is covered by said cover plate;
In the body of said pond, have carrier gas passage on the direction vertical with said pond body opening, said carrier gas passage and pond body opening connect, and pass whole pond body, and the two ends of said carrier gas passage are connected to a cutting ferrule joint respectively, form described air intake opening and exhausr port;
Said cover plate is fixed on Chi Tishang through set bolt.
Use a kind of analytical approach of described micropetrological unit laser ablation isotope analysis device, said method comprises:
(1) laser ablation step is used for organic matter is carried out laser ablation;
(2) oxidation enriching step is used for oxidation and enrichment organic matter fraction;
(3) analytical procedure is used for organic matter fraction is carried out mass spectrophotometry, confirms the isotope of organic matter fraction.
Wherein, said (1) laser ablation step comprises:
(11) state that injector is set is an enrichment state, and sample is carried out decontamination handle;
(12) confirm to reach positioning step, sample is placed in the sample cell, confirm component to be measured and location through microscopic examination;
(13) degrade step, utilize high energy laser to degrade sample, generate the gaseous state organic component; Said (2) oxidation enriching step comprises:
(21) oxidation step, carrier gas is brought the gaseous state organic component that said step (13) generates into the high-temperature oxydation stove, and the gaseous state organic component is oxidized to carbon dioxide;
(22) one-level enriching step, carrier gas are brought the carbon dioxide that generates in the step (21) into enricher and are carried out enrichment;
(23) state with injector switches to the sample introduction state;
(24) secondary enriching step, carbon dioxide carries out enrichment once more in enricher; Said (3) analytical procedure: carry out on-line analysis in the carbon dioxide entering isotope mass spectrometer through step (2) enrichment, thereby confirm the isotope value of various organic micropetrological units.
Compared with prior art; The invention has the beneficial effects as follows, realized the breakthrough of organic component constituent analysis technology, laser ablation system and isotope analysis system have been carried out type selecting and assembling; Developed sample cell and whole enrichment transmission system has been designed; Developed organic matter fraction laser ablation isotope analysis (La-IRMS) technology, really realized the independent studies of organic micropetrological unit constituent analysis, its GEOLOGICAL APPLICATION has been worth has obtained breakthrough lifting; Having avoided the isotopic mixing of different rock constituents effectively, improved the geologic interpretation precision, organic geochemistry information more targetedly is provided, is the petroleum and gas geology and exploration service better.
Description of drawings
Fig. 1-the 1st, micropetrological unit laser ablation isotope analysis device synoptic diagram of the present invention, wherein the state of injector is an enrichment state.
Fig. 1-2 is a micropetrological unit laser ablation isotope analysis device synoptic diagram of the present invention, and wherein the state of injector is the sample introduction state.
Fig. 2 is laser instrument and microscope integrate body schematic diagram.
Fig. 3 is the sample pool structure figure in the micropetrological unit laser ablation isotope analysis device of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
The present invention mainly is to different organic micropetrological unit laser ablation isotope analysis in the rock sample and the analysis of design device.As shown in Figure 1, this analytical equipment comprises that micro laser degrades system, oxidation enrichment system and analytical equipment.
The micro laser system of degrading comprises laser instrument 101, microscope 102 and special-purpose sample cell 103.According to the research needs; At Olympus microscope 102 (the BX51 type microscope of Olympus Corp; Performance requirement be for can carry out Halogen lamp LED white light and mercury lamp Fluirescence observation, and has been equipped with the special-purpose laser camera lens that is suitable for laser ablation) on assemble laser instrument 101.Laser instrument 101 is Geolas Pro quasi-molecule gas laser (the relevant company (Coherent) of Germany produces, and performance requirement is that maximum laser power reaches 200mJ, and optical maser wavelength is 193nm, and the I of laser beam spot reaches 4um).On Olympus microscope 101, be furnished with mercury lamp and transmitted light system, can observe the various organic micropetrological unit in the rock mating plate, the ccd image system of microscope 101 is convenient to the researchist and carries out image observation and measuring point location on computers.
Fig. 2 is quasi-molecule gas laser and the microscopical integrate body synoptic diagram of a 193nm, three-dimensional controlled the moving of sample stage, and sample cell places on the sample stage.The principle of work of laser instrument and microscope integrate body is following: the laser that laser excitation device 201 produces is mapped on first light path adjustment refracting telescope 214 after through safety shutter 202; And be mapped on second light path adjustment refracting telescope 214 after changing energy in the change direction entering attenuator 203, and be mapped on the beam separation mirror 215 through prism 204 and photomultiplier cell 205.Laser is assigned on the energy detector 210 at beam separation mirror 215 last branches; 210 detect behind the laser energy transmission signals gives SM1E attenuation controller 211; By SM1E attenuation controller 211 control attenuators 203; And then change the energy of attenuator 203 output laser, and change laser behind the energy by attenuator 203 and inject to and repeat this energy behind second light path adjustment refracting telescope 214 always and detect the Control Circulation process again, remain laser energy and satisfy job requirement; After another road laser on the beam separation mirror 215 focuses on through laser condensing lens 206; Be mapped on the 3rd light path adjustment refracting telescope 214 through laser spot size converter 213, and the change direction is carried out laser ablation through schwarzschild laser camera lens 207 backs to sample 208.The laser that differs in size is arranged through the hole on the laser spot size converter 213, be 80um to the maximum, minimum is 4um, can select laser spot size as required flexibly.Microscopical three-dimensional platform 209 is used to adjust the position of sample under object lens and is beneficial to observe and laser ablation, and microscopical ccd video camera 212 can realize that sample degrades the online in real time observation of process.
After the pith of organic micropetrological unit laser ablation isotope analysis system is the laser ablation organic matter, to the high efficiency of transmission of organic matter and to the enrichment of the carbon dioxide after the oxidation.
Said oxidation enrichment system comprise injector, enrichment with carrier gas device, oxidation unit, sample introduction with carrier gas device and enricher.Wherein injector adopts six-way valve 108, and it has enrichment and two states of sample introduction.Six-way valve 108 has six interfaces of A-F, and these six interfaces communicate in twos.
Shown in Fig. 1-1, under enrichment state, B-C; D-E; F-A communicates, and carrier gas 104 gets into six-way valve through sample cell 103 and high-temperature oxydation stove 107 from the A interface, and flows out six-way valve entering one-level cold-trap 109 through F interface; The other end by one-level cold-trap 109 gets into six-way valve through C interface again, and discharges through B interface; Carrier gas 111 gets into six-way valve through D interface; And (effect of carrier gas 111 under enrichment state provides inert gas and flows in the isotope mass spectrometer 112, because isotope mass spectrometer 112 needs inert gas protection to flow out six-way valve entering secondary cold-trap 110 through E interface.)。
Rotate six-way valve 108 to the sample introduction state, at this moment, shown in Fig. 1-2; A-B, C-D, E-F then change communicating state over to; Carrier gas 104 gets into six-way valve through sample cell 103 and high-temperature oxydation stove 107 from the A interface, and (under the sample introduction state, carrier gas 104 has gas to flow out equally from the B interface discharge; This carrier gas high-temperature oxydation stove 107 back of flowing through gets into six-way valves, through six-way valve emptying, plays the effect of protection high-temperature oxydation stove 107); Carrier gas 111 then gets into six-way valve from D interface; And from C interface outflow six-way valve entering one-level cold-trap 109; And bring the carbon dioxide of the enrichment in the one-level cold-trap 109 into F interface; And flow out six-way valve from the E interface of six-way valve and get into secondary cold-trap 110, from secondary cold-trap 110, flow out again and get into isotope mass spectrometer 112, obtain analysis result at last.
A flowrate control valve 105 and a threeway 106 are housed in said enrichment successively in the pipeline between the air intake opening of carrier gas source 104 and sample cell 103.A connection traffic operation valve 105 of threeway 106; The other end connects the air intake opening of sample cell; The 3rd interface seals with dottle pin; Can carry out the injection of gaseous sample, its result and gaseous sample are directly compared with the result that the analysis of isotope appearance obtains, can analyze the isotope of component exactly to confirm this system.
It is the mass spectrometer of Thermo Delta V Advantage that said isotope mass spectrometer 112 adopts model; The instrumental analysis parameter is: the Nier ion gun, and mass number scope 1-96, detection mode is that Faraday cup receives more; Electronic capability is 120eV; Accelerating field is 3000V, and transmitter current is 1.5mA, and dynamic vacuum continuous flow mode dynamic vacuum is 7.2 * 10
-7Mba.
Said sample cell be the micro laser key component that degrades system also be the ingredient of oxidation enrichment system simultaneously, it is important parameter that its laser sees through efficient, heating temperature and dead volume.Sample cell of the present invention adopts the design of loculus volume, can integral body be heated to 100 ℃, and accuracy of temperature control is 1 ℃, and transparent glass is highly purified quartz glass.Concrete sample pool structure is as shown in Figure 3, and said sample cell comprises pond body 307 and covers the cover plate 305 on pond body 307; On said pond body 307, have vertical pond body opening (shape of cross section can be designed to circle or other shape) having vertical through-via (can be designed to infundibulate or other shape) on the said cover plate 305; Said vertical through-via and said pond body opening connect, and sample is placed in the body opening of described pond; O type circle 304 (sealing) is equipped with on the top of body opening in said pond, and quartz glass plate 303 (let light transmission, can observation sample, quartzy material can let laser see through and sample effect) is housed above said O type circle 304; The edge of said quartz glass plate 303 is covered by said cover plate 305;
In said pond body 307, have carrier gas passage 308 on the direction vertical with said pond body opening; Said carrier gas passage 308 connects with the pond body opening; And pass whole pond body 307; The two ends of said carrier gas passage 308 are connected to a cutting ferrule joint respectively, and an end that connects cutting ferrule joint 301 forms described air intake opening, and an end that connects cutting ferrule joint 306 forms described exhausr port;
Said cover plate 305 is fixed on Chi Tishang through set bolt 302.
The pipeline that is connected with sample cell adopts 1/16 inch metal pipe line, and it can remain on 300 ℃ in whole experiment, and accuracy of temperature control is 1 ℃; The organic matter that degrades is oxidized to carbon dioxide and water through high-temperature oxydation stove 107, analyzes through getting into isotope mass spectrometer 112 after two cold-traps (109,110) enrichment, and cold-trap carries out enrichment through the principle that stainless-steel tube immerses liquid nitrogen to carbon dioxide.Sample all will carry out decontamination before degrading handles.
The method of application of apparatus of the present invention is: at first under enrichment state (shown in Fig. 1-1); Sample (rock mating plate etc.) is positioned in the special sample cell 103; Observe for 102 times, select suitable organic micropetrological unit at microscope again, each measuring point that needs are degraded moves to ken center successively; Open laser instrument 101, the laser work condition is set, component is carried out laser ablation; Organic component receives degrading of PRK and can stay and degrade vestige, and makes and the organic component gasification of laser contact part, imports high-temperature oxydation stove 107 by carrier gas and carries out oxidation and be formed into carbon dioxide and water, and bring 109 enrichments of one-level cold-trap into by carrier gas.Then; Switch to sample introduction state (shown in Fig. 1-2); One-level cold-trap 109 is heated to room temperature, with the online mode gradation carbon dioxide in the one-level cold-trap 109 is imported in the secondary cold-trap 110 and carries out enrichment once more, and the impurity such as water that oxidation forms are then stayed in the one-level cold-trap 109.At last, cold-trap 2 is heated to room temperature, through carrier gas the carbon dioxide in the secondary cold-trap 110 is imported isotope mass spectrometer 112 and analyzes, thereby obtain the carbon isotope value of the organic micropetrological unit of various differences.
Through experiment, device of the present invention has all been obtained effect preferably in the analysis experiment to several samples such as solid bitumen, methane standard specimen, black mud stone.
Technique scheme is one embodiment of the present invention; For those skilled in the art; On the basis that the invention discloses application process and principle, be easy to make various types of improvement or distortion, and be not limited only to the described method of the above-mentioned embodiment of the present invention; Therefore the mode of front description is preferably, and does not have restrictive meaning.
Claims (7)
1. micropetrological unit laser ablation isotope analysis device, it is characterized in that: said micropetrological unit laser ablation isotope analysis device comprises that micro laser degrades system, oxidation enrichment system and analytic system;
The said micro laser system of degrading comprises laser instrument, microscope and sample cell; Said laser instrument and said microscope are assembled on the same table top, and the laser beam that said laser instrument produces is refracted on the microscopical sample stage through said microscopical light path adjustment refracting telescope; Said sample cell places on the said sample stage, and said sample cell is provided with air intake opening and exhausr port;
Said oxidation enrichment system comprise injector, enrichment with carrier gas device, oxidation unit, sample introduction with carrier gas device and enricher; Said enrichment comprises that with carrier gas device enrichment uses carrier gas source, and said enrichment is connected with the air intake opening of said sample cell through pipeline with carrier gas source; Said oxidation unit is the high-temperature oxydation stove, and the entrance point of said high-temperature oxydation stove is connected with the exhausr port of said sample cell through pipeline, and endpiece is connected with said injector; Said sample introduction comprises that with carrier gas device sample introduction uses carrier gas source, and said sample introduction is connected with said injector through pipeline with carrier gas source; Said enricher adopts cold-trap, and said cold-trap is connected with said injector;
Said analytic system adopts isotope mass spectrometer;
Said micro laser degrades system and is communicated with said oxidation enrichment system, and the oxidation enrichment system is communicated with isotope mass spectrometer again; Sample degrades in the system at said micro laser and is degraded; The gaseous state organic component that produces gets into the oxidation enrichment system; The carbon dioxide that after reaction, generates gets into and carries out on-line analysis in the isotope mass spectrometer, thereby confirms the isotope value of various organic micropetrological units.
2. micropetrological unit laser ablation isotope analysis device according to claim 1 is characterized in that: a flowrate control valve and a threeway are housed in said enrichment successively in the pipeline between the air intake opening of carrier gas source and sample cell; Said enrichment is all adopted helium with carrier gas source and sample introduction with carrier gas source.
3. micropetrological unit laser ablation isotope analysis device according to claim 1, it is characterized in that: said enricher comprises two cold-traps, is respectively one-level cold-trap and secondary cold-trap; The two ends of one-level cold-trap are connected with injector, and an end of secondary cold-trap is connected with injector, and the other end links to each other with isotope mass spectrometer.
4. micropetrological unit laser ablation isotope analysis device according to claim 3 is characterized in that: said injector adopts six-way valve, and its six interfaces communicate in twos; Five interfaces of said six-way valve are connected with carrier gas source with the endpiece of said high-temperature oxydation stove, the two ends of one-level cold-trap, an end and the sample introduction of secondary cold-trap respectively, and the 6th interface is gas discharge outlet; Said six-way valve has enrichment and sample introduction two states.
5. according to the described micropetrological unit laser ablation of one of claim 1 to 4 isotope analysis device, it is characterized in that:
Said sample cell comprises the pond body and covers the cover plate at Chi Tishang;
On said cover plate, have vertical through-via, on the body of said pond, have vertical pond body opening, said vertical through-via and said pond body opening connect, and sample is placed in the body opening of described pond; O type circle is equipped with on the top of body opening in said pond, above said O type circle, quartz glass plate is housed; The edge of said quartz glass plate is covered by said cover plate;
In the body of said pond, have carrier gas passage on the direction vertical with said pond body opening, said carrier gas passage and pond body opening connect, and pass whole pond body, and the two ends of said carrier gas passage are connected to a cutting ferrule joint respectively, form described air intake opening and exhausr port;
Said cover plate is fixed on Chi Tishang through set bolt.
6. application rights requires a kind of analytical approach of one of 1 to 4 described micropetrological unit laser ablation isotope analysis device, and it is characterized in that: said method comprises:
(1) laser ablation step is used for organic matter is carried out laser ablation;
(2) oxidation enriching step is used for oxidation and enrichment organic matter fraction;
(3) analytical procedure is used for organic matter fraction is carried out mass spectrophotometry, confirms the isotope of organic matter fraction.
7. analytical approach according to claim 6 is characterized in that: wherein, said (1) laser ablation step comprises:
(11) state that injector is set is an enrichment state, and sample is carried out decontamination handle;
(12) confirm to reach positioning step, sample is placed in the sample cell, confirm component to be measured and location through microscopic examination;
(13) degrade step, utilize high energy laser to degrade sample, generate the gaseous state organic component; Said (2) oxidation enriching step comprises:
(21) oxidation step, carrier gas is brought the gaseous state organic component that said step (13) generates into the high-temperature oxydation stove, and the gaseous state organic component is oxidized to carbon dioxide;
(22) one-level enriching step, carrier gas are brought the carbon dioxide that generates in the step (21) into enricher and are carried out enrichment;
(23) state with injector switches to the sample introduction state;
(24) secondary enriching step, carbon dioxide carries out enrichment once more in enricher; Said (3) analytical procedure: carry out on-line analysis in the carbon dioxide entering isotope mass spectrometer through step (2) enrichment, thereby confirm the isotope value of various organic micropetrological units.
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