CN103868783A - Thermal treatment method for inclusion chip applicable to micro laser raman analysis - Google Patents
Thermal treatment method for inclusion chip applicable to micro laser raman analysis Download PDFInfo
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- CN103868783A CN103868783A CN201410079649.7A CN201410079649A CN103868783A CN 103868783 A CN103868783 A CN 103868783A CN 201410079649 A CN201410079649 A CN 201410079649A CN 103868783 A CN103868783 A CN 103868783A
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Abstract
The invention discloses a thermal treatment method for an inclusion chip applicable to micro laser raman analysis. The method comprises the following steps: a, heating the inclusion chip and a glass slide, so that the inclusion chip is separated from the glass slide, and then soaking the inclusion chip into ethyl alcohol; and taking out and then wiping off organic gum on the surface of the inclusion chip by using the ethyl alcohol; b, carrying out petrography observation on the inclusion chip processed in the step a, dividing the inclusion type, and carrying out primary micro-thermometry research on the inclusion, and determining the lowest uniform temperature of the inclusion inside the inclusion chip; c, determining the thermal treatment temperature of the inclusion chip according to a primary micro-thermometry result, wherein the thermal treatment temperature of the inclusion chip is 40-80 DEG C lower than the lowest uniform temperature of the inclusion, and the thermal treatment temperature is not lower than 80 DEG C, and not higher than 150 DEG C; and d, heating the inclusion chip to the set thermal treatment temperature for 20 minutes on an electric heating plate, then slowly cooling to the room temperature, and then carrying out micro laser raman spectroscopy.
Description
Technical field:
The invention belongs to inclusion experimental technique field, be specifically related to a kind of inclusion thin slice heat treatment method that micro laser Raman spectroscopy is analyzed that is applicable to.
Background technology:
Inclusion be Diagenesis And Mineralization fluid (containing fluid or the molten silicate body of gas-liquid) in crystallizable mineral growth course, be wrapped in mineral lattice defect, still in host, seal up for safekeeping and have that a part of material of the boundary of phase with host so far.It can provide the various GEOLOGICAL AND GEOCHEMICAL information of geologic media at that time.Fluid Inclusion Compositions analysis is one of basic task of study on inclusions, and the physical chemistry information that it can provide accurately detailed relevant paleocurrent body to form as much as possible, to set up the geochemical model of paleocurrent body mechanism.
Mainly by laser micro-raman spectrometry (LRM) technology to the constituent analysis of inclusion at present.By laser micro-raman spectrometry technology, the gas phase in mineral, liquid phase, water-soluble liquid phase and Solid Inclusion composition are studied, comparatively simple and reliable means of testing is provided, avoid sample contamination, be conducive to the geochemical investigation (Zhang Meizhen etc. to same period not time, different generations, different origins inclusion, oil experiment geology, 2008).Utilize the composition of Raman spectrum convection cell inclusion to carry out qualitative analysis very convenient, only need feature Raman peaks position just can judge to its composition (Ge Yunjin etc., the test of rock ore deposit, 2008).
In the process of measuring Fluid Inclusion Compositions, often can run into the situation that does not measure Raman peaks, the Raman spectrum of measuring is the shape at born of the same parents peak, so just causes the composition of inclusion to measure.Reason mainly contains following several respects: 1, the degree of depth of the inclusion of surveying is larger, cause instrument obtain signal a little less than; 2, sheet surface is unclean, is stained with organic gel, may produce surface fluorescence, and some host (as fluorite) meeting generation fluorescence itself, and fluorescence can shield some more weak Raman scatterings, interference analysis result; 3, residual organic composition in host crack; 4, crystal growth and thin slice manufacturing process Minerals itself have accumulated the fluorescent effect that thermal stress produces, interference Instrument picked up signal.For the fluorescent effect that in the thermal stress accumulating in crystal growth and thin slice manufacturing process and inclusion surface and crack, residual organic matter (organic glue) produces, also there is no at present the tired elimination of good method.
Summary of the invention:
The object of the invention is to overcome the deficiency of existing inclusion Raman test result, provide a kind of inclusion thin slice heat treatment method that is applicable to micro laser Raman spectroscopy analysis that can overcome the fluorescent effect that in the thermal stress that accumulates in crystal growth and thin slice manufacturing process and inclusion surface and crack, residual organic matter (organic glue) produces, the result accurate and effective more that inclusion Raman is tested.
The present invention is under the not destroyed prerequisite of inclusion, remove the fluorescent effect producing in the thermal stress of crystal growth and the accumulation of thin slice manufacturing process Minerals by heat packs body thin slice, and the fluorescent effect that in inclusion sheet surface and crack, residual organic matter (organic glue) produces, thereby make the result accurate and effective more of inclusion Raman test, and realize object of the present invention.
The inclusion thin slice heat treatment method that is applicable to micro laser Raman spectroscopy analysis of the present invention, is characterized in that, comprises the following steps:
A, inclusion thin slice is separated the heating of inclusion thin slice and microslide with microslide, then inclusion thin slice is put into alcohol and soak, take out the organic gel of wiping again inclusion sheet surface with alcohol off;
B, the inclusion thin slice that step a is handled well carry out petrography observation, divide inclusion type, carry out the research of the preliminary micro-thermometric of inclusion, determine the minimum homogenization temperature of inclusion in this inclusion thin slice;
C, determine the heat treatment temperature of inclusion thin slice according to preliminary micro-temperature-measuring results, the heat treatment temperature of inclusion thin slice is low 40～80 DEG C compared with the minimum homogenization temperature of inclusion, but heat treatment temperature should be lower than 80 DEG C, also should be higher than 150 DEG C;
D, inclusion thin slice is warming up to fixed heat treatment temperature constant temperature 20min on electric hot plate, is then slowly down to room temperature, then carries out laser micro-raman spectrometry analysis.
Described step a heats inclusion thin slice inclusion thin slice is separated with microslide with microslide, then inclusion thin slice is put into alcohol, take out again by the organic gel that alcohol is wiped inclusion sheet surface off and be preferably inclusion thin slice and microslide are placed on the temperature control plate of 80 DEG C and are heated, inclusion thin slice is separated with microslide, inclusion thin slice is put into fill in spirituous glass dish again and soaked 24 hours, inclusion thin slice is taken out, with two surfaces that repeatedly wipe inclusion thin slice with spirituous cotton swab along a direction, remove surperficial organic gel.
Described steps d carry out laser micro-raman spectrometry analysis, its inclusion should select to approach inclusion sheet surface as far as possible.
Compare and prior art, beneficial effect of the present invention is as follows:
1, the present invention utilizes the characteristic of inclusion thin slice, and inclusion thin slice is heat-treated, and has reduced the influence factor of fluorescent effect to laser micro-raman spectrometry analysis result, has significantly improved the sensitivity of micro laser Raman spectroscopy Measurement results.
2, the present invention is by the Study of Heat Treatment to dissimilar inclusion thin slice, determine the selection principle of the heat treatment temperature based on the preliminary micro-thermometric research of inclusion, in the sensitivity that ensures to improve under the prerequisite that inclusion is not destroyed micro laser Raman spectroscopy analysis.
3, the present invention is simple to operate, and operating process is easily controlled.
Therefore, method of the present invention can overcome the thermal stress accumulating in crystal growth and thin slice manufacturing process and inclusion is surperficial and crack in the fluorescent effect that produces of residual organic matter (organic glue), therefore can effectively utilize micro laser Raman spectroscopy and measure the composition through method of the present invention inclusion after treatment, and the method is with low cost, flow process simple, easy operating and applying.
Brief description of the drawings:
Fig. 1 is the laser micro-raman spectrometry figure without fluid inclusion gas phase in the inclusion thin slice of bakingout process in embodiment 1;
Fig. 2 is the laser micro-raman spectrometry figure through fluid inclusion gas phase in heat treated inclusion thin slice in embodiment 1.
Fig. 3 is the laser micro-raman spectrometry figure without fluid inclusion gas phase in the inclusion thin slice of bakingout process in embodiment 2;
Fig. 4 is the laser micro-raman spectrometry figure through fluid inclusion gas phase in heat treated inclusion thin slice in embodiment 2.
Embodiment
Following examples are to further illustrate of the present invention, instead of limitation of the present invention.
Inclusion sample in embodiment is all selected from the quartzy druse in the Chang Wu rock mass of Fujian, because the inclusion in quartz is more.In order better to embody the superiority of the inventive method, we had carried out laser micro-raman spectrometry analysis with in contrast before thermal treatment to same inclusion in an embodiment.
Embodiment 1:
1, inclusion thin slice (cw01-1) and microslide are placed on to the temperature control plate heating of 80 DEG C, inclusion thin slice is separated with microslide; Inclusion thin slice (cw01-1) is put into fill in spirituous glass dish and soak 24 hours; Inclusion thin slice is taken out, with two surfaces that repeatedly wipe inclusion sheet with spirituous cotton swab along a direction, remove surperficial organic gel.
2, examine under a microscope step 1 inclusion thin slice after treatment, carry out petrography observation, divide the type (primary inclusion and secondary inclusion) of inclusion.In this inclusion thin slice, do not find secondary inclusion, so only need carry out preliminary micro-thermometric to connate fluid inclusion, determine minimum inclusion homogenization temperature.Then select size approximately 20 μ m, phase boundary line clear and approach the inclusion of inclusion sheet surface, for laser micro-raman spectrometry analysis, to compare with following inclusion laser micro-raman spectrometry analysis result after bakingout process, its result as shown in Figure 1.
3, the preliminary micro-thermometric that carries out to step 1 inclusion thin slice after treatment (cw01-1).Preliminary micro-temperature-measuring results shows that the homogenization temperature of this inclusion thin slice inner fluid inclusion is between 175～186 DEG C, and we have chosen the temperature of heat-treating as inclusion thin slice lower than approximately 40 DEG C of the minimum homogenization temperatures of inclusion (135 DEG C).
4, inclusion thin slice after treatment step 1 is placed on electric hot plate, temperature is risen to 135 DEG C of about 20min of constant temperature, then powered-down after being slowly down to room temperature takes off inclusion thin slice.
5, the fluid inclusion (inclusion thin slice) in the step 2 of processing through step 4 with micro laser Raman spectroscopy analysis, its result as shown in Figure 2.
As can be seen from Figure 1, there is no obvious characteristic peaks without the micro laser Raman spectroscopy analysis result of fluid inclusion gas phase composition in bakingout process thin slice, laser Raman spectroscopy becomes born of the same parents peak shape; As can be seen from Figure 2, in bakingout process thin slice, the micro laser Raman spectroscopy analysis result of fluid inclusion gas phase composition has obvious water peak and CO2 peak value, and has measured the part secondary peak value of host quartz.
Embodiment 2:
Embodiment 2 heat-treats inclusion thin slice (cw01-1a), and except heat treatment temperature is lower than 80 DEG C of the minimum homogenization temperatures of measured inclusion, all the other steps are with the same in embodiment 1.
Preliminary micro-temperature-measuring results shows that the homogenization temperature of this inclusion thin slice inner fluid inclusion is between 205～213 DEG C, and we have chosen the temperature of heat-treating as inclusion thin slice lower than approximately 80 DEG C of the minimum homogenization temperatures of inclusion (125 DEG C).
As can be seen from Figure 3, there is no obvious characteristic peaks without the micro laser Raman spectroscopy analysis result of fluid inclusion gas phase composition in bakingout process thin slice, laser Raman spectroscopy becomes born of the same parents peak shape; As can be seen from Figure 4, in bakingout process thin slice, the micro laser Raman spectroscopy analysis result of fluid inclusion gas phase composition has obvious water peak and CO2 peak value, and has measured the part secondary peak value of host quartz.
Claims (3)
1. be applicable to the inclusion thin slice heat treatment method that micro laser Raman spectroscopy is analyzed, it is characterized in that, comprise the following steps:
A, inclusion thin slice is separated the heating of inclusion thin slice and microslide with microslide, then inclusion thin slice is put into alcohol and soak, take out the organic gel of wiping again inclusion sheet surface with alcohol off;
B, the inclusion thin slice that step a is handled well carry out petrography observation, divide inclusion type, carry out the research of the preliminary micro-thermometric of inclusion, determine the minimum homogenization temperature of inclusion in this inclusion thin slice;
C, determine the heat treatment temperature of inclusion thin slice according to preliminary micro-temperature-measuring results, the heat treatment temperature of inclusion thin slice is low 40～80 DEG C compared with the minimum homogenization temperature of inclusion, but heat treatment temperature should be lower than 80 DEG C, also should be higher than 150 DEG C;
D, inclusion thin slice is warming up to fixed heat treatment temperature constant temperature 20min on electric hot plate, is then slowly down to room temperature, then carries out laser micro-raman spectrometry analysis.
2. inclusion thin slice heat treatment method according to claim 1, it is characterized in that, described step a heats inclusion thin slice inclusion thin slice is separated with microslide with microslide, then inclusion thin slice is put into alcohol, take out again by the organic gel that alcohol is wiped inclusion sheet surface off and be specially inclusion thin slice and microslide are placed on the temperature control plate of 80 DEG C and are heated, inclusion thin slice is separated with microslide, inclusion thin slice is put into fill in spirituous glass dish again and soaked 24 hours, inclusion thin slice is taken out, with two surfaces that repeatedly wipe inclusion thin slice with spirituous cotton swab along a direction, remove surperficial organic gel.
3. inclusion thin slice heat treatment method according to claim 1, is characterized in that, described steps d carry out laser micro-raman spectrometry analysis, its inclusion should select to approach inclusion sheet surface as far as possible.
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Cited By (4)
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| CN106482990A (en) * | 2015-08-28 | 2017-03-08 | 中国石油化工股份有限公司 | The manufacture method of fluid inclusion thin slice |
| CN106932832A (en) * | 2015-12-30 | 2017-07-07 | 核工业北京地质研究院 | One kind contains CO2Fluid inclusion light microscope recognition methods |
| CN111751176A (en) * | 2019-03-26 | 2020-10-09 | 中国石油化工股份有限公司 | Slice moving device for rock inclusion slice |
| CN113533331A (en) * | 2021-07-15 | 2021-10-22 | 西南石油大学 | Method for determining deep ancient salt lake deposition temperature based on halite inclusion |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106482990A (en) * | 2015-08-28 | 2017-03-08 | 中国石油化工股份有限公司 | The manufacture method of fluid inclusion thin slice |
| CN106482990B (en) * | 2015-08-28 | 2020-10-20 | 中国石油化工股份有限公司 | Method for making fluid inclusion sheet |
| CN106932832A (en) * | 2015-12-30 | 2017-07-07 | 核工业北京地质研究院 | One kind contains CO2Fluid inclusion light microscope recognition methods |
| CN111751176A (en) * | 2019-03-26 | 2020-10-09 | 中国石油化工股份有限公司 | Slice moving device for rock inclusion slice |
| CN111751176B (en) * | 2019-03-26 | 2024-02-23 | 中国石油化工股份有限公司 | Rock inclusion thin slice moves piece device |
| CN113533331A (en) * | 2021-07-15 | 2021-10-22 | 西南石油大学 | Method for determining deep ancient salt lake deposition temperature based on halite inclusion |
| CN113533331B (en) * | 2021-07-15 | 2023-10-17 | 西南石油大学 | Method for determining deposition temperature of deep palaeomized salt lake based on rock salt inclusion |
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