CN114384009A - Sealed sample pool for laser high-temperature melting of carbonate sample and use method thereof - Google Patents
Sealed sample pool for laser high-temperature melting of carbonate sample and use method thereof Download PDFInfo
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- CN114384009A CN114384009A CN202110535661.4A CN202110535661A CN114384009A CN 114384009 A CN114384009 A CN 114384009A CN 202110535661 A CN202110535661 A CN 202110535661A CN 114384009 A CN114384009 A CN 114384009A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
Abstract
The invention provides a sealed sample cell for laser high-temperature melting of a carbonate sample and a use method thereof, a sealing clamping groove is formed on the lower surface of the upper sample cell seat, the base of the sample cell adopts a convex structure, the tail end of the upper sample cell seat is inserted into the head end of the base of the sample cell, a central counter bore is formed at the center of the upper surface of the sample cell base, a stepped central hole penetrating through the sample cell upper seat is formed in the sealing clamping groove, the stepped central hole consists of a sample placing hole and a sealing hole, a sample limiting step is formed at the joint of the sample placing hole and the sealing hole, the sample is arranged at the sample limiting step, a glass sheet and a spring are arranged between the lower surface of the sample and the upper surface of the sample cell base, an air inlet which penetrates through the side wall of the sample cell upper seat is arranged on the side wall of the sample cell upper seat positioned in the sample placing hole, and an air outlet which penetrates through the side wall of the upper sample cell seat is formed in the side wall of the upper sample cell seat positioned in the sealing hole. The sealed sample cell has good reproducibility and sealing property.
Description
Technical Field
The invention relates to the technical field of sealed sample pools, in particular to a sealed sample pool for a laser high-temperature molten carbonate sample and a using method thereof.
Background
Laser CO2The melting system emits a high-energy laser beam which is focused by a laser lens (the beam spot is about 100 mu m) on the slice with the determined carbonate micro-area structure, and the carbonate micro-area structure is heated at high temperature with enough energy to decompose and generate CO2Gas, CO obtained by dewatering, purifying, separating by chromatographic column and purifying2The gas is sent into an isotope mass spectrometer to measure C, O isotope value (delta)13CPDBAnd delta18OPDB). How to convert CO in the above process2The enrichment of gases in a closed space is an important step.
At present, the carbon-oxygen isotope technology of carbonate by laser is formed by laser CO2The device comprises a melting system, a purification system and an isotope mass spectrometer. Laser CO2The fusion system generally includes a laser source, a laser delivery system, an inspection system, and a sample cell portion. The purification system generally comprises a water trap, a coarse cold trap, a fine cold trap and a chromatographic column, and the isotope mass spectrometer comprises an ion source, an interface cone, a quadrupole mass analyzer, a detector, a vacuum pump and the like.
Wherein the sample cell is for influencing laser CO2The melting system is one of the main components for analyzing performance, the sample cell is used for placing a sample and melting by laser, so the design of the sample cell is important, and the design of the sample cell can control the transient of signals because the minimum laser spot can be controlled to be 100 mu m.
At present, there is not the sealed sample cell that has pertinence, and current common sample cell when putting into the sample, need rotate the breather pipe that the gas outlet links to each other, can cause the leakage of gas circuit, and the lid also probably drops and falls to the ground and cause the damage, because laser incident window is located the lid, the frequent action of lid can cause the unbalance of window, and laser focusing is influenced, and the reproducibility is relatively poor.
Disclosure of Invention
The invention overcomes the defects in the prior art, and the problems of gas path leakage, cover body falling and falling damage and poor reproducibility of the existing sample cell, and provides a sealed sample cell for laser high-temperature molten carbonate samples and a using method thereof.
The purpose of the invention is realized by the following technical scheme.
A sealed sample cell for laser high-temperature melting of a carbonate sample comprises a sample cell upper seat and a sample cell base, wherein a sealed clamping groove is formed in the lower surface of the sample cell upper seat, the sample cell base is of a convex structure, the tail end of the sample cell upper seat is inserted into the head end of the sample cell base to achieve the purpose of sealing, a central counter bore is formed in the center of the upper surface of the sample cell base, a stepped central hole penetrating through the sample cell upper seat is formed in the sealed clamping groove, the central counter bore is communicated with the stepped central hole to form a sealed cavity, the stepped central hole consists of a sample placing hole and a sealed hole, a sample limiting step is formed at the connection position of the sample placing hole and the sealed hole, the sample is arranged at the sample limiting step, and a top support assembly is arranged between the lower surface of the sample and the upper surface of the sample cell base, the sample cell top support comprises a glass sheet and a spring, the tail end of the spring is in contact with the upper surface of a sample cell base, the head end of the spring is in contact with the lower surface of the glass sheet, the upper surface of the glass sheet is in contact with the lower surface of the sample, a window mirror placing groove is formed in the upper surface of a sample cell top support, the window mirror placing groove is communicated with a sealing hole, a zinc sulfide window mirror is arranged in the window mirror placing groove, an air inlet penetrating through the sample cell top support side wall is formed in the sample cell top support side wall of the sample placing hole, and an air outlet penetrating through the sample cell top support side wall is formed in the sample cell top support side wall of the sealing hole.
The upper surface of the sample cell upper seat is also provided with a fixed cover, a fixed through hole is formed in the center of the fixed cover, and the fixed through hole is opposite to the sealing hole, so that a laser beam can penetrate through the fixed through hole and the zinc sulfide window mirror and then is injected into the sealing cavity.
The fixing covers on the two sides of the fixing through hole are provided with fixing screw holes, the corresponding positions of the upper surface of the sample pool upper seat are provided with screw holes, the fixing screw holes and the screw holes are arranged in a one-to-one correspondence mode, the fixing covers are fixed on the upper surface of the sample pool upper seat after the fastening screws penetrate through the fixing screw holes and the screw holes, and therefore the purpose that the zinc sulfide window glasses are fixed in the window glass arranging grooves is achieved.
The upper surface in window mirror mounting groove has seted up the window mirror seal groove the seal groove has been seted up to the upper surface of sample cell base the window mirror seal groove with all be provided with the sealing washer in the seal groove to realize the sealed purpose of zinc sulfide window mirror and sample cell upper seat and sample cell base and sample cell upper seat.
And an external thread is formed on the outer wall of the convex part of the sample cell base, an internal thread is formed on the side wall of the sealing clamping groove, and the sample cell base is in threaded connection with the internal thread of the sample cell upper seat through the external thread.
And a clamping sleeve interface is formed in the air inlet and the air outlet so as to be communicated with the pipeline.
The ferrule interface is 1/16 inches in size.
A method for using a sealed sample cell for laser high-temperature melting of a carbonate sample comprises the steps of fixing the sample between a sample limiting step and a glass sheet, connecting an upper sample cell seat and a sample cell base through threads, communicating an air inlet with a He gas inlet pipeline, communicating an air outlet with a He gas exhaust pipeline, allowing the He gas to enter from the lower surface of the sample and flow from bottom to top, and starting a laser transmitter after a sealed cavity is filled with the He gas to perform high-temperature melting operation on the sample.
The invention has the beneficial effects that: this zinc sulfide window mirror of sealed sample cell is in the stationary state, can not influence the focus, and the reproducibility is good, and this sealed sample cell passes through sample cell upper seat, the fixed stroke of sample cell base to utilize two static seals to guarantee holistic gas tightness, in order to avoid the loss of sample and the doping of air, through the central shoulder hole that forms in the sample cell upper seat, realize holding to the sample, guarantee through spring and glass piece to the fixing of sample.
Drawings
FIG. 1 is a cross-sectional view of the present invention taken along the air intake;
FIG. 2 is a cross-sectional view of the present invention taken along the outlet port;
FIG. 3 is a schematic view of the position of a fastening screw in the present invention;
in the figure: 1 is sample cell seat of honour, 2 is the zinc sulfide window mirror, 3 is the sealing washer, 4 is the sample, 5 is the glass piece, 6 is the spring, 7 is the sample cell base, 8 is the air inlet, 9 is the gas outlet, 10 is fastening screw, 11 is sealed cavity, 12 is the spacing step of sample, 13 is the cutting ferrule interface, 14 is fixed lid, 15 is the external screw thread.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example one
A sealed sample cell for laser high-temperature melting of a carbonate sample comprises a sample cell upper seat 1 and a sample cell base 7, wherein a sealed clamping groove is formed on the lower surface of the sample cell upper seat 1, the sample cell base 7 adopts a structure in a shape like a Chinese character 'tu', the tail end of the sample cell upper seat 1 is inserted into the head end of the sample cell base 7 so as to achieve the purpose of sealing, a central counter bore is formed at the center of the upper surface of the sample cell base 7, a stepped central hole penetrating through the sample cell upper seat is formed in the sealed clamping groove, the central counter bore is communicated with the stepped central hole to form a sealed cavity 11, the stepped central hole consists of a sample placing hole and a sealed hole, a sample limiting step 12 is formed at the joint of the sample placing hole and the sealed hole, a sample 4 is arranged at the sample limiting step 12, and a top support component is arranged between the lower surface of the sample 4 and the upper surface of the sample cell base 7, the sample supporting device is used for supporting a sample 4, the top support component comprises a glass sheet 5 and a spring 6, the tail end of the spring 6 is contacted with the upper surface of a sample pool base 7, the head end of the spring 6 is contacted with the lower surface of the glass sheet 5, the upper surface of the glass sheet 5 is contacted with the lower surface of the sample 4, a window mirror placing groove is formed in the upper surface of a sample pool upper seat 1, the window mirror placing groove is communicated with a sealing hole, a zinc sulfide window mirror 2 is arranged in the window mirror placing groove, an air inlet 8 penetrating through the side wall of the sample pool upper seat 1 is formed in the side wall of the sample pool upper seat 1 in the sample placing hole, and an air outlet 9 penetrating through the side wall of the sample pool upper seat 1 is formed in the side wall of the sample pool upper seat 1 in the sealing hole.
Example two
On the basis of the first embodiment, a fixing cover 14 is further arranged on the upper surface of the sample cell upper seat 1, a fixing through hole is formed in the center of the fixing cover 14, and the fixing through hole and the sealing hole are arranged oppositely, so that a laser beam can penetrate through the fixing through hole and the zinc sulfide window mirror 2 and then enter the sealed cavity 11.
The fixing cover 14 on the two sides of the fixing through hole is provided with a fixing screw hole, the corresponding position of the upper surface of the sample cell upper seat 1 is provided with a screw hole, the fixing screw holes and the screw holes are arranged in a one-to-one correspondence mode, and the fixing cover 14 is fixed on the upper surface of the sample cell upper seat 1 after the fastening screws 10 penetrate through the fixing screw holes and the screw holes, so that the purpose of fixing the zinc sulfide window mirror 2 in the window mirror arranging groove is achieved.
The window mirror sealing groove is formed in the upper surface of the window mirror placing groove, the sealing groove is formed in the upper surface of the sample pool base 1, and the sealing rings 3 are arranged in the window mirror sealing groove and the sealing groove, so that the purpose of sealing the zinc sulfide window mirror 2 and the sample pool upper seat 1 and the purpose of sealing the sample pool base 7 and the sample pool upper seat 1 are achieved.
EXAMPLE III
On the basis of the second embodiment, an external thread 15 is formed on the outer wall of the protruding portion of the sample cell base 7, an internal thread is formed on the side wall of the sealing clamping groove, and the sample cell base 7 is in threaded connection with the internal thread of the sample cell upper seat 1 through the external thread.
A cutting sleeve interface 13 is formed in the air inlet 8 and the air outlet 9 so as to be communicated with the pipeline.
The ferrule interface 13 is 1/16 inches in size.
Example four
A method for using a sealed sample cell for laser high-temperature melting of a carbonate sample comprises the steps of fixing the sample between a sample limiting step and a glass sheet, connecting an upper sample cell seat and a sample cell base through threads, communicating an air inlet with a He gas inlet pipeline, communicating an air outlet with a He gas exhaust pipeline, allowing the He gas to enter from the lower surface of the sample and flow from bottom to top, and starting a laser transmitter after a sealed cavity is filled with the He gas to perform high-temperature melting operation on the sample.
He gas flows from the lower part of the sample 4 and flows from bottom to top, so that the sealed cavity 11 is filled with the He gas, a blank background signal of the sealed sample cell is very low, the method is more advanced than the conventional method, and data obtained by testing is more accurate.
Spatially relative terms, such as "upper," "lower," "left," "right," and the like, may be used in the embodiments for ease of description to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that the spatial terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "below" other elements or features would then be oriented "above" the other elements or features. Thus, the exemplary term "lower" can encompass both an upper and a lower orientation. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
Moreover, relational terms such as "first" and "second," and the like, may be used solely to distinguish one element from another element having the same name, without necessarily requiring or implying any actual such relationship or order between such elements.
The present invention has been described in detail, but the above description is only a preferred embodiment of the present invention, and is not to be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (8)
1. A sealed sample cell for laser high temperature melting of carbonate samples, characterized by: the sample tank comprises a sample tank upper seat and a sample tank base, wherein a sealing clamping groove is formed in the lower surface of the sample tank upper seat, the sample tank base is of a convex structure, the tail end of the sample tank upper seat is inserted into the head end of the sample tank base to achieve the purpose of sealing, a central counter bore is formed in the center of the upper surface of the sample tank base, a stepped central hole penetrating through the sample tank upper seat is formed in the sealing clamping groove, the central counter bore is communicated with the stepped central hole to form a sealed cavity, the stepped central hole is composed of a sample placing hole and a sealing hole, a sample limiting step is formed at the connection part of the sample placing hole and the sealing hole, a sample is arranged at the sample limiting step, and a top support assembly is arranged between the lower surface of the sample and the upper surface of the sample tank base and used for supporting the sample, the top supporting component comprises a glass sheet and a spring, the tail end of the spring is in contact with the upper surface of the sample pool base, the head end of the spring is in contact with the lower surface of the glass sheet, the upper surface of the glass sheet is in contact with the lower surface of the sample, a window mirror placing groove is formed in the upper surface of the sample pool upper seat, the window mirror placing groove is communicated with the sealing hole, a zinc sulfide window mirror is arranged in the window mirror placing groove, an air inlet penetrating through the sample pool upper seat side wall is formed in the sample pool upper seat side wall of the sample placing hole, and an air outlet penetrating through the sample pool upper seat side wall is formed in the sample pool upper seat side wall of the sealing hole.
2. The sealed sample cell for laser high temperature molten carbonate samples according to claim 1, wherein: the upper surface of the sample cell upper seat is also provided with a fixed cover, a fixed through hole is formed in the center of the fixed cover, and the fixed through hole is opposite to the sealing hole.
3. The sealed sample cell for laser high temperature molten carbonate samples according to claim 2, wherein: the fixing covers on the two sides of the fixing through hole are provided with fixing screw holes, the corresponding positions of the upper surface of the sample cell upper seat are provided with screw holes, the fixing screw holes and the screw holes are arranged in a one-to-one correspondence mode, and the fastening screws penetrate through the fixing screw holes and the screw holes and then fix the fixing covers on the upper surface of the sample cell upper seat.
4. The sealed sample cell for laser high temperature molten carbonate samples according to claim 3, wherein: the upper surface in window mirror mounting groove has seted up the window mirror seal groove the seal groove has been seted up to the upper surface of sample cell base the window mirror seal groove with all be provided with the sealing washer in the seal groove.
5. The sealed sample cell for laser high temperature molten carbonate samples according to claim 1, wherein: and an external thread is formed on the outer wall of the convex part of the sample cell base, an internal thread is formed on the side wall of the sealing clamping groove, and the sample cell base is in threaded connection with the internal thread of the sample cell upper seat through the external thread.
6. The sealed sample cell for laser high temperature molten carbonate samples according to claim 1, wherein: and a clamping sleeve interface is formed in the air inlet and the air outlet so as to be communicated with the pipeline.
7. The sealed sample cell for laser high temperature molten carbonate samples according to claim 6, wherein: the ferrule interface is 1/16 inches in size.
8. A use method of a sealed sample cell for laser high-temperature melting of carbonate samples is characterized in that: fixing the sample between the sample limiting step and the glass sheet, connecting the sample cell upper seat and the sample cell base through threads, communicating the gas inlet with a He gas inlet pipeline, communicating the gas outlet with a He gas exhaust pipeline, allowing the He gas to enter from the lower surface of the sample, flowing from bottom to top, and starting a laser transmitter after the sealed cavity is filled with the He gas to perform high-temperature melting operation on the sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110535661.4A CN114384009A (en) | 2021-05-17 | 2021-05-17 | Sealed sample pool for laser high-temperature melting of carbonate sample and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110535661.4A CN114384009A (en) | 2021-05-17 | 2021-05-17 | Sealed sample pool for laser high-temperature melting of carbonate sample and use method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN114384009A true CN114384009A (en) | 2022-04-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110535661.4A Pending CN114384009A (en) | 2021-05-17 | 2021-05-17 | Sealed sample pool for laser high-temperature melting of carbonate sample and use method thereof |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5750989A (en) * | 1995-02-10 | 1998-05-12 | Molecular Imaging Corporation | Scanning probe microscope for use in fluids |
| CN203672702U (en) * | 2013-12-06 | 2014-06-25 | 宁波检验检疫科学技术研究院 | Sample pond for solid ablation with laser |
| CN104458979A (en) * | 2014-12-31 | 2015-03-25 | 中国地质科学院矿产资源研究所 | Measuring device and measuring method for carbon-oxygen isotope of carbonate rock |
| US20170348687A1 (en) * | 2016-06-01 | 2017-12-07 | Government Of The United States Of America, As Represented By The Secretary Of Commerce | Vacuum compatible fluid sampler |
| CN107449651A (en) * | 2017-08-03 | 2017-12-08 | 核工业北京地质研究院 | Laser pool device for laser sample preparation mass spectrum oxygen isotope composition analysis |
| CN206990435U (en) * | 2017-07-10 | 2018-02-09 | 合肥国轩高科动力能源有限公司 | A kind of multichannel sealing system infrared spectrum analysis sample cell |
| CN211350574U (en) * | 2020-03-17 | 2020-08-25 | 中国科学院地球化学研究所 | Laser ablation platform sample loading device |
-
2021
- 2021-05-17 CN CN202110535661.4A patent/CN114384009A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5750989A (en) * | 1995-02-10 | 1998-05-12 | Molecular Imaging Corporation | Scanning probe microscope for use in fluids |
| CN203672702U (en) * | 2013-12-06 | 2014-06-25 | 宁波检验检疫科学技术研究院 | Sample pond for solid ablation with laser |
| CN104458979A (en) * | 2014-12-31 | 2015-03-25 | 中国地质科学院矿产资源研究所 | Measuring device and measuring method for carbon-oxygen isotope of carbonate rock |
| US20170348687A1 (en) * | 2016-06-01 | 2017-12-07 | Government Of The United States Of America, As Represented By The Secretary Of Commerce | Vacuum compatible fluid sampler |
| CN206990435U (en) * | 2017-07-10 | 2018-02-09 | 合肥国轩高科动力能源有限公司 | A kind of multichannel sealing system infrared spectrum analysis sample cell |
| CN107449651A (en) * | 2017-08-03 | 2017-12-08 | 核工业北京地质研究院 | Laser pool device for laser sample preparation mass spectrum oxygen isotope composition analysis |
| CN211350574U (en) * | 2020-03-17 | 2020-08-25 | 中国科学院地球化学研究所 | Laser ablation platform sample loading device |
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