Multifunctional light and quality dual-purpose denudation pool

Abstract

The invention discloses a multifunctional light and quality dual-purpose denudation pool which comprises a laser denudation pool body. A homogenizing cavity is formed in the laser ablation pool main body; an optical fiber probe coupling interface is formed in the top of the laser denudation pool main body, penetrates through the homogenizing cavity and is over against a laser denudation point; a multifunctional auxiliary gas interface is formed in the side wall of the laser ablation pool main body and penetrates through the homogenizing cavity; an aerosol extraction pipeline fixing groove is formed in the bottom of the laser denudation pool body. Mass spectrum signals and spectral signals can be analyzed at the same time, the time cost is saved, various data are obtained at the same time, and the analysis efficiency is improved; meanwhile, the transmission pipeline structure is simplified, the economic cost is reduced, the sample extraction efficiency is improved, and the tailing effect is reduced.

Description

Technical Field

[0001] The invention belongs to the technical field of solid sample analysis, and in particular relates to a multifunctional light-quality dual-purpose ablation cell. Background Art

[0002] Laser ablation sampling inductively coupled plasma mass spectrometry technology plays an extremely important role in the fields of semiconductors, environment, medicine, earth science, analytical chemistry, materials, etc. due to its advantages such as simple sampling method, high spatial resolution, and in-situ analysis. During the laser ablation sample process, a plasma light source will be generated; the emission spectrum of characteristic elements can quickly realize the qualitative and semi-quantitative analysis of elements in the sample. However, in the current analysis system of laser ablation combined with mass spectrometer, only the mass spectrometer analyzes the element content (or isotope); there is no simultaneous isotope analysis and element content analysis. The aerosol generated during the laser ablation process is only introduced into the mass spectrometer for analysis, and the characteristic spectrum generated during the laser ablation process is not collected, resulting in a great waste of resources. It is impossible to obtain the data contained in the spectral signal while obtaining the mass spectrometry signal. The key point of its limitation is how to collect the spectral signal while collecting the aerosol.

[0003] In addition, in laser ablation mass spectrometry, the matrix effect caused by different matrix samples often seriously affects the reliability of the analysis results. In view of the matrix effect, the online introduction of gas substances (such as water vapor, nitrogen, etc.) can significantly suppress the deviation caused by the matrix effect and improve the signal response of the elements in the analysis process. However, in the existing technology, gas substances can usually only be introduced online after the laser ablation produces aerosols; this makes it impossible to correct the matrix effect during the laser ablation process, and only corrects the matrix effect during the aerosol transmission process. The key point that restricts its development is that it is impossible to introduce gas substances into the ablation cell of the ablation sample; because the large volume of the double chamber will produce large fluctuations when introducing gas substances, and it takes a very long time to wait for the gas substances to form a stable gas atmosphere in the ablation cell, which is time-consuming and labor-intensive. Although the traditional single sample cell is small in size and can introduce gas substances, the single cell has a very strong position effect, which is not conducive to high-precision element content and isotope composition analysis.

[0004] Second, in laser ablation technology, laser acts on the sample surface to generate aerosol, which is usually agglomerated. In order to make the signal obtained by the mass spectrometer more stable, it is often necessary to perform online homogenization on the generated aerosol. This usually requires adding a homogenizer to the transmission pipeline, making the system complex and increasing the cost.

[0005] Third, the traditional dual-chamber sample cell has low aerosol extraction efficiency and slow mass spectrometer signal response, which causes serious tailing and is not conducive to mass spectrometry analysis.

[0006] It can be seen that the existing laser ablation inductively coupled plasma mass spectrometer sampling method has technical disadvantages such as single signal acquisition, low extraction efficiency, complex homogenization system, and inability to introduce gas substances to reduce matrix effect. Summary of the invention

[0007] The purpose of the present invention is to provide a multifunctional light-mass dual-purpose ablation cell to address the above-mentioned deficiencies in the prior art, so as to solve the problems of the existing laser ablation inductively coupled plasma mass spectrometer sampling method, such as single signal acquisition, low extraction efficiency, complex homogenization system, and inability to introduce gaseous substances to reduce the matrix effect.

[0008] In order to achieve the above object, the technical solution adopted by the present invention is: A multifunctional light-quality dual-purpose ablation cell, comprising a laser ablation cell body; a homogenization cavity is arranged inside the laser ablation cell body; a fiber optic probe coupling interface is provided on the top of the laser ablation cell body, the fiber optic probe coupling interface passes through the homogenization cavity and is directly opposite to the laser ablation point; a multifunctional auxiliary gas interface is provided on the side wall of the laser ablation cell body, the multifunctional auxiliary gas interface passes through the homogenization cavity; an aerosol extraction pipeline fixing groove is provided at the bottom of the laser ablation cell body.

[0009] Furthermore, a window sealing assembly is provided on the homogenization chamber; the window sealing assembly includes a window fixing plate, a highly transparent window and an O-ring; the window fixing plate is ring-shaped, the highly transparent window is fixed to the window fixing plate by an O-ring, and the window fixing plate is arranged on a step opened in the homogenization chamber.

[0010] Furthermore, a fiber optic coupling assembly is installed at the coupling interface of the fiber optic probe; the fiber optic coupling assembly includes a fiber optic probe and a sealing O-ring sleeved on the fiber optic probe, and the position of the sealing O-ring is adjusted to adjust the sampling depth of the fiber optic probe; the fiber optic probe is connected to the high-resolution spectrometer signal.

[0011] Furthermore, a plurality of auxiliary gas connectors are installed at the multifunctional auxiliary gas interface; the plurality of auxiliary gas connectors are connected to an extraction pipeline; and the extraction pipeline is connected to an analytical instrument.

[0012] Furthermore, two aerosol extraction pipeline fixing grooves are symmetrically provided at the bottom of the laser ablation cell body; the two aerosol extraction pipeline fixing grooves are respectively fixed with a purge pipeline and an extraction pipeline; the purge pipeline and the extraction pipeline are closely attached to the sample surface.

[0013] Furthermore, the sample is fixed in a large bin and is located below the homogenization chamber.

[0014] Furthermore, the multiple auxiliary gas joints and the purge pipeline are perpendicular to each other in a plane.

[0015] Furthermore, a plurality of fixing holes are provided on the main body of the laser ablation pool.

[0016] The multifunctional light-quality dual-purpose ablation pool provided by the present invention has the following beneficial effects: 1. The present invention can analyze mass spectrometry signals and spectral signals simultaneously, saving time and cost, acquiring multiple data at the same time, and improving analysis efficiency; at the same time, it simplifies the transmission pipeline structure, reduces economic costs, improves sample extraction efficiency, and reduces tailing effects.

[0017] 2. The spectral sampling depth of the present invention can be adjusted arbitrarily to adapt to spectral signals of different intensities.

[0018] 3. The present invention has three different aerosol extraction methods, which can mix the aerosol in situ online to produce a smoother mass spectrometry signal; during linear purge extraction, it is close to the sample surface, the purge extraction efficiency is greatly improved, the signal response is fast, and the tail is short; in addition, it can also be used for the study of matrix effects, and auxiliary gases such as water vapor and nitrogen are introduced online for laser ablation, which greatly reduces the matrix effect and improves the precision and accuracy of the original analysis.

[0019] 4. The sample pool of the present invention can be made of PEEK, which has corresponding strength and extremely low background, and is suitable for isotope and element content analysis; all pipelines are made of stainless steel pipes to reduce electrostatic adsorption and adsorption caused by surface dirt, reduce purge time, and have a higher signal-to-noise ratio. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is an exploded view of the multifunctional light-quality dual-purpose ablation pool of the present invention.

[0021] Figure 2 It is a top view of the multifunctional light-quality dual-purpose erosion pool of the present invention.

[0022] Figure 3 The cross-sectional view of the multifunctional light-quality dual-purpose ablation pool of the present invention Figure 1 .

[0023] Figure 4 The cross-sectional view of the multifunctional light-quality dual-purpose ablation pool of the present invention Figure 2 .

[0024] Figure 5 The cross-sectional view of the multifunctional light-quality dual-purpose ablation pool of the present invention Figure 3 .

[0025] Among them, 1. ablation cell; 11. laser ablation cell body; 12. multifunctional auxiliary gas interface; 13. optical fiber probe coupling interface; 14. fixing hole; 15. aerosol extraction pipeline fixing groove; 16. homogenization chamber; 2. Aerosol pipeline; 21. Purge pipeline; 22. Extraction pipeline; 3. Optical fiber coupling assembly; 31. Optical fiber probe; 32. Sealing O-ring; 4. Window sealing assembly; 41. Window fixing plate; 42. Highly transparent window; 43. O-ring; 5. Multiple auxiliary gas joints; 6. Laser; 7. Sample. DETAILED DESCRIPTION

[0026] The specific implementation modes of the present invention are described below so that those skilled in the art can understand the present invention. However, it should be clear that the present invention is not limited to the scope of the specific implementation modes. For those of ordinary skill in the art, as long as various changes are within the spirit and scope of the present invention as defined and determined by the attached claims, these changes are obvious, and all inventions and creations utilizing the concept of the present invention are protected.

[0027] Example 1 This embodiment provides a multifunctional dual-purpose light-mass ablation cell, which can be used for laser ablation plasma mass spectrometry (LA-MC / ICP-MS) and spectroscopy (LIBS) dual-purpose ablation cell; while laser ablation transmits aerosol, it can couple the optical fiber to the laser ablation point for spectral signal collection, and simultaneously obtain spectral data and mass spectral data, thereby improving analysis efficiency. Figure 1 and Figure 2 , which specifically includes a denudation pool 1; The ablation pool 1 of this embodiment includes a laser ablation pool body 11. This embodiment does not limit the shape of the laser ablation pool body 11. Preferably, this embodiment sets the laser ablation pool body 11 to be a cone shape. The laser ablation pool body 11 is provided with a plurality of fixing holes 14 for fixing the laser ablation pool body 11.

[0028] refer to Figure 3~Figure 5 A homogenization chamber 16 is arranged inside the cone-shaped laser ablation pool body 11, which is the main place for forming the auxiliary gas atmosphere and the homogenized aerosol. The homogenization chamber 16 is cone-shaped, and its radius gradually decreases from top to bottom. Both ends are opened. The sample 7 is located at the bottom of the homogenization chamber 16, and the sample 7 is fixed in the large chamber. Usually, the double-chamber laser ablation pool is divided into a large chamber and a small chamber (ablation pool 1). Since the large chamber is a prior art, it will not be repeated here. The present invention mainly protects the small chamber (ablation pool 1).

[0029] A window sealing assembly 4 for sealing the homogenizing chamber 16 is provided at the top of the homogenizing chamber 16. As a preferred embodiment of the present embodiment, the window sealing assembly 4 includes a window fixing plate 41, a highly transparent window 42 and an O-ring 43. The window fixing plate 41 is in a ring shape. The highly transparent window 42 is fixed to the window fixing plate 41 by the O-ring 43. The window fixing plate 41 is provided on a step opened in the homogenizing chamber 16. During specific operation, the laser 6 is perpendicular to the highly transparent window 42 and passes through the homogenizing chamber 16 to reach the surface of the sample 7.

[0030] The top of the laser ablation cell body 11 is provided with an optical fiber probe coupling interface 13, Figure 1 and Figure 5 As a preferred configuration of this embodiment, the optical fiber probe coupling interface 13 is opened obliquely downward from the top of the laser ablation pool body 11 and passes through the homogenization cavity 16, and is directly opposite to the laser ablation point; an optical fiber coupling assembly 3 is installed at the optical fiber probe coupling interface 13, and the optical fiber coupling assembly 3 includes an optical fiber probe 31 and a sealing O-ring 32 sleeved on the optical fiber probe 31, refer to Figure 5 By adjusting the position of the sealing O-ring 32, the depth of the optical fiber probe 31 extending into the optical fiber probe coupling interface 13 can be adjusted, thereby adjusting the sampling depth of the optical fiber probe 31. The optical fiber probe 31 is connected to the high-resolution spectrometer signal. During the specific operation, the spectrum signal generated by the laser induced breakdown (LIBS) is collected by the optical fiber probe 31 and transmitted to the high-resolution spectrometer for analysis. The sealing O-ring 32 of this embodiment not only has the function of adjusting the depth of the optical fiber probe 31, but also has the function of sealing the entire ablation pool.

[0031] A multifunctional auxiliary gas interface 12 is provided on the side wall of the laser ablation pool body 11. As a preferred configuration of this embodiment, the multifunctional auxiliary gas interface 12 is provided along the upper side wall of the laser ablation pool body 11 and passes through the homogenization chamber 16 in the horizontal direction.

[0032] A multi-auxiliary gas connector 5 is installed at the multi-functional auxiliary gas interface 12, and the multi-auxiliary gas connector 5 is connected to the extraction pipeline 22, and the extraction pipeline 22 is connected to the analysis instrument to perform mass spectrometry analysis.

[0033] The aerosol pipeline 2 includes a purge pipeline 21 and an extraction pipeline 22. As a preferred embodiment of this embodiment, the multi-auxiliary gas connector 5 and the purge pipeline 21 are perpendicular to each other in a plane.

[0034] Generally, the depth of field of conventional lasers is short, the energy concentration range is small, and the effective ablation range of materials is small. Therefore, the materials are usually very close to the bottom of the laser ablation to effectively ablate the materials. However, the aerosol purge gas path is far away from the sample ablation point, the aerosol extraction efficiency is low, the signal response is slow, and the tailing is serious. To address this problem, an aerosol extraction pipeline fixing groove 15 is provided at the bottom of the laser ablation cell body 11 of this embodiment. For more details, refer to Figure 2 and Figure 3 In this embodiment, two aerosol extraction pipeline fixing grooves 15 are symmetrically opened at the bottom of the laser ablation pool body 11; the two aerosol extraction pipeline fixing grooves 15 are respectively fixed with a purge pipeline 21 and an extraction pipeline 22, and the purge pipeline 21 and the extraction pipeline 22 are close to the sample surface. Such a design can improve the aerosol extraction efficiency.

[0035] This embodiment introduces airflow from the side to perform in-situ aerosol homogenization; reduces the complexity of the aerosol transmission pipeline and improves the homogenization efficiency; moreover, the additional airflow introduction can increase the pressure of the sample chamber, further improving the aerosol transmission efficiency. In addition, the gas path introduction interface designed in the homogenization chamber 16 can be used for research on reducing the laser ablation matrix effect, forming an atmosphere for introducing gas in the homogenization chamber; the small volume of the homogenization chamber does not require long-term stabilization, the waiting time is short, and the analysis efficiency is further improved.

[0036] The erosion tank is designed with a gas introduction interface, a multifunctional auxiliary gas interface 12, which has three different usage schemes in the present invention: 1. To suppress the matrix effect and introduce the interface as an auxiliary gas: This interface is mainly used to introduce water vapor, nitrogen and other gas substances online that help suppress the matrix effect of laser ablation technology, and form such gas atmosphere in the homogenization chamber; 2. When aerosol is extracted linearly with high efficiency, this interface is mainly used to introduce argon or helium to form a positive pressure in the homogenization chamber so that the aerosol is extracted by straight-line blowing in the extraction pipeline 22; 3. When the aerosol is homogenized in situ: the interface is connected to the aerosol outlet pipe of the extraction pipeline 22, and the aerosol purge pipe is used to purge the aerosol particles at the bottom. The aerosol particles spirally rise in the homogenization chamber, are mixed, and then are transmitted to the analysis instrument through the outlet pipe of the extraction pipeline 22.

[0037] The working principle of a multifunctional light-quality dual-purpose ablation cell in this embodiment includes: refer to Figure 3 and Figure 5, the sample is placed in the large chamber and located at the bottom of the homogenization chamber. The laser 6 is perpendicular to the high-transparency window 42 and reaches the surface of the sample 7 through the homogenization chamber 16, eroding the sample to produce aerosol particles. At this time, the aerosol purge pipeline 21 uses helium or argon to purge the generated particulate matter to the extraction pipeline 22, and the extraction pipeline 22 outputs the pipe to transmit the analysis instrument. At the same time, the spectral signal generated by the laser induced breakdown (LIBS) is collected by the optical fiber probe 31 and transmitted to the high-resolution spectrometer for analysis.

[0038] refer to Figure 4 , the multi-auxiliary gas connector 5 is fixedly connected to the multi-functional auxiliary gas interface 12 for introducing gas or transmitting aerosol; When the extraction pipeline 22 is moved to the multi-auxiliary gas connector 5, the aerosol generated by laser ablation rises and rotates under the purge of the carrier gas, is highly mixed in the homogenization chamber 16, and then is transmitted to the analysis instrument through the multi-auxiliary gas connector 5 for mass spectrometry analysis.

[0039] Although the specific implementation of the invention is described in detail in conjunction with the drawings, it should not be understood as limiting the scope of protection of this patent. Within the scope described in the claims, various modifications and variations that can be made by those skilled in the art without creative work still fall within the scope of protection of this patent.

Claims

1. A multifunctional light-quality dual-purpose ablation pool, characterized in that: It comprises a laser ablation pool body; a homogenization cavity is arranged inside the laser ablation pool body; a fiber optic probe coupling interface is provided on the top of the laser ablation pool body, the fiber optic probe coupling interface passes through the homogenization cavity and is directly opposite to the laser ablation point; a multifunctional auxiliary gas interface is provided on the side wall of the laser ablation pool body, the multifunctional auxiliary gas interface passes through the homogenization cavity; an aerosol extraction pipeline fixing groove is provided at the bottom of the laser ablation pool body.

2. The multifunctional light-quality dual-purpose ablation pool according to claim 1, characterized in that: A window sealing assembly is provided on the homogenization chamber; the window sealing assembly includes a window fixing plate, a highly transparent window and an O-ring; the window fixing plate is ring-shaped, the highly transparent window is fixed on the window fixing plate by an O-ring, and the window fixing plate is arranged on a step opened in the homogenization chamber.

3. The multifunctional light-quality dual-purpose ablation pool according to claim 1, characterized in that: A fiber coupling assembly is installed at the coupling interface of the fiber optic probe; the fiber coupling assembly includes a fiber optic probe and a sealing O-ring sleeved on the fiber optic probe, and the position of the sealing O-ring is adjusted to adjust the sampling depth of the fiber optic probe; the fiber optic probe is connected to the high-resolution spectrometer signal.

4. The multifunctional light-quality dual-purpose ablation pool according to claim 1, characterized in that: The multifunctional auxiliary gas interface is provided with multiple auxiliary gas connectors; the multiple auxiliary gas connectors are connected to an extraction pipeline; and the extraction pipeline is connected to an analysis instrument.

5. The multifunctional light-quality dual-purpose ablation pool according to claim 4, characterized in that: Two aerosol extraction pipeline fixing grooves are symmetrically arranged at the bottom of the laser ablation cell body; a purge pipeline and an extraction pipeline are respectively fixed to the two aerosol extraction pipeline fixing grooves; and the purge pipeline and the extraction pipeline are closely attached to the sample surface.

6. The multifunctional light-quality dual-purpose ablation pool according to claim 4, characterized in that: The sample is fixed in a large chamber and is located below the homogenization chamber.

7. The multifunctional light-quality dual-purpose ablation pool according to claim 5, characterized in that: The multiple auxiliary gas joints and the purge pipeline are perpendicular to each other in a plane.

8. The multifunctional light-quality dual-purpose ablation pool according to any one of claims 1 to 7, characterized in that: The laser ablation pool body is provided with a plurality of fixing holes.

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