CN107202731B - Ultrafast multi-outlet laser ablation pool - Google Patents

Ultrafast multi-outlet laser ablation pool Download PDF

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Publication number
CN107202731B
CN107202731B CN201710338858.2A CN201710338858A CN107202731B CN 107202731 B CN107202731 B CN 107202731B CN 201710338858 A CN201710338858 A CN 201710338858A CN 107202731 B CN107202731 B CN 107202731B
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sample cell
sample
insertion type
cell
fast
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CN107202731A (en
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胡兆初
陈力飞
史光予
罗涛
张文
宗克清
刘勇胜
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China University of Geosciences
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China University of Geosciences
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
    • G01N27/628Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas and a beam of energy, e.g. laser enhanced ionisation

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Optics & Photonics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention provides an ultra-fast multi-outlet laser ablation cell, which comprises a sample cell shell and a fast-insertion type sample cell, wherein an observation window and a transmission light window are respectively arranged on the upper surface and the lower surface of the sample cell shell, a sample placing port is formed in the left side surface of the sample cell shell, the fast-insertion type sample cell is fixed in a hollow cavity in the sample cell shell through the sample placing port, the fast-insertion type sample cell is provided with a sample accommodating cavity recessed from the upper surface of the fast-insertion type sample cell, the upper surface and the neck of the fast-insertion type sample cell are hermetically arranged with the sample cell shell, a plurality of parallel air outlet holes are formed in the right side surface of the sample cell shell, a carrier gas inlet hole is formed in the left side surface of the sample cell shell, and the air outlet hole and the carrier gas inlet hole. The invention has the beneficial effects that: can effectively restrain the generation of eddy current and reduce or even eliminate memory effect.

Description

Ultrafast multi-outlet laser ablation pool
Technical Field
The invention relates to the technical field of laser ablation, in particular to an ultra-fast multi-outlet laser ablation pool.
Background
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a new technology for solid analysis generated in the middle and late stages of the 80 s. The LA-ICP-MS technology has the advantages of in-situ, real-time and rapid analysis, higher sensitivity, better spatial resolution, multi-element determination and detection capability for providing isotope ratio information. The technology has been widely applied in the fields of earth science, material science, environmental science, nuclear science and the like. Has become the mainstream conventional mineral micro-area element and isotope analysis instrument.
In laser ablation plasma mass spectrometry, a sample to be detected is firstly placed in a laser ablation pool, and sample aerosol generated on the surface of the laser ablation sample is brought into the plasma mass spectrometry by carrier gas to carry out element and isotope analysis. The design of different laser ablation cells will have a significant impact on elemental analysis signal strength, signal stability, elemental fractionation, and sample preparation efficiency. Vortex is easily generated at the side of the traditional laser ablation pool, so that the serious element fractionation and memory effect are caused, and the transmission of aerosol and the accuracy of an analysis result are finally influenced. The conventional laser ablation pool has the problems that the sample changing time is long, and air is easily mixed in the sample changing process to cause plasma flameout.
The traditional laser ablation pool is provided with only one air outlet corresponding to the air inlet and horizontally penetrates through the side face of the sample chamber. Therefore, in the air outlet process, only the aerosol in the middle of the denudation pool and at the position close to the air outlet is easy to transmit. Because only a single air outlet is used for air outlet, aerosol at a plurality of corner positions cannot be well transmitted, vortex is easy to generate, and the stability of an analysis result is finally influenced. In addition, the sample changing is complicated and frequent and the working efficiency is lower due to the limited number of samples placed in the sample chamber.
The inner diameter of a gas inlet pipeline of a traditional laser ablation pool is generally larger than 0.5mm, the larger the inner diameter of the gas inlet pipeline is, and the lower the gas flow rate is under the condition of certain carrier gas flow. The low gas flow rate results in longer aerosol residence time in the ablation cell, resulting in a more severe memory effect. The lower gas flow velocity at the laser ablation point also leads to the larger particle size of solid aerosol generated by laser ablation, and the larger particle size of the solid aerosol is easier to be incompletely ionized in plasma, thereby generating element fractionation.
Disclosure of Invention
In view of the above, embodiments of the present invention provide an ultrafast multi-outlet laser ablation cell capable of effectively suppressing generation of eddy currents and reducing or even eliminating memory effects.
The embodiment of the invention provides an ultra-fast multi-outlet laser ablation cell, which comprises a sample cell shell and a fast-insertion type sample cell, wherein an observation window and a transmission light window are respectively arranged on the upper surface and the lower surface of the sample cell shell, a sample placing port is formed in the left side surface of the sample cell shell, the fast-insertion type sample cell is fixed in a hollow cavity in the sample cell shell through the sample placing port, the fast-insertion type sample cell is provided with a sample accommodating cavity recessed from the upper surface of the fast-insertion type sample cell, the upper surface and the neck of the fast-insertion type sample cell are hermetically arranged with the sample cell shell, a plurality of parallel air outlet holes are formed in the right side surface of the sample cell shell, a carrier gas inlet hole is formed in the left side surface of the sample cell shell, and the air outlet hole and the carrier gas inlet hole both.
Furthermore, one end of a carrier gas inlet joint penetrates through the front side surface or the rear side surface of the sample chamber shell and is vertically communicated with the carrier gas inlet hole, and one end, close to the outside, of the carrier gas inlet hole is blocked so as to prevent carrier gas from overflowing.
Further, the aperture of the carrier gas inlet hole is 0.2-0.3 mm.
Furthermore, the upper surface of the fast-insertion type sample cell is provided with a fast-insertion type sample cell top sealing ring groove, a fluorine rubber O-shaped sealing ring is placed in the fast-insertion type sample cell, and the upper surface of the fast-insertion type sample cell is sealed with the top of the sample cell shell through the fluorine rubber O-shaped sealing ring.
Furthermore, the neck of the fast-insertion type sample cell is provided with a fast-insertion type sample cell neck sealing ring groove, a fluorine rubber O-shaped sealing ring is placed in the fast-insertion type sample cell neck, and the neck of the fast-insertion type sample cell is sealed with the left end region of the sample chamber shell through the fluorine rubber O-shaped sealing ring.
Furthermore, the upper surface of the sample chamber shell is concavely provided with an observation window accommodating cavity, an observation window sealing ring groove is arranged on the periphery of the side edge of the observation window, a fluorine rubber O-shaped sealing ring is placed in the observation window sealing ring groove, and the periphery of the side edge of the observation window is sealed with the side wall of the observation window accommodating cavity through the fluorine rubber O-shaped sealing ring.
Furthermore, a plurality of semicircular sinking grooves are formed in one side edge of the opening end of the observation window accommodating cavity.
The sample chamber further comprises an air outlet curtain connector, the air outlet curtain connector is provided with a plurality of butt joint holes in butt joint with the air outlet holes, and an air exhaust valve is further arranged on the right side face of the sample chamber shell.
Furthermore, the number of the air outlet holes is 3-6, and the inner diameter of each air outlet hole is 1-3 mm.
Further, the open end of sample placing opening is equipped with the chamfer, still includes the button head handle, insert soon the left surface of formula sample cell seted up with button head handle complex button head handle screw hole.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: according to the ultrafast multi-outlet laser ablation cell, the right side surface of the sample chamber shell is provided with the plurality of air outlets which are arranged in parallel, aerosol in the middle and at the corners of the laser ablation cell can be transmitted simultaneously, so that the serious element fractionation and memory effects caused by the generated vortex can be effectively restrained, and the accuracy of an analysis result is improved by improving the transmission rate of the aerosol.
Drawings
FIG. 1 is a schematic diagram of an overall construction of an ultrafast multi-exit laser ablation cell in accordance with the present invention;
FIG. 2 is a schematic structural view of a sample chamber housing in the ultrafast multi-exit laser ablation cell of FIG. 1;
FIG. 3 is a schematic diagram of a fast-insert sample cell in the ultrafast multi-exit laser ablation cell of FIG. 1;
FIG. 4 is a schematic diagram of a view window in the ultrafast multi-exit laser ablation cell of FIG. 1;
Fig. 5 is a schematic diagram of the structure of the base plate in the ultrafast multi-exit laser ablation tank of fig. 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, an embodiment of the present invention provides an ultrafast multi-exit laser ablation cell, which mainly includes: the sample chamber comprises a sample chamber hollow shell 1, a quick-insertion type sample cell 2 and an observation window 3 which are arranged on the sample chamber hollow shell 1, and a bottom plate 4 for fixing the sample chamber hollow shell 1.
Referring to fig. 2, the sample chamber housing 1 is a hollow structure, that is, a hollow cavity is formed inside, and the hollow cavity is used for accommodating the quick-insertion sample chamber. The upper surface and the lower surface of the sample chamber shell are respectively provided with an observation window 3 and a transmission light window 20, the condition in the hollow cavity can be observed through the observation window 3, and laser can enter the hollow cavity through the transmission light window 20.
A sample placing port 13 is formed in the left side face of the sample chamber shell 1, a chamfer 12 is formed in the opening end of the sample placing port 13, and the quick-insertion type sample cell 2 is fixed in a hollow cavity in the sample chamber shell 1 through the sample placing port 13. A plurality of parallel air outlet holes 9 are formed in the right side face of the sample chamber shell 1, and in the embodiment, the number of the air outlet holes 9 is 3-6, preferably 5. The inner diameter of each air outlet 9 is 1-3 mm, and the inner diameter of each air outlet is preferably 2 mm. The right side surface of the sample chamber shell 1 is further provided with an air outlet curtain connector 6, the air outlet curtain connector 6 is provided with a plurality of butt joint holes in butt joint with the air outlet holes 9, the butt joint holes are in one-to-one butt joint with the corresponding air outlet holes 9, and the number of the butt joint holes is preferably 5. The air outlet 9 is used for collecting the aerosol in the hollow cavity to the air outlet curtain connector 6, so that the aerosol is finally transmitted away by the air outlet curtain connector 6. The right side surface of the sample chamber shell is also provided with an exhaust valve 7, when the quick-insertion type sample cell 2 is placed, the exhaust valve 7 is loosened, air in the hollow cavity is exhausted, and when the quick-insertion type sample cell 2 is placed in place, the exhaust valve 7 is closed, so that aerosol is prevented from flowing out of the exhaust valve 7.
A carrier gas inlet hole 11 is formed in the left side face of the sample chamber shell 1, the carrier gas inlet hole 11 is arranged at a position 1mm below the upper surface of the sample chamber shell 1, the inner diameter of the carrier gas inlet hole 11 is smaller than 0.5mm, specifically 0.2-0.3 mm, and the inner diameter of the carrier gas inlet hole is preferably 0.3 mm. One end of a carrier gas inlet joint 5 penetrates through the front side surface or the rear side surface of the sample chamber shell 1 and is vertically communicated with the carrier gas inlet hole 11, and the left side end of the carrier gas inlet hole 11 is sealed by epoxy resin, so that carrier gas can only flow out from the right side end of the carrier gas inlet hole 11.
The air outlet 9 and the carrier gas inlet 11 both extend inwards to be communicated with the hollow cavity.
Referring to fig. 2 and 4, an observation window accommodating cavity is formed in the upper surface of the sample chamber housing 1 in a downward concave manner, an observation window sealing ring groove 17 is formed around the side edge of the observation window 3, a fluorine rubber O-shaped sealing ring is placed in the observation window sealing ring groove, and the periphery of the side edge of the observation window 3 is sealed with the side wall of the observation window accommodating cavity through the fluorine rubber O-shaped sealing ring. The high lens sheet 18 is arranged on the observation window 3, the thickness of the high lens sheet 18 is 0.4-1 mm, the light transmittance of the high lens sheet is over 90%, and the high lens sheet is beneficial to reducing the loss of laser ablation energy. The viewing window 3 is substantially rectangular.
A plurality of semicircular sinking grooves 10 are formed in one side edge of the opening end of the observation window accommodating cavity, preferably, the number of the semicircular sinking grooves 10 is two, and the two semicircular sinking grooves 10 are mainly used for facilitating disassembly or replacement of the high-lens sheet 18, so that the observation window 3 can be maintained and cleaned conveniently.
Referring to fig. 3, the quick-plug sample cell 2 has a sample receiving cavity recessed from an upper surface thereof, and the sample receiving cavity is used for receiving a sample. The sample containing cavity is positioned under the observation window 3, and the condition in the sample containing cavity can be observed through the observation window 3.
The upper surface of the fast-inserting sample cell 2 is provided with a fast-inserting sample cell top sealing ring groove 15, and the sample accommodating cavity is surrounded by the fast-inserting sample cell top sealing ring groove 15 and is positioned on the inner side of the fast-inserting sample cell top sealing ring groove 15. A fluorine rubber O-shaped sealing ring is placed in the quick-insertion type sample cell top sealing ring groove 15, and the upper surface of the quick-insertion type sample cell 2 is sealed with the top of the sample chamber shell 1 through the fluorine rubber O-shaped sealing ring.
the neck of the fast-insertion type sample cell 2 is provided with a fast-insertion type sample cell neck sealing ring groove 14, a fluorine rubber O-shaped sealing ring is placed in the fast-insertion type sample cell neck, and the neck of the fast-insertion type sample cell 2 is sealed with the left end region of the sample chamber shell 1 through the fluorine rubber O-shaped sealing ring.
The neck and the upper surface of the fast-insertion type sample cell 2 adopt the design of installing a fluorine rubber 0-shaped sealing ring, so that the introduced carrier gas cannot flow to two sides and only can flow into the air outlet curtain connector 6, and the effective volume of the denudation cell is reduced. Discharge valve 7 has been added to the right side end in the pond of ultrafast multi-outlet laser ablation, loosens when the trade appearance discharge valve 7, the air that the trade appearance process was sneaked into can be followed fast discharge valve 7 discharges, has avoided the instrument flame-out problem that conventional loaded down with trivial details consuming time exhaust flow and sneak into the air and lead to, is showing and has improved work efficiency.
referring to fig. 1 and 3, the ultrafast multi-exit laser ablation cell further includes a round-head handle 18, and a round-head handle screw hole 16 matched with the round-head handle 18 is formed on the left side surface of the fast-insertion type sample cell 2. The round-head handle 18 is fixed on the quick-insertion type sample cell 2 through the round-head handle screw hole 16, and the quick-insertion type sample cell 2 can be easily taken out of the sample chamber shell 1 by pulling the round-head handle 18.
referring to fig. 5, the bottom plate 4 is fixed to the corresponding screw hole at the bottom of the sample chamber housing 1 through a M3 flat screw hole, and the bottom plate 4 is substantially rectangular and is placed on a moving slide of a laser ablation system.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: according to the ultrafast multi-outlet laser ablation cell, the right side surface of the sample chamber shell 1 is provided with the plurality of air outlets 9 which are arranged in parallel, aerosol in the middle and at the corners of the laser ablation cell can be transmitted simultaneously, so that the serious element fractionation and memory effects caused by the generated vortex can be effectively restrained, and the accuracy of an analysis result is improved by improving the transmission rate of the aerosol.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. The utility model provides an ultrafast multi-outlet laser ablation pond, includes sample room casing and inserts the formula sample cell soon, the upper surface and the lower surface of sample room casing are equipped with observation window and transmission light window respectively, the sample has been seted up to the left surface of sample room casing and has been placed the mouth, insert the formula sample cell soon and pass through the sample is placed the mouth and is fixed in the well cavity in the sample room casing, its characterized in that: the quick-insertion type sample cell is provided with a sample accommodating cavity recessed from the upper surface of the quick-insertion type sample cell, the upper surface and the neck of the quick-insertion type sample cell are hermetically arranged with the sample cell shell, the right side surface of the sample cell shell is provided with a plurality of parallel air outlet holes, the left side surface of the sample cell shell is provided with a carrier gas inlet hole, and the air outlet holes and the carrier gas inlet hole both extend inwards and are communicated with the sample accommodating cavity; the aperture of the carrier gas inlet hole is 0.2-0.3 mm; 3-6 air outlet holes are formed, and the inner diameter of each air outlet hole is 1-3 mm; the laser ablation cell further comprises an air outlet curtain connector, the air outlet curtain connector is provided with a plurality of butt joint holes in butt joint with the air outlet holes, and an air exhaust valve is further arranged on the right side face of the sample chamber shell.
2. The ultrafast multi-outlet laser ablation cell of claim 1, wherein: one end of a carrier gas inlet joint penetrates through the front side surface or the rear side surface of the sample chamber shell and is vertically communicated with the carrier gas inlet hole, and one end, close to the outside, of the carrier gas inlet hole is blocked so as to prevent carrier gas from overflowing.
3. The ultrafast multi-outlet laser ablation cell of claim 1, wherein: the upper surface of the fast-insertion type sample cell is provided with a fast-insertion type sample cell top sealing ring groove, a fluorine rubber O-shaped sealing ring is placed in the fast-insertion type sample cell, and the upper surface of the fast-insertion type sample cell is sealed with the top of the sample chamber shell through the fluorine rubber O-shaped sealing ring.
4. The ultrafast multi-outlet laser ablation cell of claim 1, wherein: the neck of the fast-insertion type sample cell is provided with a fast-insertion type sample cell neck sealing ring groove, a fluorine rubber O-shaped sealing ring is placed in the fast-insertion type sample cell neck, and the neck of the fast-insertion type sample cell is sealed with the left end region of the sample chamber shell through the fluorine rubber O-shaped sealing ring.
5. the ultrafast multi-outlet laser ablation cell of claim 1, wherein: the upper surface of the sample chamber shell is concavely provided with an observation window accommodating cavity, an observation window sealing ring groove is arranged on the periphery of the side edge of the observation window, a fluorine rubber O-shaped sealing ring is placed in the observation window sealing ring groove, and the periphery of the side edge of the observation window is sealed with the side wall of the observation window accommodating cavity through the fluorine rubber O-shaped sealing ring.
6. The ultrafast multi-outlet laser ablation cell of claim 5, wherein: and a plurality of semicircular sinking grooves are formed in one side edge of the opening end of the observation window accommodating cavity.
7. The ultrafast multi-outlet laser ablation cell of claim 1, wherein: the open end of sample placing port is equipped with the chamfer, still includes the button head handle, the left surface of inserting the sample cell soon seted up with button head handle complex button head handle screw hole.
CN201710338858.2A 2017-05-15 2017-05-15 Ultrafast multi-outlet laser ablation pool Active CN107202731B (en)

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CN110361336A (en) * 2019-07-19 2019-10-22 浙江大学 Efficiently go out sample sample room for microwave plasma torch laser ablation system

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Publication number Priority date Publication date Assignee Title
CN104075932A (en) * 2014-06-19 2014-10-01 袁洪林 Multi-target laser ablation sample chamber

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Publication number Priority date Publication date Assignee Title
CN104777155B (en) * 2015-04-15 2017-06-09 武汉上谱分析科技有限责任公司 A kind of rotating channel formula laser ablation pond

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104075932A (en) * 2014-06-19 2014-10-01 袁洪林 Multi-target laser ablation sample chamber

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Application publication date: 20170926

Assignee: Wuhan Dimande Scientific Instrument Co.,Ltd.

Assignor: CHINA University OF GEOSCIENCES (WUHAN CITY)

Contract record no.: X2022420000142

Denomination of invention: An ultra fast multi outlet laser ablation cell

Granted publication date: 20191210

License type: Common License

Record date: 20221215