CN212301411U - Laser ablation plasma mass spectrometer aerosol sample introduction focusing device - Google Patents
Laser ablation plasma mass spectrometer aerosol sample introduction focusing device Download PDFInfo
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- CN212301411U CN212301411U CN202021814243.6U CN202021814243U CN212301411U CN 212301411 U CN212301411 U CN 212301411U CN 202021814243 U CN202021814243 U CN 202021814243U CN 212301411 U CN212301411 U CN 212301411U
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Abstract
The utility model discloses a laser ablation plasma mass spectrometer aerosol advances appearance focusing device, including the aerosol focusing device, the plasma mass spectrometer, ablation pond and laser instrument, the sample of waiting to erode has been placed in the ablation pond, carrier gas aerosol transports to the carrier gas aerosol hose that the ablation pond other end is connected, the inlet nozzle of carrier gas aerosol hose connection aerosol focusing device, semi-permeable membrane pipe rear end is connected with the outlet nozzle, the seal box surrounds the semi-permeable membrane pipe and forms aerosol focusing device cavity, install electronic flashboard on the mouth of pipe outside of losing air, pressure in the control aerosol focusing device cavity, carrier gas aerosol in the center tube is through the atomization, get into plasma physique spectrometer after the ionization, detect the element that awaits measuring in the aerosol; the utility model discloses an exhaust carrier gas increases the ion concentration who gets into the element that awaits measuring in the plasma mass spectrograph to improve the sensitivity of instrument, effectively improve the limit of detection of the element that awaits measuring under the condition that does not change other instrument devices.
Description
Technical Field
The utility model relates to a chemical analysis technical field, concretely relates to laser ablation plasma mass spectrograph aerosol advances appearance focusing arrangement.
Background
Plasma mass spectrometers have become an important member of analytical instruments in the fields of analytical chemistry and geochemistry due to their superior elemental detection capabilities. The application of the compound is more and more extensive in a plurality of fields such as environment, geology, medicine, agriculture and the like. Due to the need of scientific research work combined with the ultra-strong analysis capability of ICPMS, the technology of performing micro-area in-situ analysis on samples is more and more mature at present. Instruments suitable for carrying out micro-area in-situ analysis on a sample currently comprise an electronic probe, a secondary particle probe and laser ablation plasma mass spectrometry. Laser ablation-ICP-MS is an accurate and precise in situ analysis technique for trace elements in solids, including natural and artificial silicates, carbonates, oxides, and sulfides.
The laser ablation technology is that laser generated by a laser device is focused on the surface of a sample to be detected through a laser light path, aerosol particles generated on the surface of the ablated sample are conveyed to plasma through carrier gas to be atomized and ionized, and then the aerosol particles are introduced into a mass spectrometer to be subjected to element or isotope analysis. The amount of the element to be measured which finally enters the MS mass analyzer after ionization by the plasma torch is less than 1 percent of the aerosol amount. In order to improve the sensitivity and precision of the LA-ICPMS instrument analysis. Previous research efforts have focused on measures such as changing the wavelength of laser light (1064nm, 532nm, 266nm, 248nm, 222nm, 213nm, 193nm, 157nm), changing the shape of ablation cells, adding a smoother to aerosol piping, and changing the shape of sample cone (S cone and Jet cone) skimmer cones (X cone and H cone). The performance of the instrument is greatly improved. The determination of elements in some ultra-low content samples (such as the ultra-low content uranium lead determination in quartz) is nonetheless very difficult. Therefore, an aerosol sample introduction focusing device of a laser ablation plasma mass spectrometer is urgently needed to be designed so as to solve the problem that low-content elements in a sample cannot be detected.
SUMMERY OF THE UTILITY MODEL
To the problem that exists among the prior art, the utility model aims to provide a laser ablation plasma mass spectrograph aerosol advances a kind focusing device.
The utility model provides a technical scheme that its technical problem adopted is: laser ablation plasma mass spectrometer aerosol advances a kind focusing device, including aerosol focusing device, plasma mass spectrometer, ablation pond and laser instrument, it has to wait to erode the sample to have placed in the ablation pond, it forms the aerosol to wait to erode the sample through the irradiation of laser instrument, ablation pond one side is connected with the gas cylinder, carrier gas and aerosol in the gas cylinder form carrier gas aerosol in the ablation pond, carrier gas aerosol transports to the carrier gas aerosol hose that the ablation pond other end is connected, the inlet pipe mouth of carrier gas aerosol hose connection aerosol focusing device, inlet pipe mouth rear end is connected with the semi-permeable membrane pipe, the semi-permeable membrane pipe adopts frustum type structure and inside cavity, be used for oozing out the carrier gas, semi-permeable membrane pipe rear end is connected with the outlet pipe mouth, inlet pipe mouth and outlet pipe mouth are installed relatively on the tank wall of seal box, the seal box surrounds the semi-permeable membrane and forms the aerosol focusing device cavity, be equipped with two snuffl, an electric flashboard is arranged on the outer portion of the air leakage pipe orifice and used for controlling the pressure in the cavity of the aerosol focalizer, the rear end of the air outlet pipe orifice is connected with a central pipe of the plasma rectangular pipe through a transition hose, and carrier gas aerosol in the central pipe enters the plasma mass spectrometer through an interface after being subjected to atomization and ionization of ICP (inductively coupled plasma) and is used for detecting elements to be detected in the aerosol.
Specifically, the rear end of the laser refracts laser through an installed lens, and a focusing objective lens is installed below the lens and used for focusing and irradiating the laser on a sample to be ablated in an ablation pool.
Specifically, a camera with a microscope is mounted above the lens and used for observing and recording laser ablation.
Specifically, the pipe wall of the semi-permeable membrane pipe adopts a microporous tubular semi-permeable membrane frustum type pipe, and the semi-permeable membrane pipe adopts polytetrafluoroethylene or a siliceous material.
Specifically, the inner diameter of one end of the semi-permeable membrane tube is 4mm consistent with that of the air inlet tube opening, and the inner diameter of the other end of the semi-permeable membrane tube is 2mm or 1mm consistent with that of the air outlet tube opening.
Specifically, the carrier gas adopts helium or argon or a mixed gas of the helium and the argon, and the helium or the argon passes through the outside of the semi-permeable membrane under the action of pressure.
Specifically, the electric flashboard of the air release pipe orifice is connected with the controller through a communication line and used for controlling the opening of the air release pipe orifice, and the air release pipe orifice at one end is connected with a purge air pipe as required and used for exhausting carrier gas in the cavity of the aerosol focalizer.
Specifically, the interface is a sampling cone and a truncated cone.
Specifically, the seal box is made of transparent polytetrafluoroethylene.
The utility model discloses following beneficial effect has:
the utility model discloses a laser ablation plasma mass spectrometer aerosol advances a kind focusing device increases the aerosol concentration that gets into in the plasma torch through discharging the carrier gas, reaches the element ion concentration that awaits measuring in the increase plasma torch, makes the element ion number that awaits measuring that gets into LA-ICPMS mass analyzer through interface (sampling awl and intercepting awl) increase to improve the sensitivity of instrument, effectively improve the detection limit of the element that awaits measuring under the condition that does not change other instrument devices; the designed electric flashboard automatically controls the opening size of the air leakage pipe orifice, controls the pressure in the cavity of the aerosol focuser and controls the discharge amount of carrier gas; the device has the advantages of easily available materials, simple structure, convenient manufacture, simple and convenient operation, low cost and easy popularization and application.
Drawings
Fig. 1 is a schematic diagram of a work flow structure of a laser ablation plasma mass spectrometer.
Fig. 2 is a schematic structural diagram of a laser ablation plasma mass spectrometer aerosol sample introduction focusing device.
In the figure: 1-an aerosol focuser; 2-a plasma mass spectrometer; 3-denudation pool; 4-plasma rectangular tube; 5-a laser; 6-camera with microscope; 7-a lens; 8-a sample to be denudated; 9-a gas cylinder; 10-a focusing objective lens; 11-carrier gas aerosol hose; 101-aerosol focuser cavity; 102-a seal box; 103-semipermeable membrane tube; 104-an air inlet pipe orifice; 105-an outlet nozzle; 106-air leakage pipe orifice; 107-carrier gas aerosol flow direction; 401-sampling cone; 402-a truncated cone; 403-a cold gas inlet; 404-central tube.
Detailed Description
The technical solution in the embodiments of the present invention will be described in further detail in the following clearly and completely with reference to the accompanying drawings in the embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
As shown in fig. 1-2, the laser ablation plasma mass spectrometer aerosol sample introduction focusing device includes an aerosol focusing device 1, a plasma mass spectrometer 2, an ablation tank 3, a plasma rectangular tube 4, a laser 5 and a camera 6 with a microscope, wherein the rear end of the laser 5 refracts laser through an installed lens 7, and a focusing objective lens 10 is installed below the lens 7 and is used for focusing and irradiating the laser on a sample 8 to be ablated in the ablation tank 3. Above the lens 7 is mounted a camera 6 with a microscope for observing and recording laser ablation.
A sample 8 to be ablated is placed in the ablation pool 3, the sample 8 to be ablated generates aerosol through laser irradiation of the laser 5, one side of the ablation pool 3 is connected with a gas cylinder 9, carrier gas and the aerosol contained in the gas cylinder 9 form carrier gas aerosol in the ablation pool, the carrier gas adopts helium or argon or mixed gas of the helium and the argon, the helium or the argon penetrates out of the semi-permeable membrane under the pressure effect, and the carrier gas transports the carrier gas aerosol to a carrier gas aerosol hose 11 connected with the other end of the ablation pool 3.
The carrier gas aerosol enters an air inlet pipe orifice 104 of the aerosol focalizer 1 connected with the rear end through a carrier gas aerosol hose 11, the rear end of the air inlet pipe orifice 104 is connected with a semi-permeable membrane pipe 103, the semi-permeable membrane pipe 103 is of a frustum structure and hollow inside and is used for seepage of carrier gas, the pipe wall of the semi-permeable membrane pipe 103 is a microporous tubular semi-permeable membrane frustum type pipe, and the semi-permeable membrane pipe 103 is made of polytetrafluoroethylene or siliceous materials. The rear end of the semi-permeable membrane tube 103 is connected with an air outlet tube opening 105, the air inlet tube opening 104 and the air outlet tube opening 105 are oppositely arranged on the wall of the sealing box 102, the sealing box 102 surrounds the semi-permeable membrane tube 103 to form an aerosol focuser cavity 101, two air leakage tube openings 106 are arranged on the wall of the sealing box 102, an electric flashboard is arranged on the outer portion of each air leakage tube opening 106 and used for controlling the pressure in the aerosol focuser cavity 101, the electric flashboards of the air leakage tube openings 106 are connected with a controller through communication lines and used for controlling the opening degree of the air leakage tube openings 106, and a blowing and sweeping air tube is connected to the air leakage tube openings 106 at one end as required and used for discharging carrier gas in the aerosol focuser cavity 101 so as to ensure that the flow rate of the carrier gas concentrated in the semi-permeable membrane tube 103 enters a central tube 404 of the plasma rectangular tube 4. The pressure in the aerosol focuser cavity 101 is controlled, the discharge amount of the carrier gas is controlled, and the carrier gas can be discharged at an increased speed by connecting with a purge gas.
The rear end of the air outlet pipe opening 105 enters a central pipe 404 of the plasma rectangular pipe 4 through a transition hose, and carrier gas aerosol in the central pipe 404 enters the plasma mass spectrometer 2 through an interface (a sampling cone 401 and a cutting cone 402) after being atomized and ionized by ICP (inductively coupled plasma) of the plasma rectangular pipe 4, so as to be used for detecting elements to be detected in the aerosol.
The inner diameter of one end of the semi-permeable membrane tube 103 is consistent with that of the air inlet pipe orifice 104 and is 4mm, the inner diameter of the other end of the semi-permeable membrane tube 103 is consistent with that of the air outlet pipe orifice 105 and is 2mm or 1mm, and the caliber of the semi-permeable membrane tube is consistent with that of a central tube 404 of the plasma rectangular tube 4. The sealing box 102 is made of transparent polytetrafluoroethylene.
The device is added to a laser ablation plasma mass spectrometer and comprises the following working steps:
1) laser emitted by the laser 5 is refracted by the lens 7, and then is focused by the focusing objective lens 10 to enable the laser beam to be irradiated onto a sample 8 to be ablated in the ablation tank 3, so that aerosol is formed in the ablation tank 3;
2) the carrier gas in the gas cylinder 9 conveys the aerosol into a carrier gas aerosol hose 11, then enters the semi-permeable membrane tube 103 through the gas inlet pipe orifice 104, the controller controls the electric flashboard to open the gas leakage pipe orifice 106, the carrier gas generates pressure difference inside and outside the semi-permeable membrane tube 103 due to the reduction of the outlet in the semi-permeable membrane tube 103, and the carrier gas is discharged out of the semi-permeable membrane tube 103 through the micropores and is discharged through the gas leakage pipe orifice;
3) the concentration of the carrier gas aerosol after carrier gas removal is increased, so that the ion concentration of the element to be detected in the plasma is increased, and the element to be detected enters the plasma mass spectrometer 2 through the central tube 404, the sampling cone 401 and the intercepting cone 402 to detect the element to be detected.
The device improves the sensitivity of the instrument and effectively improves the detection limit of the element to be detected under the condition of not changing other instrument devices.
The utility model discloses not be limited to above-mentioned embodiment, anybody should learn the structural change who makes under the teaching of the utility model, all with the utility model discloses have the same or close technical scheme, all fall into the utility model discloses an within the protection scope.
The technology, shape and construction parts which are not described in detail in the present invention are all known technology.
Claims (9)
1. A laser ablation plasma mass spectrometer aerosol sample introduction focusing device is characterized by comprising an aerosol focusing device, a plasma mass spectrometer, an ablation pool and a laser, wherein a sample to be ablated is placed in the ablation pool, the sample to be ablated forms aerosol through irradiation of the laser, one side of the ablation pool is connected with a gas cylinder, carrier gas and the aerosol in the gas cylinder form carrier gas aerosol in the ablation pool, the carrier gas aerosol is conveyed into a carrier gas aerosol hose connected with the other end of the ablation pool, the carrier gas aerosol hose is connected with a gas inlet pipe orifice of the aerosol focusing device, the rear end of the gas inlet pipe orifice is connected with a semi-permeable membrane pipe, the semi-permeable membrane pipe adopts a frustum type structure and is hollow inside and used for seeping carrier gas, the rear end of the semi-permeable membrane pipe is connected with a gas outlet pipe orifice, the gas inlet pipe orifice and the gas outlet pipe orifice are oppositely arranged on the wall of a sealing box, the wall of the seal box is provided with two air leakage nozzles, the electric flashboards are arranged outside the air leakage nozzles and used for controlling the pressure in the cavity of the aerosol focuser, the rear end of the air leakage nozzle is connected with the central tube of the plasma rectangular tube through a transition hose, and carrier gas aerosol in the central tube enters the plasma mass spectrometer through the interface after the atomization and ionization of ICP and is used for detecting elements to be detected in the aerosol.
2. The laser ablation plasma mass spectrometer aerosol sample introduction focusing device according to claim 1, wherein the rear end of the laser refracts laser light through a lens, and a focusing objective lens is mounted below the lens and used for focusing and irradiating the laser light on a sample to be ablated in the ablation tank.
3. The laser ablation plasma mass spectrometer aerosol sample introduction focusing device according to claim 2, wherein a camera with a microscope is installed above the lens for observing and recording laser ablation.
4. The laser ablation plasma mass spectrometer aerosol sample introduction focusing device according to claim 1, wherein the wall of the semi-permeable membrane tube is a microporous tubular semi-permeable membrane frustum type tube, and the semi-permeable membrane tube is made of polytetrafluoroethylene or siliceous materials.
5. The laser ablation plasma mass spectrometer aerosol sample introduction focusing device according to claim 1, wherein the inner diameter of one end of the semi-permeable membrane tube is consistent with that of the air inlet tube orifice and is 4mm, and the inner diameter of the other end of the semi-permeable membrane tube is consistent with that of the air outlet tube orifice and is 2mm or 1 mm.
6. The laser ablation plasma mass spectrometer aerosol sample feeding and focusing device as claimed in claim 1, wherein the carrier gas is helium or argon or a mixture of helium and argon, and the helium or argon passes through the outside of the semi-permeable membrane under the pressure.
7. The laser ablation plasma mass spectrometer aerosol sample introduction focusing device according to claim 1, wherein the electric flashboard of the air leakage orifice is connected with the controller through a communication line for controlling the opening of the air leakage orifice, and a purge gas pipe is connected with the air leakage orifice at one end as required for discharging carrier gas in the cavity of the aerosol focalizer.
8. The laser ablation plasma mass spectrometer aerosol sample introduction focusing device of claim 1, wherein the interface is a sampling cone and a skimmer cone.
9. The laser ablation plasma mass spectrometer aerosol sample introduction focusing device according to claim 1, wherein the seal box is made of transparent polytetrafluoroethylene.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021814243.6U CN212301411U (en) | 2020-08-27 | 2020-08-27 | Laser ablation plasma mass spectrometer aerosol sample introduction focusing device |
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| CN202021814243.6U CN212301411U (en) | 2020-08-27 | 2020-08-27 | Laser ablation plasma mass spectrometer aerosol sample introduction focusing device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117110175A (en) * | 2023-09-02 | 2023-11-24 | 上海凯来仪器有限公司 | Femtosecond laser ablation mass spectrum flow type all-in-one machine and application method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117110175A (en) * | 2023-09-02 | 2023-11-24 | 上海凯来仪器有限公司 | Femtosecond laser ablation mass spectrum flow type all-in-one machine and application method thereof |
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