CN117110020B - Automatic online solution laser ablation pond - Google Patents
Automatic online solution laser ablation pond Download PDFInfo
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- CN117110020B CN117110020B CN202311376796.6A CN202311376796A CN117110020B CN 117110020 B CN117110020 B CN 117110020B CN 202311376796 A CN202311376796 A CN 202311376796A CN 117110020 B CN117110020 B CN 117110020B
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- laser
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- sealing cover
- digestion tank
- moving platform
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- 238000000608 laser ablation Methods 0.000 title claims abstract description 43
- 230000029087 digestion Effects 0.000 claims abstract description 107
- 230000007246 mechanism Effects 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000010439 graphite Substances 0.000 claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000007789 sealing Methods 0.000 claims description 88
- 239000000443 aerosol Substances 0.000 claims description 45
- 239000007789 gas Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 15
- 239000000741 silica gel Substances 0.000 claims description 15
- 229910002027 silica gel Inorganic materials 0.000 claims description 15
- 239000012159 carrier gas Substances 0.000 claims description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 13
- 239000011737 fluorine Substances 0.000 claims description 13
- 229910052731 fluorine Inorganic materials 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 8
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 8
- 210000001503 joint Anatomy 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 12
- 238000002133 sample digestion Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 46
- 239000000523 sample Substances 0.000 description 30
- 230000005540 biological transmission Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 101150035751 GSP2 gene Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 238000011298 ablation treatment Methods 0.000 description 1
- 229910052612 amphibole Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005383 fluoride glass Substances 0.000 description 1
- 239000010438 granite Substances 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydroxide ions Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000000095 laser ablation inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000004427 solution nebulization inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating 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
- G01N27/626—Investigating 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
- G01N27/628—Investigating 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
Abstract
The invention discloses an automatic on-line solution laser ablation pool, which belongs to the technical field of solution laser ablation and comprises the following components: the laser ablation device comprises a three-dimensional moving platform, a laser ablation mechanism and a manipulator; a plurality of digestion tanks are fixed on the high-temperature graphite heating plate and are fixed with the three-dimensional moving platform through a manipulator; the three-dimensional moving platform moves the digestion tank to a position corresponding to the laser ablation mechanism, and the laser ablation mechanism can perform laser ablation on the solution in the digestion tank; the method and the device realize the analysis from sample digestion to online laser digestion solution analysis so as to obtain data, save a plurality of intermediate links, and provide an automatic online solution laser digestion tank which is efficient, avoids flow pollution, saves energy and protects environment and can be seamlessly combined with automatic digestion equipment for sample pretreatment.
Description
Technical Field
The invention relates to the technical field of solution laser ablation, in particular to an automatic online solution laser ablation tank.
Background
Inductive waxy plasma mass spectrometry (ICP-MS) is a high-precision element and isotope analysis technology and is widely used in the field of earth science. The conventional sampling mode of ICP-MS is a solution atomization method (SN), an aqueous solution introduced by the solution atomization method is a main source of hydrogen and oxygen in plasma, and the interference of oxides and hydroxides corresponding to the two elements is one of the most difficult interference types in the traditional ICP-MS analysis. For example, when testing rare earth elements in geological samples, the samples can be interfered by oxide and hydroxide ions from Ba elements, especially for samples with Ba content significantly higher than the rare earth elements, such as International geological Standard GSP-2 (granite amphibole); when the light rare earth content in the sample is significantly higher than the medium heavy rare earth, the former will also have a significant impact on the testing of the latter.
As the solution atomization method has the above-mentioned drawbacks, the art gradually adopts new sample introduction methods, such as laser ablation. The laser ablation method is originally a sample injection technology of a solid sample, and has the advantages of being in situ and micro-area, and being gradually applied to a solution sample after the solid sample is not needed to be digested. The method adopts the laser ablation solution sample to introduce ICP-MS for element or isotope analysis, on one hand, the problems of low transmission efficiency, large sample consumption, high multi-atom ion interference related to solvents, serious matrix effect and memory effect and the like of the existing SN-ICP-MS analysis technology are overcome; on the other hand, the method remarkably expands the applicable sample type range of LA-ICP-MS, so that the method extends the traditional solid micro-area analysis field to liquid samples such as natural waters of underground water, river water, pore water, sea water and the like, liquid minerals of brine, petroleum and the like, environmental forensic tools of wine, honey and the like, solution samples prepared by various pretreatment methods and the like.
The solution laser ablation technology disclosed in patent CN 201811383157.1 is to dilute and fix the volume of the digested (pre-ablation treatment) sample solution, extract 15uL of the obtained solution, inject the extracted solution into a hole groove or other grooves with different shapes with the aperture of 2mm of the solution sample target, and then put the solution sample target into a conventional solid laser ablation pool for ablation; in the process, sample solution sample replacement is complicated, a solution sample target is not easy to clean and flow pollution is easy to generate, and batch analysis and automation cannot be realized. However, the automatic digestion equipment is commonly used for sample digestion in modern laboratories, and the existing solution digestion technology cannot be connected with the automatic digestion equipment, so that the experimental progress is slow.
In view of the foregoing, it is an urgent need in the art to provide a solution laser ablation apparatus that can automate solution laser ablation and can be used in conjunction with an automatic digestion apparatus.
Disclosure of Invention
The invention aims to provide an automatic online solution laser ablation pool, which solves the problems existing in the prior art and can realize the automation of solution laser ablation and the linkage use with automatic digestion equipment.
In order to achieve the above object, the present invention provides the following solutions: the invention provides an automatic online solution laser ablation pool, which comprises:
the three-dimensional moving platform can move along the X-axis, Y-axis and Z-axis directions;
the digestion carrier is fixed with a plurality of digestion tanks and can be detachably connected with the three-dimensional moving platform;
the digestion carrier and the three-dimensional mobile platform can be connected and fixed by the mechanical arm;
and the three-dimensional moving platform can move the digestion tank to a position corresponding to the laser digestion mechanism, and the laser digestion mechanism can perform laser digestion on the solution in the digestion tank.
Further, the digestion carrier is a high-temperature graphite heating plate, a plurality of fixing holes are formed in the high-temperature graphite heating plate, and the digestion tank is installed in the fixing holes.
Further, the laser ablation mechanism includes:
the laser is arranged adjacent to the three-dimensional moving platform;
one end of the bracket is fixed on the ground, the other end of the bracket extends towards the direction of the three-dimensional moving platform, and the bracket is positioned above the digestion carrier after the digestion carrier is fixedly connected with the three-dimensional moving platform; the bracket is provided with a total reflection mirror and a focusing mirror;
the laser sealing cover is used for reflecting laser beams emitted by the laser through the total reflection mirror and focusing the laser beams through the focusing mirror, and then emitting the laser beams from the laser sealing cover, and the laser sealing cover corresponds to the central position of the tank opening of the digestion tank.
Further, the method further comprises the following steps: the calcium fluoride lens is clamped between the two lens fluorine rubber sealing rings and is fixed in the lens mounting holes through the lens thread pressing rings.
Further, the laser digestion tank further comprises a silica gel sealing ring, the silica gel sealing ring is fixedly arranged on the bottom surface of the laser sealing cover, and when the digestion tank moves upwards and is close to the laser sealing cover, the silica gel sealing ring can seal the laser sealing cover and the digestion tank.
Further, the method further comprises the following steps:
the carrier gas inlet connector is communicated with the laser sealing cover in a sealing way through a connector fluorine rubber sealing ring, an air inlet pipeline is arranged in the laser sealing cover, one end of the air inlet pipeline is communicated with the carrier gas inlet connector, the other end of the air inlet pipeline extends to the lower part of the laser sealing cover, and when the laser sealing cover is in butt joint with the digestion tank, the other end of the air inlet pipeline is communicated with the digestion tank;
the aerosol is discharged out of the connector, the aerosol is discharged out of the connector and is communicated with the laser sealing cover in a sealing way through the connector fluorine rubber sealing ring, an air outlet pipeline is arranged in the laser sealing cover, one end of the air outlet pipeline is communicated with the aerosol discharging connector, the other end of the air outlet pipeline extends to the lower portion of the laser sealing cover, and when the laser sealing cover is in butt joint with the digestion tank, the other end of the air outlet pipeline is communicated with the digestion tank.
Further, the device also comprises an aerosol self-extraction pipe, wherein the aerosol self-extraction pipe is fixedly arranged in the air outlet pipeline, and one end, which is close to the digestion tank, of the aerosol self-extraction pipe extends into the digestion tank and is close to the liquid level of the solution sample in the digestion tank.
Further, the aerosol self-extracting tube is a telescopic tube, the included angle between the aerosol self-extracting tube and the liquid level of the solution sample is 35 degrees, and the distance between one end of the aerosol self-extracting tube, which is close to the digestion tank, and the center of the liquid level of the solution sample is 8mm.
The invention discloses the following technical effects:
1. solution sample is cleared up the equipment through automatic clear back accessible manipulator and shifts to carry out online laser ablation solution analysis and then obtain data in the equipment that this application disclosed fast, has saved other intermediate links, efficient, avoid the flow pollution, energy-concerving and environment-protective.
2. The digestion tanks can be sequentially moved to the lower part of the laser ablation mechanism through the three-dimensional moving platform to perform laser ablation operation, so that the technical effect of automatic online solution laser ablation test is realized. The automatic digestion equipment for sample pretreatment and the laser ablation equipment can be used in a linkage way by combining a mechanical arm.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a schematic diagram of the connection of a laser sealing cap to a digestion tank;
1, a laser; 2. a laser beam; 3. a total reflection mirror; 4. a focusing mirror; 5. a laser sealing cover; 6. a three-dimensional mobile platform; 7. a digestion tank; 8. a high temperature graphite heating plate; 9. a bracket; 10. a carrier gas inlet connection; 11. an aerosol outlet fitting; 12. a lens thread pressing ring; 13. a calcium fluoride lens; 14. an aerosol self-extraction tube; 15. a joint fluorine rubber sealing ring; 16. a lens fluorine rubber sealing ring; 17. a silica gel sealing ring; 18. the solution sample level.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
Referring to fig. 1-2, the present invention provides an automatic on-line solution laser ablation cell comprising: the three-dimensional moving platform 6, the three-dimensional moving platform 6 can move along the directions of the X axis, the Y axis and the Z axis, the specific model of the three-dimensional moving platform 6 is unlimited, as long as the three-dimensional moving platform can drive the digestion carrier and the digestion tanks 7 to move along the three axes, the moving stroke can reach the outline dimension of the digestion carrier, and each digestion tank 7 can be ensured to move to the position corresponding to the laser ablation mechanism, and the embodiment is not repeated; the digestion carrier is fixedly provided with a plurality of digestion tanks 7 and can be detachably connected with the three-dimensional moving platform 6; the digestion carrier and the three-dimensional moving platform 6 can be connected and fixed by the mechanical arm; and the three-dimensional moving platform 6 can move the digestion tank 7 in the digestion carrier to a position corresponding to the laser digestion mechanism, and the laser digestion mechanism can perform laser digestion on the solution in the digestion tank 7.
In this embodiment, the digestion carrier is a high-temperature graphite heating plate 8, a plurality of fixing holes are formed in the high-temperature graphite heating plate 8, and the digestion tank 7 is installed in the fixing holes. The three-dimensional moving platform 6 is provided with a bayonet lock, the bottom of the high-temperature graphite heating plate 8 is provided with a plurality of spacing fixed clamping grooves, and the manipulator can realize the connection fixation of the high-temperature graphite heating plate 8 and the three-dimensional moving platform 6 by clamping the spacing fixed clamping grooves to the bayonet lock.
In this embodiment, the laser ablation mechanism includes: the laser 1, the laser 1 is set up adjacent to three-dimensional moving platform 6; the support 9, one end of the support 9 is fixed on the ground, the other end extends towards the direction of the three-dimensional moving platform 6, and the support 9 is positioned above the digestion carrier after the digestion carrier is fixedly connected with the three-dimensional moving platform 6; the bracket 9 is provided with a total reflection mirror 3 and a focusing mirror 4; the laser sealing cover 5, the laser beam 2 emitted by the laser 1 is reflected by the total reflection mirror 3 and focused by the focusing mirror 4, and then emitted from the laser sealing cover 5, and the laser sealing cover 5 corresponds to the central position of the tank mouth of the digestion tank 7. The laser sealing cover 5 is made of PFA material; the outer diameter is 65mm, the thickness is 10-20 mm (15 mm in the embodiment), two M5 countersunk screw holes are arranged for fixing the bracket 9. The bracket 9 is made of stainless steel, and the surface of the bracket 9 is provided with anticorrosive treatment of teflon. The parameter setting and the movement of the laser 1, the three-dimensional moving platform 6, the manipulator and the automatic digestion equipment for sample pretreatment are automatically controlled by a software program.
In this embodiment, further comprising: the calcium fluoride lens 13, the laser seal lid 5 runs through the upper and lower surface and has seted up the lens mounting hole, and calcium fluoride lens 13 centre gripping is between two lens fluorine rubber sealing washer 16 and is fixed in the lens mounting hole through lens screw thread clamping ring 12. The center of the laser sealing cover 5 is provided with a laser transmission window, an M20 fine thread is arranged, and a sealing groove is arranged at a position corresponding to the contact position of the sealing cover. After the calcium fluoride glass is placed, the laser transmission window and the laser sealing cover 5 are sealed through a sealing groove, the outer diameter of the sealing groove is 13mm, and the width is 1mm. The outer diameter of the lens thread pressing ring 12 is M22 fine threads, the wire diameter of the lens fluorine rubber sealing ring 16 is 1mm, the outer diameter is 11mm, in order to ensure the transmittance, the thickness of the calcium fluoride lens 13 is 0.4mm, and the diameter is 14.9mm.
In this embodiment, the laser digestion tank further comprises a silica gel sealing ring 17, the silica gel sealing ring 17 is fixedly arranged on the bottom surface of the laser sealing cover 5, and when the digestion tank 7 moves upwards and approaches to the laser sealing cover 5, the silica gel sealing ring 17 can seal the laser sealing cover 5 and the digestion tank 7. The outer diameter of the silica gel sealing ring 17 is slightly larger than the tank opening of the digestion tank 7 and the laser transmission window of the laser sealing cover 5, the thickness of the silica gel sealing ring is set to be 2-5 mm (5 mm in the embodiment), and the solution sample with the liquid level difference smaller than 4mm in the digestion tank 7 can be finely tuned and focused due to the softer characteristic of the silica gel material.
Further, the method further comprises the following steps: the carrier gas inlet connector 10, the carrier gas inlet connector 10 is communicated with the laser sealing cover 5 in a sealing way through the connector fluorine rubber sealing ring 15, an inlet pipeline is arranged in the laser sealing cover 5, one end of the inlet pipeline is communicated with the carrier gas inlet connector 10, the other end of the inlet pipeline extends to the lower part of the laser sealing cover 5, and when the laser sealing cover 5 is in butt joint with the digestion tank 7, the other end of the inlet pipeline is communicated with the digestion tank 7; the aerosol gas outlet joint 11, the aerosol gas outlet joint 11 is communicated with the laser sealing cover 5 in a sealing way through the joint fluorine rubber sealing ring 15, a gas outlet pipeline is arranged in the laser sealing cover 5, one end of the gas outlet pipeline is communicated with the aerosol gas outlet joint 11, the other end of the gas outlet pipeline extends to the lower part of the laser sealing cover 5, and when the laser sealing cover 5 is in butt joint with the digestion tank 7, the other end of the gas outlet pipeline is communicated with the digestion tank 7. The device also comprises an aerosol self-extraction pipe 14, wherein the aerosol self-extraction pipe 14 is fixedly arranged in the air outlet pipeline, one end of the aerosol self-extraction pipe, which is close to the digestion tank 7, extends into the digestion tank 7 and is close to the solution sample liquid level 18 in the digestion tank 7, so that the degraded aerosol is rapidly extracted and transmitted, and serious element split caused by vortex is prevented. The inner diameter of the carrier gas inlet joint 10 and the aerosol outlet joint 11 is 3mm, the outer diameter is 4.5mm, the carrier gas inlet joint can be quickly inserted into a conventional air pipe with the outer diameter of 6mm and the inner diameter of 4mm, and the carrier gas is helium. In order to reduce aerosol attachment, the bore of the carrier gas inlet fitting 10 and the aerosol outlet fitting 11 are specular. The outer diameter of the mounting groove of the fluorine rubber sealing ring is 7mm, and the width is 1mm. . In order to ensure the optimal focusing and extraction distance between the air inlet of the aerosol self-extracting tube 14 and the liquid level 18 of the solution sample, the other side of the aerosol self-extracting tube 14 is provided with M3 threads, the included angle between the aerosol self-extracting tube 14 and the center of the liquid level in the digestion tank 7 is 35 degrees, the distance between the end face of the tube orifice of the aerosol self-extracting tube 14 and the center of the liquid level 18 of the solution sample is 8mm, and the aerosol self-extracting tube can stretch up and down by 0-8 mm. Larger aerosol particles and solution droplets degraded by laser are not easy to be adsorbed on the aerosol self-extraction tube 14, so that unreal element content and error are avoided, the aerosol degraded by the laser 1 is sucked into an aerosol air outlet joint 11 connected with the aerosol self-extraction tube 14 by the aerosol self-extraction tube 14, and the sample aerosol is transmitted into an inductively coupled plasma mass spectrum for analysis and detection.
The specific working process is as follows:
and the mechanical arm moves the high-temperature graphite heating plate 8 and the digestion tanks 7 of the high-temperature graphite heating plate 8, which are subjected to digestion and constant volume completion, in the automatic digestion equipment to the three-dimensional moving platform 6 according to a set program, and correspondingly clamps the limiting fixing clamping grooves and the clamping pins, so that the high-temperature graphite heating plate 8 and the three-dimensional moving platform 6 are fixedly connected.
The three-dimensional moving platform 6 sequentially moves the plurality of digestion tanks 7 to the lower side of the laser sealing cover 5 according to a set program, and then the three-dimensional moving platform 6 drives the digestion tanks 7 to move upwards, so that the tank openings of the digestion tanks 7 are tightly attached to the silica gel sealing ring 17, and the silica gel sealing ring 17 seals the tank openings of the digestion tanks 7.
The laser 1 is started, the laser beam 2 emitted by the laser 1 is reflected by the total reflection mirror 3 and focused by the focusing mirror 4, and finally is emitted into the digestion tank 7 from the laser transmission window in the laser sealing cover 5 through the calcium fluoride lens 13, so that the solution sample in the digestion tank 7 is subjected to laser ablation. In the laser ablation process, helium enters the digestion tank 7 from the carrier gas inlet joint 10, aerosol from the extraction pipe 14 after being ablated by the laser 1 is adsorbed, flows to the gas outlet pipeline from the aerosol, and finally the sample aerosol is transmitted to the inductively coupled plasma mass spectrum from the aerosol gas outlet joint 11 for analysis and detection.
The invention provides an automatic online solution laser ablation pool, which can quickly transfer a solution sample to equipment disclosed by the application through a manipulator for online laser ablation solution analysis after the solution sample is digested by automatic digestion equipment, so that data are obtained, other intermediate links are omitted, the efficiency is high, the process pollution is avoided, and the automatic online solution laser ablation pool is energy-saving and environment-friendly.
The digestion tanks can be sequentially moved to the lower part of the laser ablation mechanism through the three-dimensional moving platform to perform laser ablation operation, so that the technical effect of automatic online solution laser ablation test is realized. The automatic digestion equipment for sample pretreatment and the laser ablation equipment can be used in a linkage way by combining a mechanical arm.
In the description of the present invention, it should be understood that the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (3)
1. An automatic on-line solution laser ablation cell comprising:
a three-dimensional moving platform (6), wherein the three-dimensional moving platform (6) can move along the X-axis, Y-axis and Z-axis directions;
the digestion carrier is fixedly provided with a plurality of digestion tanks (7) and can be detachably connected with the three-dimensional moving platform (6);
the digestion carrier and the three-dimensional moving platform (6) can be connected and fixed by the mechanical arm;
the three-dimensional moving platform (6) can move the digestion tank (7) to a position corresponding to the laser digestion mechanism, and the laser digestion mechanism can perform laser digestion on a solution in the digestion tank (7); the laser ablation mechanism includes:
the laser (1) is arranged adjacent to the three-dimensional moving platform (6);
the support (9), one end of the support (9) is fixed on the ground, the other end extends towards the direction of the three-dimensional moving platform (6), and the support (9) is positioned above the digestion carrier after the digestion carrier is fixedly connected with the three-dimensional moving platform (6); the bracket (9) is provided with a total reflection mirror (3) and a focusing mirror (4);
the laser sealing cover (5), the laser beam (2) emitted by the laser (1) is reflected by the total reflection mirror (3) and focused by the focusing mirror (4) and then emitted from the laser sealing cover (5), and the laser sealing cover (5) corresponds to the central position of the tank opening of the digestion tank (7);
further comprises: the laser sealing cover (5) penetrates through the upper surface and the lower surface and is provided with a lens mounting hole, and the calcium fluoride lens (13) is clamped between two lens fluorine rubber sealing rings (16) and is fixed in the lens mounting hole through a lens thread pressing ring (12);
the silica gel sealing ring (17), the silica gel sealing ring (17) is fixedly arranged on the bottom surface of the laser sealing cover (5), and when the digestion tank (7) moves upwards and is close to the laser sealing cover (5), the silica gel sealing ring (17) can seal the laser sealing cover (5) and the digestion tank (7);
the carrier gas air inlet connector (10), the carrier gas air inlet connector (10) is communicated with the laser sealing cover (5) in a sealing way through a connector fluorine rubber sealing ring (15), an air inlet pipeline is arranged in the laser sealing cover (5), one end of the air inlet pipeline is communicated with the carrier gas air inlet connector (10), the other end of the air inlet pipeline extends to the lower part of the laser sealing cover (5), and when the laser sealing cover (5) is in butt joint with the digestion tank (7), the other end of the air inlet pipeline is communicated with the digestion tank (7);
the aerosol gas outlet connector (11), the aerosol gas outlet connector (11) is communicated with the laser sealing cover (5) in a sealing way through a connector fluorine rubber sealing ring (15), a gas outlet pipeline is arranged in the laser sealing cover (5), one end of the gas outlet pipeline is communicated with the aerosol gas outlet connector (11), the other end of the gas outlet pipeline extends to the lower part of the laser sealing cover (5), and when the laser sealing cover (5) is in butt joint with the digestion tank (7), the other end of the gas outlet pipeline is communicated with the digestion tank (7);
the aerosol is from extracting tube (14), aerosol from extracting tube (14) fixed set up in the pipeline of giving vent to anger, it is close to one end of digestion tank (7) extend to in digestion tank (7) and be close to solution sample liquid level (18) setting in digestion tank (7).
2. The automatic online solution laser ablation tank according to claim 1, wherein the digestion carrier is a high-temperature graphite heating plate (8), a plurality of fixing holes are formed in the high-temperature graphite heating plate (8), and the digestion tank (7) is installed in the fixing holes.
3. An automatic on-line solution laser ablation cell according to claim 1, wherein the aerosol self-extraction tube (14) is a telescopic tube, the angle between the aerosol self-extraction tube (14) and the solution sample liquid level (18) is 35 °, and the distance between the end of the aerosol self-extraction tube (14) close to the digestion tank (7) and the liquid level center is 8mm.
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