A double cone cleaning device for the interface of inductively coupled plasma mass spectrometer

Abstract

The present invention discloses a double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer. The cleaning device includes a numerical control workbench, on which a mobile grinding device, an abrasive paste coating device, and a fixed cone rotating device are provided. The abrasive paste coating device contains abrasive paste. The numerical control workbench also includes a waste recovery device and a three-dimensional numerical control controller. The device provides a new formula of abrasive paste, and applies the newly formulated abrasive paste to the double cone through the abrasive paste coating device. The mobile grinding device and the fixed cone rotating device are used to perform mechanical and chemical reaction grinding and cleaning on the double cone coated with the abrasive paste. The device has the technical effects of saving time and labor in machine operation, avoiding personal injury, high numerical control accuracy, effective removal of salt accumulation on the double cone surface, increasing the service life of the double cone, and improving the accuracy of analysis results and the sensitivity and stability of the analytical instrument.

Description

Technical Field

[0001] The invention belongs to the technical field of analytical instruments, and in particular relates to a double-cone cleaning device for an interface of an inductively coupled plasma mass spectrometer. Background Art

[0002] During the sample measurement process of the inductively coupled plasma mass spectrometer (ICP-MS), the mass spectrometer part of the test work is under high vacuum conditions to ensure the ion transmission efficiency, while the ICP part is a high-temperature ion source working under conventional atmospheric pressure. Therefore, it is necessary to achieve temperature isolation and vacuum transition at the interface between the mass spectrometer part and the ICP part. Usually, a double-cone design, namely a sampling cone and a skimmer cone, is adopted at the interface. The sampling cone has a higher temperature at the cone mouth, while the skimmer cone has a lower temperature at the cone mouth. When the sample ion flow passes through the two cone holes, the solid salts in the sample are deposited near the cone mouth, causing the cone mouth to be blocked and solid salts to be deposited on the surface of the cone, affecting the passage of the ion flow, reducing the sensitivity of the ICP-MS and reducing the stability, thereby affecting the precision and accuracy of the measurement results and affecting the analysis quality of the sample.

[0003] Therefore, the sampling cone and the intercepting cone need to be manually cleaned or replaced regularly to eliminate the solid salt on the cone. The manual cleaning method is that the staff repeatedly scrubs with a cotton swab dipped in dilute nitric acid. However, due to the different molecular structures of the samples of salt accumulated on the double cone, the reaction conditions of the acid and the manual operation strength are all different. It is difficult to eliminate the salt accumulation by relying solely on the manual scrubbing method using acid. In the process of manual scrubbing, on the one hand, the different scrubbing strengths can easily cause deformation of the cone mouth of the double cone, thereby affecting the service life of the double cone and the sensitivity and stability of the analytical instrument. On the other hand, if the staff makes an operational error when using acid, especially strong acid, it will cause serious harm to the body. At the same time, the price of replacing the double cone is also relatively expensive, which has caused a serious economic burden on the analytical testing unit. Therefore, the cleaning of the double cone in the existing technology in ICP-MS has the technical problems of difficult to eliminate salt accumulation, easy to make mistakes during manual cleaning, causing deformation of the cone mouth, reducing the service life of the double cone and reducing the sensitivity and stability of the analytical instrument, causing harm to the staff and high cost of replacing the double cone. Summary of the Invention

[0004] In order to at least solve the technical problems in the above-mentioned background technology, such as the difficulty in removing salt accumulation in the cleaning of the double cone, the easy occurrence of mistakes during manual cleaning causing deformation of the cone mouth, the reduction of the service life of the double cone and the reduction of the sensitivity and stability of the analytical instrument, the harm to the workers and the high cost of replacing the double cone, the present invention provides a double cone cleaning device at the interface of an inductively coupled plasma mass spectrometer. The method provides a new formula of abrasive paste, and applies the new formula of abrasive paste to the cone through a grinding paste application device, and uses a mobile grinding device and a fixed cone rotating device to mechanically grind and chemically clean the double cone coated with the grinding paste. The machine operation saves time and effort, avoids personal injury, has high numerical control accuracy, effectively removes salt accumulation on the surface of the double cone, increases the service life of the double cone, improves the accuracy of the analysis results, and improves the sensitivity and stability of the analytical instrument.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions:

[0006] The present invention provides a double-cone cleaning device at the interface of an inductively coupled plasma mass spectrometer. The cleaning device includes a numerically controlled workbench, on which a movable grinding device, an abrasive paste smearing device, and a fixed-cone rotating device are provided. Abrasive paste is placed in the abrasive paste smearing device. The numerically controlled workbench also includes a waste recovery device and a three-dimensional numerical control controller. The movable grinding device, the abrasive paste storage device, and the fixed-cone rotating device cooperate with each other to clean the double cone. The three-dimensional numerical control controller electrically controls the movable grinding device, the abrasive paste smearing device, the fixed-cone rotating device, and the waste recovery device.

[0007] According to an embodiment of the present invention, the grinding paste comprises aluminum oxide powder, nitric acid, deionized water and a metal chelating agent.

[0008] According to one embodiment of the present invention: the specification of the alumina powder is less than 200 mesh, and the metal chelating agent includes aminotriacetic acid and sodium gluconate.

[0009] According to one embodiment of the present invention: the mass ratio of the alumina powder, nitric acid, deionized water and metal chelating agent is: 1000-2000:10-20:500-1000:20-30; the mass ratio of aminotriacetic acid and sodium gluconate is: 1:1.

[0010] According to one embodiment of the present invention: a cleaning groove is provided on the upper surface of the CNC workbench, a mobile grinding device is placed in the cleaning groove, the mobile grinding device includes a slide rail fixedly installed at the bottom of the cleaning groove, a plurality of through holes are evenly provided on the side of the slide rail, a slider is slidingly provided in the slide rail, an electrically controlled telescopic rod parallel to the side surface of the double cone is fixedly installed on the slider, the end of the electrically controlled telescopic rod away from the slider is connected to a grinding rod with grinding balls through a rotating part, the grinding balls are wrapped with absorbent cotton, and the mobile grinding device also includes a baffle.

[0011] According to one embodiment of the present invention: the electrically controlled telescopic rod includes a hollow tube I fixedly mounted on a slider, a hollow tube II is sleeved inside the hollow tube I, a telescopic cylinder is installed in the hollow tube I and the hollow tube II, the rotating part includes an electrically controlled gear rotatably mounted on the hollow tube II, a polishing rod with grinding balls is fixedly mounted on the electrically controlled gear, and the telescopic cylinder and the electrically controlled gear are electrically connected to a three-dimensional numerical control controller.

[0012] According to one embodiment of the present invention: the fixed cone rotating device is installed in the cleaning tank, the fixed cone rotating device includes a rotating pile passing through the bottom of the cleaning tank, the rotating pile is electrically connected to a variable speed motor, an adjusting clamp is fixedly installed on the rotating pile, the adjusting clamp includes a fixing part with a tightening bolt fixedly installed on the upper surface of the rotating pile, and the fixing part is fixedly connected to a clamping claw.

[0013] According to one embodiment of the present invention: the waste recycling device includes a waste port opened at the bottom of the cleaning tank, the waste port is connected downwardly to a waste pipe, the end of the waste pipe away from the waste port is threadedly connected to a recycling box, and the waste port is installed with an electrically controlled switch valve I for controlling the opening and closing of the waste port.

[0014] According to one embodiment of the present invention: the abrasive paste applying device includes an abrasive paste storage box placed on a CNC workbench, an electrically controlled pressure pump is provided in the abrasive paste storage box, a abrasive paste circulation pipeline pointing to a double cone is installed at the bottom of the abrasive paste storage box, an electrically controlled switch valve II is installed at the connection between the abrasive paste storage box and the abrasive paste circulation pipeline, a sealing plate is fixedly installed at one end of the abrasive paste circulation pipeline away from the abrasive paste storage box, a hollow hose connected to the abrasive paste circulation pipeline is installed on the sealing plate, and a brush head is installed on the hollow hose.

[0015] The technical solution of the present invention is to provide a new formula of abrasive paste, apply the abrasive paste with the new formula to the double cone through a grinding paste applying device, and use a mobile grinding device and a fixed cone rotating device to perform mechanical and chemical reaction grinding and cleaning on the double cone that has been coated with the grinding paste. The method has the technical effects of saving time and labor in machine operation, avoiding personal injury, high numerical control accuracy, effective removal of salt accumulation on the double cone surface, increasing the service life of the double cone, and improving the accuracy of analysis results and the sensitivity and stability of the analysis instrument. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 A simplified diagram of a double-cone cleaning device for an inductively coupled plasma mass spectrometer interface according to the present invention;

[0017] Figure 2 A simplified diagram of a double-cone cleaning device for an inductively coupled plasma mass spectrometer interface according to the present invention;

[0018] Figure 3 An enlarged view of an embodiment of a double-cone cleaning device for an inductively coupled plasma mass spectrometer interface according to the present invention;

[0019] Figure 4 An enlarged view of an embodiment of a double-cone cleaning device for an inductively coupled plasma mass spectrometer interface according to the present invention;

[0020] Figure 5 An enlarged view of an embodiment of a double-cone cleaning device for an inductively coupled plasma mass spectrometer interface according to the present invention;

[0021] Figure 6 An enlarged view of an embodiment of a double-cone cleaning device for an inductively coupled plasma mass spectrometer interface according to the present invention;

[0022] In the figure: 1-CNC workbench, 2-3D CNC controller, 3-cone, 10-cleaning tank, 11-slide rail, 12-through hole, 13-slider, 14-grinding rod, 15-grinding ball, 16-hollow tube I, 17-hollow tube II, 18-electric control gear, 20-rotating pile, 21-tightening bolt, 22-fixing part, 23-clamping claw, 30-waste port, 31-waste pipe, 32-recycling box, 40-abrasive paste storage box, 41-abrasive paste circulation pipeline, 42-sealing plate, 43-hollow hose, 44-brush head. DETAILED DESCRIPTION

[0023] The following will clearly and completely describe the technical solutions of the present invention in conjunction with the drawings in the specification. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0024] Please refer to Figure 1 The present invention provides a double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer. The cleaning device includes a CNC workbench, on which a movable polishing device, an abrasive paste coating device, and a fixed cone rotating device are provided. Abrasive paste is placed in the abrasive paste coating device. The CNC workbench also includes a waste recycling device and a three-dimensional CNC controller; the three-dimensional CNC controller is provided with buttons and knobs corresponding to different functions.

[0025] The mobile grinding device, the grinding paste storage device and the fixed cone rotating device cooperate with each other to clean the double cone, and the three-dimensional numerical control controller electrically controls the mobile grinding device, the grinding paste applying device, the fixed cone rotating device and the waste recycling device.

[0026] The technical solution of the present invention provides a new formula of abrasive paste, and applies the abrasive paste with the new formula to the cone of a double cone (sampling cone or cutting cone) through a grinding paste applying device, and uses a mobile grinding device and a fixed cone rotating device to mechanically and chemically grind and clean the cone coated with the grinding paste. It has the technical effects of saving time and labor in machine operation, avoiding personal injury, high CNC control accuracy, effectively removing salt accumulation on the surface of the double cone, increasing the service life of the double cone, and improving the accuracy of analysis results and the sensitivity and stability of the analysis instrument.

[0027] According to one embodiment of the present invention, the lapping paste comprises aluminum oxide powder, nitric acid, deionized water, and a metal chelating agent. In this embodiment, the mechanical grinding action of the fine abrasive particles in the lapping paste on salt accumulation effectively removes the accumulated salt. The chemical reaction between the nitric acid and the metal chelating agent on the accumulated salt, particularly cationic salt, also effectively removes the accumulated salt. Therefore, this embodiment effectively removes salt accumulated on the surface of the cone.

[0028] According to one embodiment of the present invention, the alumina powder has a size of less than 200 mesh, and the metal chelating agent includes aminotriacetic acid and sodium gluconate. Alumina powder with a size of less than 200 mesh is the optimal particle size for achieving optimal cleaning, as currently discovered in experimental studies. Aminotriacetic acid can chelate metal ions, is stable, and is inexpensive. Sodium gluconate is an excellent all-round chelating agent with excellent chelating properties for a variety of metal ions. Therefore, this embodiment achieves the technical benefits of low cost and strong metal chelating ability for metal ions.

[0029] According to one embodiment of the present invention, the mass ratio of aluminum oxide powder, nitric acid, deionized water, and metal chelating agent is 1000-2000:10-20:500-1000:20-30; and the mass ratio of aminotriacetic acid and sodium gluconate is 1:1. These mass ratios are optimal experimentally determined, achieving the technical effect of cost savings and effectively removing salt from the cone surface.

[0030] Please refer to Figure 2 、 3 And 4, according to one embodiment of the present invention, a cleaning groove is provided on the upper surface of the above-mentioned CNC workbench, and a mobile grinding device is placed in the cleaning groove. The mobile grinding device includes a slide rail fixedly installed at the bottom of the cleaning groove, and a plurality of through holes are evenly provided on the side of the slide rail. A slider is slidingly provided in the slide rail, and an electrically controlled telescopic rod parallel to the side surface of the double cone is fixedly installed on the slider. The end of the electrically controlled telescopic rod away from the slider is connected to a grinding rod with grinding balls through a rotating part, and the grinding balls are wrapped with absorbent cotton. The mobile grinding device also includes a baffle. In this embodiment, the grinding ball is a polyurethane ball processing head, and the slider moves in the slide rail to approach or move away from the fixed cone rotating device to achieve grinding of the surfaces of cones of different volumes. Multiple through holes are evenly and tightly arranged on the side of the slide rail for the baffle to pass through to fix the slider. After the slider is fixed, it no longer moves, and the grinding ball with cotton wool is tightly attached to the surface of the double cone without lateral movement. The horizontal rotation and up and down grinding and cleaning of the double cone are achieved by electrically controlling the extension and contraction of the telescopic rod. Therefore, this embodiment has the technical effect of simple operation and is suitable for double cones of different volumes.

[0031] Please refer to Figure 5 According to one embodiment of the present invention, the electrically controlled telescopic rod comprises a hollow tube I fixedly mounted on a slider, a hollow tube II being sheathed within hollow tube I, and a telescopic cylinder mounted within both hollow tubes I and II. The rotating member comprises an electrically controlled gear rotatably mounted on hollow tube II, a polishing rod with grinding balls being fixedly mounted on the electrically controlled gear, and the telescopic cylinder and the electrically controlled gear are electrically connected to a three-dimensional numerical control controller. In this embodiment, the telescopic cylinder extends and contracts under the control of the three-dimensional numerical control controller to enable the polishing head to polish and clean the cone from top to bottom. The electrically controlled gear rotates forward and reverse under the control of the three-dimensional numerical control controller to control the angle between the polishing rod and the electrically controlled telescopic rod, thereby controlling whether the polishing head is in close contact with the surface of the double cone. This embodiment has the technical advantages of simple configuration, uniform force applied to the polishing surface of the cone, and effectively preventing deformation of the cone caused by uneven force during cleaning.

[0032] According to one embodiment of the present invention, the fixed cone rotation device is installed in a cleaning tank. The fixed cone rotation device includes a rotating pile extending through the bottom of the cleaning tank, the rotating pile being electrically connected to a variable speed motor, and an adjustment fixture fixedly mounted on the rotating pile. The adjustment fixture includes a fixing member with a tightening bolt fixedly mounted on the upper surface of the rotating pile, and the fixing member is fixedly connected to a clamping claw. The adjustment fixture in this embodiment controls the distance between the clamping claws by tightening and loosening the tightening bolt to secure cones of different sizes. Therefore, this embodiment has the technical effect of being simple to operate and capable of securing cones of different sizes.

[0033] According to one embodiment of the present invention, the waste recycling device includes a waste port at the bottom of the cleaning tank, the waste port being connected downwardly to a waste pipe, the end of the waste pipe being threadedly connected to a recycling box away from the waste port, and an electrically controlled on-off valve I installed on the waste port to control the opening and closing of the waste port. The electrically controlled on-off valve I is electrically connected to a three-dimensional numerical control controller, and the recycling box is removably threadedly connected to the waste pipe. After the surface of the cone is cleaned, the solid salt and abrasive paste removed by mechanical grinding and chemical reactions can be flushed into the recycling box, preventing the solid salt and abrasive paste from splashing and contaminating the working environment. The abrasive paste in the recycling box can be separated and purified and then reused to prepare abrasive paste. This has the technical effect of preventing solid salt and abrasive paste from contaminating the working environment, preventing the waste of abrasive paste raw materials, and reducing the cost of abrasive paste.

[0034] Please refer to Figure 6 According to one embodiment of the present invention, the abrasive paste application device includes an abrasive paste storage box placed on a CNC workbench, an electrically controlled pressure pump installed within the abrasive paste storage box, an abrasive paste circulation pipeline directed toward the double cones installed at the bottom of the abrasive paste storage box, an electrically controlled on / off valve II installed at the connection between the abrasive paste storage box and the abrasive paste circulation pipeline, a sealing plate fixedly installed at the end of the abrasive paste circulation pipeline away from the abrasive paste storage box, a hollow hose connected to the abrasive paste circulation pipeline installed on the sealing plate, and a brush head installed on the hollow hose. The electrically controlled pressure pump and electrically controlled on / off valve II are electrically connected to a three-dimensional CNC controller, and the brush head of the hollow hose is made of a soft material, so it can apply to cones of different sizes. Therefore, this embodiment has the technical effect of simple operation and strong applicability.

[0035] The specific implementation of the present invention is as follows: during actual operation, first prepare the grinding paste according to the ratio of the grinding paste, use a three-dimensional numerical control controller to control the closing of the electric control switch valve I and the electric control switch valve II, place the cone (sampling cone or intercepting cone) on the rotating pile, adjust the tightening bolt to make the clamping claw clamp the cone, at this time the long hollow hose and brush head of soft material are close to the surface of the cone, secondly, slide the slider in the slide rail to make the grinding head close to the cone, and the absorbent cotton on the grinding head presses the cone, and fix the slider by inserting the baffle into the through hole, and use the three-dimensional numerical control controller to control the rotation of the electric control gear so that the grinding head is perpendicular to the surface of the cone, and use the three-dimensional numerical control controller to control the extension and contraction of the telescopic cylinder so that the hollow tube II is away from or close to the hollow tube I, so as to realize the horizontal grinding of the cone up and down, and finally the flowing The mud with smaller viscosity is poured into the grinding paste storage box, and the three-dimensional numerical control controller is used to control the electric control switch valve II and the electric control pressure pump to open. The variable speed motor is used to control the rotation of the rotating pile, and the rotating pile drives the cone fixed on it to rotate. At this time, the grinding paste flowing out of the grinding paste circulation pipeline is smeared on the rotating cone through the hollow hose and the brush head, and the solid salt accumulation on the surface of the cone is removed by mechanical grinding and chemical reaction. After the cleaning is completed, the three-dimensional numerical control controller is used to turn off the electric control pressure pump and the electric control switch valve II, and the electric control gear is controlled to rotate to make the grinding head away from the cone, and the baffle is removed from the through hole. The slider is moved in the opposite direction, the variable speed motor is turned off, the tightening bolt is loosened, and the cone is taken out. The three-dimensional numerical control controller is used to open the electric control switch valve I, and the solid salt accumulation and grinding paste in the cleaning tank are blown or flushed into the recovery box.

[0036] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0037] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer, characterized by: The cleaning device includes a CNC workbench, on which a movable grinding device, an abrasive paste applying device, and a fixed cone rotating device are provided. The fixed cone rotating device is used to fix and rotate the vertebral body. The abrasive paste applying device contains abrasive paste. The CNC workbench also includes a waste recovery device and a three-dimensional CNC controller. The mobile grinding device, the grinding paste storage device and the fixed cone rotating device cooperate with each other to clean the cone, and the three-dimensional numerical control controller electrically controls the mobile grinding device, the grinding paste applying device, the fixed cone rotating device and the waste recycling device; The grinding paste comprises aluminum oxide powder, nitric acid, deionized water and a metal chelating agent; The specification of the alumina powder is less than 200 mesh, and the metal chelating agent includes aminotriacetic acid and sodium gluconate; A cleaning groove is provided on the upper surface of the CNC workbench, and a mobile grinding device is placed in the cleaning groove. The mobile grinding device includes a slide rail fixedly installed at the bottom of the cleaning groove, and a plurality of through holes are evenly provided on the side of the slide rail. A slider is slidably provided in the slide rail, and an electrically controlled telescopic rod parallel to the side surface of the double cone is installed on the slider. The end of the electrically controlled telescopic rod away from the slider is connected to a grinding rod with a grinding ball through a rotating member, and the grinding ball is wrapped with absorbent cotton. The mobile grinding device also includes a baffle; Mechanical grinding and chemical reaction are used to remove solid salt deposits on the surface of the vertebral body.

2. The double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer according to claim 1, characterized in that: The mass ratio of the aluminum oxide powder, nitric acid, deionized water and metal chelating agent is 1000-2000:10-20:500-1000:20-30; the mass ratio of aminotriacetic acid and sodium gluconate is 1:

1.

3. The double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer according to claim 1, characterized in that: The electrically controlled telescopic rod includes a hollow tube I fixedly mounted on a slider, a hollow tube II is sleeved inside the hollow tube I, a telescopic cylinder is installed inside the hollow tube I and the hollow tube II, the rotating part includes an electrically controlled gear rotatably mounted on the hollow tube II, a polishing rod with grinding balls is fixedly mounted on the electrically controlled gear, and the telescopic cylinder and the electrically controlled gear are electrically connected to a three-dimensional numerical control controller.

4. The double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer according to claim 1, characterized in that: The fixed cone rotating device is installed in the cleaning tank, and the fixed cone rotating device includes a rotating pile passing through the bottom of the cleaning tank, the rotating pile is electrically connected to a variable speed motor, and an adjusting clamp is fixedly installed on the rotating pile. The adjusting clamp includes a fixing part with a tightening bolt fixedly installed on the upper surface of the rotating pile, and the fixing part is fixedly connected to a clamping claw.

5. The double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer according to claim 1, characterized in that: The waste recycling device includes a waste port opened at the bottom of the cleaning tank, the waste port is connected downwardly to a waste pipe, the end of the waste pipe away from the waste port is threadedly connected to a recycling box, and the waste port is equipped with an electrically controlled switch valve I for controlling the opening and closing of the waste port.

6. The double-cone cleaning device for the interface of an inductively coupled plasma mass spectrometer according to claim 1, characterized in that: The abrasive paste applying device includes an abrasive paste storage box placed on a CNC workbench, an electrically controlled pressure pump is provided in the abrasive paste storage box, a abrasive paste circulation pipeline pointing to the cone is installed at the bottom of the abrasive paste storage box, an electrically controlled switch valve II is installed at the connection point between the abrasive paste storage box and the abrasive paste circulation pipeline, a sealing plate is fixedly installed at one end of the abrasive paste circulation pipeline away from the abrasive paste storage box, a hollow hose connected to the abrasive paste circulation pipeline is installed on the sealing plate, and a brush head is installed on the hollow hose.

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