ICPMS automatic sampling device

Abstract

The invention discloses an ICPMS (Inductively Coupled Plasma Mass Spectrometer) automatic sampling device, which belongs to the technical field of mass spectrometers, and comprises an atomizing chamber, an atomizer and a peristaltic pump which are arranged on a main machine body, the atomizer is connected with a liquid inlet pipe and a working gas pipe, the atomizer is mounted on a mounting pipe on the atomizing chamber, a liquid outlet of the atomizing chamber is provided with a liquid outlet pipe, and the liquid outlet pipe is connected with a liquid outlet of the atomizing chamber. A sample inlet pipe of the atomizing chamber is connected with an auxiliary air pipe, a mounting pipe is provided with a mounting hole, a cleaner is mounted in the mounting hole and comprises an arc-shaped pipe and an arc-shaped rod, the arc-shaped pipe is provided with a negative pressure connector, and the negative pressure connector is externally connected with a negative pressure device. As an outlet channel of the atomizer is extremely small, cleaning is carried out mostly in an acid liquor soaking or hair dredging mode, cleaning is inconvenient, and the cleaning period is long.

Description

Technical Field

[0001] The invention belongs to the technical field of mass spectrometers, and in particular relates to an ICPMS automatic sample injection device. Background Art

[0002] ICPMS (Inductively Coupled Plasma Mass Spectrometer) is an instrument widely used for elemental analysis and isotope analysis. The high-temperature plasma generated by inductively coupled plasma is used as the sample introduction system, and the sample is analyzed for elemental and isotopic content by mass spectrometry, which has the advantages of high sensitivity, high resolution and high throughput. ICP-MS can not only be used to analyze and measure the content of trace elements in substances, but also provide information on the isotope ratio of elements. Therefore, it has a wide range of applications in earth sciences, environmental monitoring and life sciences. The sampling system of ICPMS mainly forms an aerosol state through a nebulizer, and is brought into the center of the plasma torch by a carrier gas (usually argon), where evaporation, decomposition, excitation and ionization occur. During atomization, the sample is sent into the nebulizer through a peristaltic pump to form an aerosol and enter the nebulizer chamber. Since the sample contains a lot of salt, the nebulizer is often easily blocked during use, and the nebulizer needs to be removed for cleaning or replacement. At the same time, since the nebulizer outlet channel is extremely small and there are no suitable cleaning tools, most of the cleaning is done by soaking in acid or clearing with hair, which is inconvenient and takes a long time. Summary of the invention

[0003] Based on the problems mentioned in the above background technology, the present invention provides an ICPMS automatic sampling device, which is used to solve the problem that the ICPMS nebulizer needs to be disassembled for cleaning or replacement when it is blocked. Since the nebulizer outlet channel is extremely small and there are no suitable cleaning tools, most of the cleaning is done by acid immersion or hair cleaning, which is inconvenient and takes a long time.

[0004] The technical solution adopted by the present invention is as follows:

[0005] An ICPMS automatic sample injection device comprises an atomization chamber, an atomizer and a peristaltic pump arranged on a main body, the atomizer is connected to a liquid inlet pipe and a working air pipe, the atomizer is mounted on a mounting pipe on the atomization chamber, a liquid discharge pipe is mounted on a liquid discharge port of the atomization chamber, an auxiliary air pipe is connected to a sample injection pipe of the atomization chamber, the liquid discharge pipe and the liquid inlet pipe are both clamped in the peristaltic pump, a mounting hole is opened on the mounting pipe, a cleaner is mounted in the mounting hole, the cleaner comprises a concentric arc tube and an arc rod, pistons are mounted on the ends and the middle of the arc rod, and pistons are mounted on the ends. A flexible cleaning wire is installed on the piston of the part, the piston is slidably installed in the arc tube, a rubber sealing ring is installed in the installation hole, the arc tube is slidably penetrated in the rubber sealing ring, a rubber plug is installed at one end of the arc tube located in the installation tube, a flare and a guide hole are provided at both ends of the rubber plug, when the flare is sleeved on the nozzle of the atomizer, the outlet on the nozzle corresponds to the guide hole, a sealing plug is installed at the end of the arc tube, the arc rod is penetrated in the sealing plug, a ventilation groove is provided on the outer wall of the piston, a negative pressure interface is provided on the arc tube, and a negative pressure device is externally connected to the negative pressure interface.

[0006] On the basis of the above technical solution, the present invention further makes the following improvements:

[0007] Furthermore, the rubber plug is provided with a contraction cavity at the expanded position. When the arc tube is moved to cover the rubber plug at the expanded position on the outlet of the atomizer, the expanded position is more likely to shrink under the action of the contraction cavity, so that the atomizer port is more likely to be embedded in the rubber plug, thereby maintaining a good sealing performance, and avoiding the negative pressure device from sucking out the debris that blocks the atomizer when cleaning the atomizer.

[0008] Furthermore, a shifting block is installed on the sealing plug, and a shifting ball is installed on the arc-shaped rod. The shifting block facilitates pulling the arc-shaped tube, and the shifting ball facilitates pulling the arc-shaped rod, which is convenient for operation.

[0009] Furthermore, a support is provided on the mounting tube, and the support includes a fixedly connected arc-shaped support block and a binding belt, the binding belt is fixed on the mounting tube, the circle where the curved surface of the arc-shaped support block is located is concentric with the circle where the arc-shaped tube is located, and the sealing plug contacts the arc-shaped support block. During the process of pulling the arc-shaped tube, the arc-shaped support block can support and stabilize one end of the arc-shaped tube, which can prevent stress concentration from causing the arc-shaped tube to rupture.

[0010] Furthermore, a monitoring tube is provided on the atomizing chamber, a humidity monitor is installed on the monitoring tube, and the monitoring probe of the humidity monitor is located in the monitoring tube. The humidity in the atomizing chamber can be monitored, and since the peristaltic pump feed is stable, the atomizer can maintain a relatively stable atomization state without being blocked, so the blockage of the atomizer can be judged by the change of humidity in the atomizing chamber, so as to facilitate timely cleaning.

[0011] Furthermore, a mixing component is installed on the main body, and the mixing component includes a base and a placing table. The base is provided with a bayonet, and the main body is provided with a block matching the bayonet. The base is installed on the block, and the placing table is located on the base, and a universal ball is installed at the bottom. A vortex spring is connected between the base and the placing table, and a motor is installed on the base. An eccentric piece is installed on the output shaft of the motor, and the eccentric piece is rotatably connected to the placing table. The motor drives the placing table to move through the eccentric piece, and the placing table cannot rotate under the restriction of the vortex spring and can only be shaken slightly with the eccentric piece, so that the sample container placed on the placing table can be shaken to mix the sample.

[0012] Furthermore, a stabilizer is installed on the placement table, and the stabilizer includes a base and two clamping blocks. The base is fixedly connected to the placement table, and spring plates are connected between the base and the two clamping blocks. Under the action of the spring plates, the clamping blocks can be moved closer to the middle, so that the sample container on the placement table can be stabilized by the clamping blocks of the stabilizer to prevent the sample container from tipping over when the placement table shakes.

[0013] Furthermore, a magnetic sheet is installed on the base, and the base is fixed on the placement table through the magnetic sheet. The stabilizer is easy to disassemble and install, and can be adjusted at any time according to usage requirements.

[0014] Furthermore, the liquid inlet pipe is connected to a water inlet ball, which includes a sphere and a sleeve, the sphere is provided with a water inlet hole near the sleeve, and the liquid inlet pipe is inserted into the sleeve. After the liquid inlet pipe is inserted into the sleeve, the height of the port of the liquid inlet pipe can be limited under the action of the sphere, so as to prevent the liquid inlet pipe from touching the bottom when placed in the sample container.

[0015] Beneficial effects of the present invention:

[0016] By moving the arc tube, the rubber plug at one end of the arc tube can be set on one end of the nozzle of the atomizer, and then by moving the arc rod, the flexible cleaning wire can be deflected under the action of the guide hole so that any one of the wires can be inserted into the atomizer, thereby cleaning the clogged atomizer. At the same time, the cleaning debris can be sucked out with the help of the negative pressure device to complete the cleaning of the clogged atomizer. The cleaning is convenient and the operation is relatively simple. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The present invention can be further illustrated by means of non-limiting examples given in the accompanying drawings;

[0018] Figure 1 A schematic diagram of the layout of an ICPMS device in an embodiment of the present invention Figure 1 ;

[0019] Figure 2 A schematic diagram of the layout of an ICPMS device in an embodiment of the present invention Figure 2 ;

[0020] Figure 3 The structure of the atomizer assembly in the embodiment of the present invention is shown in FIG. Figure 1 ;

[0021] Figure 4 Schematic diagram of the longitudinal structure of the atomization assembly in an embodiment of the present invention;

[0022] Figure 5 The structure of the atomizer assembly in the embodiment of the present invention is shown in FIG. Figure 2 ;

[0023] Figure 6 for Figure 5 A schematic diagram of the enlarged structure at A in the middle;

[0024] Figure 7 A schematic diagram of the longitudinal structure of the atomizing assembly when cleaning the atomizer according to an embodiment of the present invention;

[0025] Figure 8 for Figure 7 The enlarged structure diagram at B in the middle;

[0026] Fig. 9 for Figure 8 The enlarged structure diagram at C in the middle;

[0027] Fig.10 It is a schematic diagram of the longitudinal section structure of the atomizing assembly when the atomizer is cleaned according to the present invention;

[0028] Fig.11 for Fig.10 The enlarged structure at D in the middle is shown;

[0029] Fig.12 The structure of the mixing assembly in the embodiment of the present invention is shown in FIG. Figure 1 ;

[0030] Fig.13 The structure of the mixing assembly in the embodiment of the present invention is shown in FIG. Figure 2 ;

[0031] Fig.14 This is a schematic diagram of the structure of the water inlet ball in an embodiment of the present invention;

[0032] The main component symbols are described as follows:

[0033] Main body 1, atomization chamber 20, monitoring tube 201, injection tube 21, discharge port 22, discharge tube 221, liquid inlet tube 23, sphere 231, sleeve 232, water inlet hole 233, working air pipe 24, auxiliary air pipe 25, installation tube 26, monitoring probe 27, atomizer 3, peristaltic pump 4, mixing assembly 5, base 51, bayonet 511, placement table 52, universal ball 521, stabilizer 53, base 531, spring 532, clamping block 533, sample container 54, motor 55, eccentric piece 551, vortex spring 56, strap 61, arc support block 62, rubber sealing ring 63, arc tube 64, negative pressure interface 641, sealing plug 65, shift block 651, arc rod 66, piston 661, ventilation groove 662, flexible cleaning wire 663, shift ball 67, rubber plug 68. DETAILED DESCRIPTION

[0034] In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0035] like Figures 1 to 8As shown, an ICPMS automatic sample injection device includes an atomization assembly and a peristaltic pump 4 arranged on a main body 1, the atomization assembly includes an atomization chamber 20, an atomizer 3, the atomizer 3 is connected to a liquid inlet pipe 23 and a working air pipe 24, the atomizer 3 is installed on a mounting pipe 26 on the atomization chamber 20, a liquid discharge pipe 221 is installed on the liquid discharge port 22 of the atomization chamber 20, an auxiliary air pipe 25 is connected to the sample injection pipe 21 of the atomization chamber 20, the liquid discharge pipe 221 and the liquid inlet pipe 23 are both clamped in the peristaltic pump 4, and the peristaltic pump 4 simultaneously squeezes the liquid discharge pipe 221 and the liquid inlet pipe 23 to introduce the sample into the atomizer 3 while sucking out the waste liquid in the atomization chamber 20 when the peristaltic pump 4 is running. A mounting hole is opened on the mounting pipe 26, and a cleaner is installed in the mounting hole, and the cleaner includes a concentric arc tube 64 and an arc rod 66. The end and the middle of the arc rod 66 are both equipped with pistons 661, which are slidably installed in the arc tube 64. The arc rod 66 is stabilized by two pistons 661 so as to move along the arc tube 64, so that the arc rod 66 and the arc tube 64 are kept in a concentric state. The piston 661 at the end is equipped with a flexible cleaning wire 663. In this embodiment, the flexible cleaning wire 663 adopts PE wire, which has good softness and does not damage the atomizer 3. It can also maintain high toughness to better dredge the atomizer 3. The number of flexible cleaning wires 663 is 3 to 9, so that the flexible cleaning wires 663 can smoothly penetrate into the atomizer 3, and other flexible cleaning wires 663 that have not entered will not form a large resistance when bending by themselves due to the small number. A rubber sealing ring 63 is installed in the mounting hole, and the arc tube 64 is slidably inserted into the rubber sealing ring 63. A rubber plug 68 is installed at one end of the arc tube 64 located in the mounting tube 26. Both ends of the rubber plug 68 are provided with flared openings 681 and guide holes 683. After one end of the arc tube 64 overlaps with one end of the atomizer 3, the port of the atomizer 3 can be automatically inserted into the flared opening 681. When the expansion port 681 is sleeved on the nozzle of the atomizer 3, the outlet on the nozzle corresponds to the guide hole 683, so that the flexible cleaning wire 663 is also inserted into the atomizer 3 along the guide hole 683. A sealing plug 65 is installed at the end of the arc tube 64, and the arc rod 66 is inserted in the sealing plug 65. A ventilation groove 662 is opened on the outer wall of the piston 661. A negative pressure interface 641 is provided on the arc tube 64. The negative pressure interface 641 is externally connected to a negative pressure device. The negative pressure device generates negative pressure to absorb the debris generated by dredging through the ventilation groove 662. When cleaning is not needed, the end piston 661 is contacted with the guide hole 683 of the rubber plug 68 to close the arc tube 64 to prevent the aerosol in the atomization chamber 20 from entering the arc tube 64.

[0036] like Fig. 9As shown, the rubber plug 68 is provided with a convergence cavity 682 at the position of the flared opening 681. When the arc tube 64 is moved to put the rubber plug 68 on the outlet of the atomizer 3 at the flared opening 681, the flared opening 681 is more easily contracted under the action of the convergence cavity 682, so that the port of the atomizer 3 is more easily embedded in the rubber plug 68, thereby maintaining a better sealing performance, and avoiding the negative pressure device from sucking out the debris that blocks the atomizer 3 when cleaning the atomizer 3.

[0037] like Figure 6 As shown, a shifting block 651 is installed on the sealing plug 65, and a shifting ball 67 is installed on the arc rod 66. The shifting block 651 is convenient for pulling the arc tube 64, and the shifting ball 67 is convenient for pulling the arc rod, so as to facilitate operation.

[0038] like Figure 6 As shown, a support member is provided on the mounting tube 26, and the support member includes a fixedly connected arc-shaped support block 62 and a strap 61, the strap 61 is fixed on the mounting tube 26, the circle where the curved surface of the arc-shaped support block 62 is located is concentric with the circle where the arc-shaped tube 64 is located, and the sealing plug 65 is in contact with the arc-shaped support block 62. During the process of pulling the arc-shaped tube 64, the arc-shaped support block 62 can support and stabilize one end of the arc-shaped tube 64, thereby preventing stress concentration from causing the arc-shaped tube 64 to rupture.

[0039] like Figure 3 to Figure 5 As shown, a monitoring tube 201 is provided on the atomization chamber 20, and a humidity monitor is installed on the monitoring tube 201. The monitoring probe 27 of the humidity monitor is located in the monitoring tube 201, and the humidity in the atomization chamber can be monitored. Since the peristaltic pump feed is stable, the atomizer 3 can maintain a relatively stable atomization state without being blocked, so the blockage of the atomizer 3 can be judged by the change of the humidity in the atomization chamber, so as to facilitate timely cleaning.

[0040] like Figure 1 , Fig.12 , Fig.13 As shown, a mixing assembly 5 is installed on the main body 1, and the mixing assembly 5 includes a base 51 and a placing table 52. A bayonet 511 is opened on the base 51, and a block matching the bayonet 511 is provided on the main body 1. The base 51 is installed on the block, and the placing table 52 is located on the base 51, and a universal ball 521 is installed at the bottom end. A vortex spring 56 is connected between the base 51 and the placing table 52. A motor 55 is installed on the base 51, and an eccentric piece 551 is installed on the output shaft of the motor 55. The eccentric piece 551 is rotatably connected to the placing table 52. The motor 55 drives the placing table 52 to move through the eccentric piece 551. Under the restriction of the vortex spring 56, the placing table 52 cannot rotate and can only be shaken slightly with the eccentric piece 551, so that the sample container 54 placed on the placing table 52 can follow the shaking to mix the sample.

[0041] like Fig.12 , Fig.13As shown, a stabilizer 53 is installed on the placement table 52, and the stabilizer 53 includes a base 531 and two clamping blocks 533. The base 531 is fixedly connected to the placement table 52, and spring pieces 532 are connected between the base 531 and the two clamping blocks 533. Under the action of the spring pieces 532, the clamping blocks 533 can be moved toward the middle, so that the sample container 54 on the placement table 52 can be stabilized by the clamping blocks 533 of the stabilizer 53 to prevent the sample container 54 from tipping over when the placement table 52 shakes.

[0042] Specifically, a magnetic sheet is installed on the base 531, and the base 531 is fixed on the placement table 52 through the magnetic sheet. The stabilizer 53 is easy to disassemble and install, and can be adjusted at any time according to usage requirements.

[0043] like Fig.14 As shown, the liquid inlet pipe 23 is connected to a water inlet ball, which includes a sphere 231 and a sleeve 232. The sphere 231 is provided with a water inlet hole 233 near the sleeve 232, and the liquid inlet pipe 23 is inserted into the sleeve 232. After the liquid inlet pipe 23 is inserted into the sleeve 232, the height of the port of the liquid inlet pipe 23 can be limited under the action of the sphere 231 to prevent the liquid inlet pipe 23 from touching the bottom when it is placed in the sample container 54.

[0044] When cleaning the atomizer 3, the liquid inlet tube 23 can be removed from the peristaltic pump 4 and the water inlet port can be placed in a sample container containing pure water or dilute nitric acid solution. The negative pressure device is turned on and the arc tube 64 is moved so that the rubber plug 68 is sleeved on the nozzle at one end of the atomizer 3. Then the arc rod 66 is moved so that any part of the flexible cleaning wire 663 located at one end can smoothly penetrate into the nozzle of the atomizer 3 along the guide hole 683 for dredging. At the same time, under the action of negative pressure, the debris generated by cleaning can be sucked out, and the liquid in the sample container can be sucked for cleaning. The dredging of the flexible cleaning wire 663 is convenient for improving the cleaning effect. After the dredging is completed, the flux of the atomizer 3 increases, and whether it is dredged can be judged according to the speed at which the liquid in the sample container decreases. After cleaning, pull the arc tube 64 away from the atomizer 3, and at the same time, make the piston 661 of a section of the arc rod 66 press against the rubber plug 68 (such as Fig.10 , Fig.11 shown).

[0045] The above is a detailed introduction to an ICPMS automatic sample injection device provided by the present invention. The description of the specific embodiment is only used to help understand the method of the present invention and its core idea. It should be pointed out that for ordinary technicians in this technical field, without departing from the principle of the present invention, several improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims

1. An ICPMS automatic sample introduction device, comprising a spray chamber (20), a sprayer (3) and a peristaltic pump (4) arranged on a main body (1), wherein the sprayer (3) is connected to a liquid inlet pipe (23) and a working air pipe (24), the sprayer (3) is installed on a mounting pipe (26) on the spray chamber (20), a liquid discharge pipe (221) is installed on a liquid discharge port (22) of the spray chamber (20), an auxiliary air pipe (25) is connected to a sample introduction pipe (21) of the spray chamber (20), and the liquid discharge pipe (221) and the liquid inlet pipe (23) are both clamped in the peristaltic pump (4), characterized in that: The mounting tube (26) is provided with a mounting hole, a cleaner is installed in the mounting hole, the cleaner comprises a concentric arc tube (64) and an arc rod (66), pistons (661) are installed at the end and the middle of the arc rod (66), a flexible cleaning wire (663) is installed on the piston (661) at the end, the piston (661) is slidably installed in the arc tube (64), a rubber sealing ring (63) is installed in the mounting hole, the arc tube (64) is slidably inserted in the rubber sealing ring (63), and the arc tube (64) is located in the mounting tube (26). A rubber plug (68) is installed at one end of the inner portion, and a flared opening (681) and a guide hole (683) are provided at both ends of the rubber plug (68). When the flared opening (681) is sleeved on the nozzle of the atomizer (3), the outlet on the nozzle corresponds to the guide hole (683). A sealing plug (65) is installed at the end of the arc tube (64), and the arc rod (66) is inserted into the sealing plug (65). A ventilation groove (662) is provided on the outer wall of the piston (661). A negative pressure interface (641) is provided on the arc tube (64), and the negative pressure interface (641) is externally connected to a negative pressure device.

2. An ICPMS automatic sample introduction device according to claim 1, characterized in that: The rubber plug (68) is provided with a contraction cavity (682) at the expansion position (681).

3. An ICPMS automatic sample injection device according to claim 2, characterized in that: The sealing plug (65) is provided with a shifting block (651), and the arc-shaped rod (66) is provided with a shifting ball (67).

4. An ICPMS automatic sample injection device according to claim 3, characterized in that: A support member is provided on the mounting tube (26), and the support member comprises an arc-shaped support block (62) and a binding belt (61) which are fixedly connected. The binding belt (61) is fixed on the mounting tube (26). The circle where the curved surface of the arc-shaped support block (62) is located is concentric with the circle where the arc-shaped tube (64) is located. The sealing plug (65) is in contact with the arc-shaped support block (62).

5. An ICPMS automatic sample injection device according to claim 1, characterized in that: The atomization chamber (20) is provided with a monitoring tube (201), a humidity monitor is installed on the monitoring tube (201), and the monitoring probe (27) of the humidity monitor is located inside the monitoring tube (201).

6. An ICPMS automatic sample injection device according to claim 1, characterized in that: A mixing assembly (5) is installed on the main body (1), and the mixing assembly (5) comprises a base (51) and a placement platform (52). The base (51) is provided with a bayonet (511), and the main body (1) is provided with a block matching the bayonet (511). The base (51) is installed on the block, and the placement platform (52) is located on the base (51) and has a universal ball (521) installed at the bottom. A vortex spring (56) is connected between the base (51) and the placement platform (52). A motor (55) is installed on the base (51), and an eccentric piece (551) is installed on the output shaft of the motor (55). The eccentric piece (551) is rotatably connected to the placement platform (52).

7. An ICPMS automatic sample injection device according to claim 6, characterized in that: A stabilizer (53) is installed on the placement table (52), and the stabilizer (53) comprises a base (531) and two clamping blocks (533). The base (531) is fixedly connected to the placement table (52), and spring sheets (532) are connected between the base (531) and the two clamping blocks (533).

8. An ICPMS automatic sample injection device according to claim 7, characterized in that: A magnetic sheet is mounted on the base (531), and the base (531) is fixed on the placement platform (52) via the magnetic sheet.

9. An ICPMS automatic sample injection device according to claim 1, characterized in that: The liquid inlet pipe (23) is connected to a water inlet ball, the water inlet ball comprises a sphere (231) and a sleeve (232), the sphere (231) is provided with a water inlet hole (233) near the sleeve (232), and the liquid inlet pipe (23) is inserted into the sleeve (232).

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