Conveniently operated combustion on-line ion chromatography system and use method

Abstract

The application discloses a combustion on-line ion chromatography system convenient to operate, which comprises a workbench, a heating furnace and a first driving unit, a combustion tube, a sample boat chamber and a guide pipe are sequentially connected on the workbench, a push rod is arranged in the guide pipe, the push rod is used for pushing a sample boat from the sample boat chamber into the combustion tube or sending the sample boat from the combustion tube to the sample boat chamber, the sample boat chamber comprises a sample inlet chamber body and a sealing assembly, the sample inlet chamber body comprises a through hollow cavity, the through hollow cavity is communicated with a cavity in the combustion tube and a cavity in the guide pipe, the through hollow cavity is upwardly opened to form a feeding port, the sealing assembly can open or close the feeding port, and the sealing assembly comprises a liquid inlet hole which can be communicated with the feeding port. A use method of the combustion on-line ion chromatography system is adopted. The combustion on-line ion chromatography system is reasonable in structure, convenient for feeding solid and liquid samples, and is favorable for improving the accuracy and stability of detection results.

Description

Technical Field

[0001] This invention relates to the field of ion chromatography detection technology, specifically to a convenient online combustion ion chromatography system and its usage method. Background Technology

[0002] The analysis of elemental content in samples is involved in many fields such as mineral resources, metallurgical engineering, environmental science, and food safety. Ion chromatography is the most commonly used instrument for elemental content analysis. In the process of determining the elemental content of samples using ion chromatography, high-temperature pyrolysis pretreatment of samples has become a highly regarded pretreatment method for elemental analysis in recent years. This method combines the characteristics of high-temperature pyrolysis and water distillation. High-temperature pyrolysis mainly utilizes the volatility of some elements (such as halogens), releasing them from their salts or other compounds in the form of vapor at high temperatures (such as 1100℃). The vapor is then absorbed in a suitable absorbent, thereby achieving the separation and enrichment of the analyte. In existing technologies, to accurately and rapidly determine the elemental content in samples, high-temperature pyrolysis pretreatment of samples is generally performed in the high-temperature combustion tube of the detection equipment.

[0003] In this process, the sample to be tested is typically a solid or liquid. In existing technologies, the sample boat containing the sample is manually placed into the injection chamber to complete the injection operation. However, improper operation can lead to substandard sealing of the sample boat chamber, affecting the accuracy and stability of the test results. Some existing technologies use a drop-feed method for sample boat injection, as shown in patent application CN202220631605.0, entitled "A Sample Boat Chamber for a Combustion Online Ion Chromatography System with Convenient Loading and Unloading." However, when the sample to be tested is a liquid, the shaking of the sample boat during the drop-feed process and the impact of the drop on the sample boat at the front of the push rod often cause the liquid sample to splash out of the sample boat, contaminating the injection chamber and seriously affecting the accuracy and stability of the test results. Summary of the Invention

[0004] This invention discloses a convenient online combustion ion chromatography system and its usage method. It solves the technical problems in existing technologies where liquid samples easily splash and contaminate the injection chamber, affecting the accuracy and stability of detection results. It features a reasonable structure, convenient injection of both solid and liquid samples, and improved accuracy and stability of detection results. The technical solution adopted is as follows:

[0005] A user-friendly online combustion ion chromatography system includes a worktable, a heating furnace, and a first drive unit. The worktable is provided with a combustion tube, a sample boat chamber, and a guide tube connected in sequence. The heating furnace is located on the worktable for heating the combustion tube. The sample boat can be placed within the sample boat chamber. A push rod is provided inside the guide tube. The first drive unit is located on the worktable and can drive the push rod to slide axially along the guide tube to push the sample boat from the sample boat chamber into the combustion tube or to deliver the sample boat from the combustion tube to the sample boat chamber. The sample boat chamber includes an injection chamber body and a sealing assembly. The injection chamber body includes a through hollow cavity communicating with the inner cavity of the combustion tube and the inner cavity of the guide tube. The hollow cavity opens upward to form a feed inlet. The sealing assembly can open or close the feed inlet and includes a liquid inlet hole communicating with the feed inlet.

[0006] Based on the above technical solution, the sealing assembly can slide along the axial direction of the sample inlet body to open or close the inlet; or the first end of the sealing assembly is hinged to the sample inlet body, and the second end of the sealing assembly is connected to the sample inlet body through a locking member to open or close the inlet.

[0007] Based on the above technical solution, a cooling unit for cooling the sample injection chamber body and the sample boat therein is fixed below the sample injection chamber body. The cooling unit includes one or more of a fan, heat dissipation fins or Peltier modules.

[0008] Based on the above technical solution, it also includes a transfer unit and a third driving unit. The transfer unit is designed to allow the transfer unit to inject samples into the sample boat through the liquid inlet and / or the feed inlet under the action of the third driving unit, or to take samples out of and put in the sample boat through the feed inlet.

[0009] Based on the above technical solution, a sample tray for holding sample vials is also included. The sample tray includes a temperature control unit for heating or cooling the sample vials. The transfer unit can extract sample liquid from the sample vials and then inject it into the sample boat under the action of the third drive unit.

[0010] Based on the above technical solution, the end of the push rod is also provided with a support boat for supporting the sample boat upward. The support boat is connected to the end of the push rod and can swing left and right. The support boat includes an upward-opening concave cavity, and the concave cavity is larger at the top and smaller at the bottom.

[0011] Based on the above technical solution, the side wall of the support boat forming the concave cavity includes a notch to facilitate the placement and removal of the sample boat; and the bottom of the support boat includes several through holes.

[0012] Based on the above technical solution, the end of the push rod includes a U-shaped connector. One free end of the U-shaped connector passes vertically through the carrier boat and is hinged to the carrier boat. The bottom surface of the U-shaped connector is not higher than the bottom surface of the carrier boat, so as to avoid the carrier boat forming a cantilever structure.

[0013] Based on the above technical solution, the combustion tube passing through the heating furnace includes an inner tube and an outer tube. The inner tube includes a second tube section and a first tube section arranged axially along the airflow direction. A relatively closed interlayer cavity is formed between the inner tube and the outer tube. The interlayer cavity is connected to the inner cavity of the inner tube through several through holes on the first tube section. A first inlet is connected at the second end of the second tube section extending outside the outer tube. A second inlet is connected at the second end of the interlayer cavity near the second end of the second tube section.

[0014] A method of using a combustion online ion chromatography system, employing the combustion online ion chromatography system as described above, characterized by comprising the following steps:

[0015] S1. Equipment preparation;

[0016] S2. The transfer unit completes the sample injection operation under the action of the third drive unit;

[0017] S3. Remove residual gas, open the first inlet, and introduce a mixture of inert gas and ultrapure water into the inner tube. After a set time, close the first inlet. At the same time, another stream of inert gas enters the inner tube through the guide tube and the sample boat chamber. After a set time, close the guide tube. At the same time, open the second inlet and introduce oxygen into the jacketed cavity to remove residual gas in the inner tube and the jacketed cavity.

[0018] S4. Under the action of the first drive unit, the push rod pushes the sample boat to a set position inside the combustion tube, and the heating furnace preheats the sample in the moving sample boat.

[0019] S5. The push rod continues to move forward under the action of the first drive unit. The sample goes through the preheating, heating, coking and combustion stages. At the same time, inert gas carrying ultrapure water enters the inner tube through the first inlet, another stream of oxygen enters the inner tube through the sample boat chamber, and oxygen is continuously introduced through the second inlet.

[0020] S6. The sample gas after high-temperature pyrolysis is discharged from the outlet of the outer tube and flows through the absorption liquid. The volume is adjusted and the absorption liquid is tested.

[0021] S7. The first drive unit retracts the sample boat from the combustion tube into the sample boat chamber via a push rod.

[0022] Beneficial effects

[0023] This invention features a rational structure. The sample boat chamber has an upward-facing inlet, facilitating the placement and removal of the sample boat or the dropping of a sample boat containing solid particles from the inlet to the front end of the push rod. A sealing component is used to open and close the inlet, and the sealing component also has a liquid inlet hole. This allows for sample injection via a liquid injection needle through the liquid inlet hole while the sealing component closes the inlet. It is suitable for reusing the sample boat to inject liquid samples. The rational structural design simplifies the injection operation and prevents liquid samples from splashing outwards during sample boat dispensing, thus improving the accuracy and stability of the detection results. Furthermore, the sample boat chamber in this application is multifunctional, suitable not only for solid particle sample injection but also for liquid sample injection, offering good flexibility and avoiding the need to change the sample boat chamber to adapt to solid particle or liquid sample injection.

[0024] In this application, the sealing assembly can slide axially to open and close the feed inlet, or flip up and down to open and close the feed inlet, offering flexible design suitable for different working conditions. Furthermore, to prevent high-temperature environments from affecting sample properties, a cooling unit is also provided to further improve the accuracy and stability of the test results, especially for highly volatile lightweight liquid samples, where good cooling can reduce volatilization. The cooling unit also includes one or more of the following components arranged sequentially: a Peltier module, heat dissipation fins, and a fan, enabling rapid cooling and preventing high-temperature environments from affecting product properties.

[0025] In this invention, the transfer unit can perform sample boat loading or injection operations under the action of the third drive unit. It has a high degree of automation, which is conducive to improving detection efficiency, avoiding adverse effects caused by non-standard manual operation, and providing convenience for automatically recording the sample boat and the sample in it, making it easy to trace the sample before and after combustion and pyrolysis.

[0026] It also includes a sample tray for holding sample vials, the sample tray including a temperature control unit for heating or cooling the sample vials. Thus, when the sample to be tested is a heavy liquid sample with high density or large molecular weight, appropriate heating can ensure good fluidity and facilitate sample injection. Conversely, when the sample to be tested is a light liquid sample with low density, small molecular weight or high volatility, appropriate cooling can ensure the stability of the sample and reduce volatilization.

[0027] The sample boat and carrier boat in this invention are rationally designed. The concave cavity of the carrier boat is conical, wider at the top and narrower at the bottom. This design guides the sample boat when it is placed within the concave cavity, ensuring it is correctly positioned. This reduces the likelihood of sample boat misalignment after placement, preventing sample accumulation on one side and ensuring complete combustion, thus improving the accuracy of test results. Furthermore, when the sample boat is placed within the concave cavity, it can be fitted with the carrier boat with a clearance fit. This provides good tolerance for the relative positional accuracy of the sample boat and carrier boat. Even if the relative positional accuracy is low during placement, the concave cavity's design (wider at the top and narrower at the bottom) allows for automatic alignment during placement, further improving the positional accuracy of the sample boat after placement. The bottom of the carrier boat includes several through holes. When the airflow from the combustion tube impacts the sample boat assembly upwards, the airflow can diffuse through these holes, buffering and dispersing the airflow and preventing vibration of the carrier boat due to airflow impact. This ingenious structural design...

[0028] Furthermore, the connection between the support boat and the push rod allows for left-right swinging, ensuring smooth and flexible push rod advancement and preventing breakage or jamming due to obstruction. Additionally, the bottom surface of the U-shaped connector abuts against the bottom surface of the channel containing the push rod. This prevents the sample boat assembly and push rod from forming a cantilever structure that could affect their lifespan, and also avoids friction with the support boat causing vibration of the support boat and the sample boat on it. The design is therefore reasonable.

[0029] In this application, the combustion tube is reasonably designed, and the inner tube includes a first tube section and a second tube section that are connected. In this way, when the first tube section is damaged or corroded, it can be replaced to extend the service life of the entire combustion tube, which helps to reduce costs. Furthermore, the first tube section can be made of a high-temperature resistant ceramic material with better chemical stability, which further improves the service life of the combustion tube and reduces costs. Attached Figure Description

[0030] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only one embodiment of the present invention. For those skilled in the art, other embodiments can be derived from the provided drawings without creative effort.

[0031] Figure 1 Schematic diagram of the combustion online ion chromatography system in Example 1;

[0032] Figure 2 Example 1: A three-dimensional structural diagram of the combustion tube, sample boat chamber, and guide tube after assembly;

[0033] Figure 3 : Figure 2A three-dimensional structural diagram of the central sealing cylinder with the feed inlet open;

[0034] Figure 4 : Figure 3 A cross-sectional structural diagram of the main view of the central sealing cylinder with the inlet open;

[0035] Figure 5 Example 1: A three-dimensional structural diagram of the sample boat housed within a support boat at one end of a push rod;

[0036] Figure 6 Example 1: A schematic diagram of the structure of the sample boat housed inside the support boat at one end of the push rod;

[0037] Figure 7 : A three-dimensional exploded view of the sample boat and the support boat in Example 1;

[0038] Figure 8 : A schematic cross-sectional view of the combustion tube in Example 1;

[0039] Figure 9 : A three-dimensional structural diagram of the combustion tube in Example 1;

[0040] Figure 10 Schematic diagram of the combustion online ion chromatography system in Example 2;

[0041] Figure 11 Example 2: A three-dimensional structural diagram of the sample boat chamber, cooling unit, and guide tube after assembly;

[0042] Figure 12 Example 2: A three-dimensional structural diagram of the sample boat chamber and cooling unit after assembly;

[0043] Figure 13 : Figure 12 A three-dimensional structural diagram of the feed inlet on the main body of the sample inlet when the central sealing cover is opened; Detailed Implementation

[0044] The following description and accompanying drawings fully illustrate specific embodiments described herein to enable those skilled in the art to practice them. Some embodiments may include or substitute parts and features of other embodiments. The scope of the embodiments herein encompasses the entire scope of the claims and all available equivalents thereof. Throughout this document, the terms “first,” “second,” etc., are used only to distinguish one element from another without requiring or implying any actual relationship or order between the elements. Indeed, a first element can also be referred to as a second element, and vice versa. Furthermore, the terms “comprising,” “including,” or any other variations thereof are intended to cover non-exclusive inclusion, such that a structure, apparatus, or device that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a structure, apparatus, or device. Without further limitation, an element defined by the phrase “comprising one…” does not exclude the presence of other identical elements in the structure, apparatus, or device that includes said element. The various embodiments described herein are presented in a progressive manner, with each embodiment focusing on its differences from other embodiments; similar or identical parts between embodiments can be referred to interchangeably.

[0045] The terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer" used in this document to indicate orientations or positional relationships are based on the orientations or positional relationships shown in the accompanying drawings. They are used solely for the convenience of describing the document and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. In the description herein, unless otherwise specified and limited, the terms "installed," "connected," and "linked" should be interpreted broadly. For example, they can refer to mechanical or electrical connections, or internal connections between two elements; they can be direct connections or indirect connections through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms according to the specific circumstances.

[0046] In this document, unless otherwise stated, the term "multiple" means two or more.

[0047] In this article, the character " / " indicates that the objects before and after it are in an "or" relationship. For example, A / B means: A or B.

[0048] In this article, the term "and / or" describes an association between objects, indicating that three relationships can exist. For example, A and / or B means: A or B, or A and B.

[0049] Example 1

[0050] like Figures 1-9 The illustrated convenient online combustion ion chromatography system includes a worktable 1, a heating furnace 5, and a first drive unit 6, as shown. Figure 1 As shown, the workbench 1 is equipped with a combustion tube 2, a sample boat chamber 4, and a guide tube 7 connected in sequence.

[0051] A heating furnace 5 is mounted on the workbench 1 for heating the combustion tube 2. The heating furnace 5 is existing technology and can be selected by those skilled in the art according to their needs. In this embodiment, the heating furnace 5 is designed to include a first heating zone, a second heating zone, a third heating zone, and a highest temperature heating zone arranged sequentially along the airflow direction. From the first heating zone to the highest temperature heating zone, the heating power of the combustion furnace on the combustion tube 2 increases progressively to complete the process of sample preheating, heating, coking, and combustion.

[0052] The sample boat 73 can be placed inside the sample boat chamber 4, and the guide tube 7 is equipped with a push rod 71, such as Figures 2-4 As shown, the first drive unit 6 is located on the worktable 1 and can drive the push rod 71 to slide axially along the guide tube 7 to push the sample boat 73 from the sample boat chamber 4 into the combustion tube 2 or to transfer the sample boat 73 from the combustion tube 2 to the sample boat chamber 4.

[0053] In this embodiment, the sample boat chamber 4 includes a sample inlet chamber body 41 and a sealing assembly, such as... Figure 3 and 4 As shown, the sample inlet chamber body 41 includes a through hollow cavity 412, which is connected to the inner cavity of the combustion tube 2 and the inner cavity of the guide tube 7. The hollow cavity 412 opens upward to form a feed inlet 413. Mechanical grippers extend into the feed inlet 413 to complete the loading and unloading of the sample boat 73, or the sample boat 73 is dropped into the front end of the push rod 71 through the feed inlet 413 under its own weight.

[0054] The sealing assembly can open or close the feed port 413, and includes a liquid inlet 421 that communicates with the feed port 413. The liquid inlet 421 is covered with an elastic pad, through which the injection needle can pass to complete the injection. The elastic pad is designed to seal the liquid inlet well and be easily punctured by the injection needle tip, such as a rubber pad.

[0055] In this embodiment, the sealing assembly can slide axially along the sample inlet body 41 to open or close the feed inlet 413. Specifically, the sealing assembly includes a sealing cylinder 42, which is coaxially sleeved outside the sample inlet body 41 and can slide axially along the sample inlet body 41 to open or close the feed inlet 413, such as... Figure 3As shown, it also includes a second drive unit 9, which includes a motor, a lead screw, and a lead screw nut that cooperates with the lead screw. The two ends of the lead screw are rotatably connected to the worktable 1 where the sample injection chamber body 41 is located. The lead screw nut is slidably connected to the worktable. The motor is fixed to the worktable 1 and can transmit rotational motion to the lead screw. The lead screw nut is fixed to the outer wall of the sealing cylinder 42 through the connecting plate 422, so that the sealing cylinder 42 can be driven to slide along the axial direction of the sample injection chamber body 41.

[0056] like Figure 4 As shown, the side wall of the sample inlet chamber body 41 includes two oppositely arranged sample inlet notches 411 to avoid the grippers holding the sample boat 73, which facilitates the automated loading and unloading of the sample boat 73 and provides convenient conditions for tracking and recording the situation of the sample before and after combustion in the sample boat 73.

[0057] In addition, a cooling unit for cooling the sample injection chamber body 41 and the sample boat 73 therein is fixedly provided below the sample injection chamber body 41. In this embodiment, the cooling unit includes a fan 47, so that when the fan 47 is turned on, it can accelerate the airflow in and around the lower part of the sample injection chamber body 41, improve the heat exchange efficiency, and reduce the impact of the high temperature environment of the combustion tube 2 on the sample in the sample injection chamber.

[0058] like Figure 1 As shown, the system also includes a transfer unit 10, a third drive unit 101, and a sample tray 8 for holding sample bottles, all mounted on the worktable 1. The transfer unit 10 is designed to pick up and place sample boats 73 through the inlet 413 under the action of the third drive unit 101. Specifically, the transfer unit 10 includes grippers for holding or releasing the sample boats 73. The third drive unit 101 is existing technology and can drive the grippers to move up and down, left and right, or forward and backward, and control the grippers to hold or release the sample boats 73. Specifically, the third drive unit 101 includes a moving mechanism, a forward and backward moving mechanism, and an up and down moving mechanism. The grippers are connected to the moving ends of the up and down moving roller mechanism, the up and down moving mechanism is connected to the moving ends of the forward and backward moving mechanism, and the forward and backward moving mechanism is connected to the moving ends of the left and right moving mechanism. The left and right moving mechanism is mounted on the worktable 1. The sample tray 8 is mounted on the worktable 1 and includes several cavities for holding the sample boats 73.

[0059] like Figure 5 and 6 As shown, the end of the push rod 71 is also provided with a U-shaped connector 74 and a support boat 72 for supporting the sample boat 73 upward. The first free end of the U-shaped connector 74 passes vertically through the support boat 72 and is hinged to the support boat 72. The second free end of the U-shaped connector 74 is fixedly connected to the push rod 71. In this way, the support boat 72 can swing left and right and is connected to the first end of the push rod 71.

[0060] like Figure 6As shown, the bottom surface of the U-shaped connector 74 is slightly lower than the bottom surface of the support boat 72. During the advancement of the push rod 71, the bottom surface of the U-shaped connector 74 contacts the bottom surface of the channel where the push rod 71 is located. This avoids the sample boat 73 and the support boat 72 forming a cantilever structure with the push rod 71, which would affect their service life. It also prevents friction with the support boat 72 from causing vibration of the support boat 72 and the sample boat 73 on it. The design is reasonable. Furthermore, the cross-section of the U-shaped connector 74 is circular, making the bottom surface of the U-shaped connector 74 an arc surface, which helps improve the smoothness of sliding.

[0061] like Figure 5 and 6 As shown, the second end of the push rod 71 is provided with a magnetic base 75, which can drive the push rod 71 to move under the action of magnetic force. The moving end of the first driving unit 6 includes a slider that interacts with the magnetic base 75. When the slider moves back and forth along the guide tube 7, it drives the push rod 71 to move back and forth.

[0062] like Figure 7 As shown, the support boat 72 is used to support the sample boat 73 upwards, including an upward-opening cavity 723, as... Figure 2 As shown, the concave cavity 723 is larger at the top and smaller at the bottom, and the overall shape of the concave cavity 723 is elongated. The two ends of the concave cavity 723 are spherical, and the inner wall surface connecting the two ends of the concave cavity is an arc surface with the opening extending inward. In this way, when the sample boat 73 is dropped into the concave cavity 723 of the supporting boat 72, the sample boat 73 can be guided, so that the sample boat 73 is placed in the concave cavity 723 in the correct position. This can reduce the probability of the sample boat 73 being misaligned after being dropped. In other embodiments of the present invention, the concave cavity 723 is larger at the top and smaller at the bottom, and the two ends of the concave cavity 723 are conical.

[0063] The sample boat 73 is used to load the sample. When the sample boat 73 is housed in the cavity 723, the side edge of the sample boat 73 is in clearance fit with the side wall of the cavity 723, and the outer edge of the sample boat 73 is adapted to the inner wall of the cavity 723. This design provides good tolerance for the relative positional accuracy of the sample boat 73 and the carrier boat 72. Furthermore, even if the relative positional accuracy of the sample boat 73 and the carrier boat 72 is low during material unloading, the design of the cavity 723 (larger at the top and smaller at the bottom) and its clearance fit with the sample boat 73 allows the grippers to release the sample boat 73, and the sample boat 73 automatically aligns itself during unloading, improving the positional accuracy of the sample boat 73 after unloading.

[0064] like Figure 7 As shown, the bottom surface of the concave cavity 723 is a plane, and the bottom surface of the sample boat 73 that abuts against the bottom surface of the concave cavity 723 is also a plane, thus providing good support stability.

[0065] The sidewall of the support boat 72 forming the cavity 723 includes a notch 721, so that when the sample boat 73 is picked up and put down using the gripper, the gripper can be effectively avoided, making it convenient to pick up and put down the sample boat 73.

[0066] like Figure 7 As shown, the bottom of the support boat 72 includes several through holes 722. In this embodiment, the through holes 722 are arranged in three rows, with the middle row of through holes 722 arranged along the axis of the support boat 72, and the other two rows arranged side by side. When the airflow in the combustion tube 2 impacts the sample boat assembly upwards, the airflow can diffuse through the through holes 722, avoiding vibration of the support boat 72 due to airflow impact. The structural design is ingenious.

[0067] like Figure 7 As shown, the bottom surface of the support boat 72 is curved, which can better disperse and buffer the upward airflow, and facilitate the airflow to continue to diffuse from both sides of the support boat 72, reducing the impact of the airflow on the support boat 72.

[0068] The combustion tube 2 passes through the heating furnace 5 and includes an inner tube 21 and an outer tube 22. For example... Figure 8 As shown, the inner tube 21 forms a through hollow cavity 412 and includes a second tube section 212 and a first tube section 211 arranged axially along the airflow direction. In this embodiment, the first tube section 211 is made of high-temperature resistant ceramic and is integrally formed, while the second tube section 212 is made of quartz material, both of which have good high-temperature resistance.

[0069] like Figure 8 As shown, a relatively closed interlayer cavity is formed between the inner tube 21 and the outer tube 22. The interlayer cavity is connected to the hollow cavity 412 through several through holes 2111 on the first tube section 211. The several through holes 2111 are evenly arranged, and the positions of the several through holes 2111 on the first tube section 211 are designed to correspond to the positions of the sample boat 73 extending into the first tube section 211. This facilitates good gas exchange between the hollow cavity 412 and the interlayer cavity, improving combustion completeness.

[0070] like Figure 8 and 9 As shown, the outlet end of the first pipe section 211, which is away from the second pipe section 212, is inserted into the reduced diameter section 222 at the corresponding position of the outer pipe. The outlet end of the first pipe section 211 is axially abutted against the inner wall of the outer pipe 22 through the high temperature resistant filter cotton 25 to seal the interlayer cavity. In this embodiment, the high temperature resistant filter cotton 25 is made of quartz wool. In addition, those skilled in the art can select according to their needs.

[0071] like Figure 8 As shown, the inlet end of the first pipe section 211 is fitted inside the outlet end of the second pipe section 212 and abuts against the end face formed by the expanded diameter section of the second pipe section 212.

[0072] The end of the second pipe section 212 furthest from the first pipe section 211 is sealed to the outer pipe 22 through surface-to-surface contact, specifically, as follows: Figure 8As shown, the second pipe section 212 is fitted with a bulge 2121. The bulge 2121 is made of quartz and is fixed outside the second pipe section 212. A closed annular cavity is formed between the bulge 2121 and the second pipe section 212. The outer wall surface of the bulge 2121 is formed with a first conical surface 2120. The radial dimension of the first conical surface 2120 gradually decreases along the airflow direction. The inlet end of the outer pipe 22, which corresponds to the position of the bulge 2121, is formed with a second conical surface 221 that matches the first conical surface 2120. The surfaces of the first conical surface 21210 and the second conical surface 221 that come into contact are frosted surfaces. The tiny uneven structures on the two frosted surfaces work together to achieve a good sealing effect and prevent relative sliding between the inner pipe 21 and the outer pipe 22. In this way, the second pipe section 212 and the outer pipe 22 are sealed by the contact of the first conical surface 2120 and the second conical surface 221, thus effectively sealing the interlayer cavity.

[0073] like Figure 9 As shown, it also includes a clamping assembly 26. In this embodiment, the clamping assembly 26 is designed to axially clamp the inner tube 21 and the outer tube 22 to form a relatively sealed interlayer cavity. Specifically, the clamping assembly 26 includes a plurality of first hook teeth 261 and a plurality of second hook teeth 262. The plurality of first hook teeth 261 are circumferentially arranged on the outer wall surface of the outer tube 22, and the plurality of second hook teeth 262 are circumferentially arranged on the outer wall surface of the bulge 2121 extending out of the outer tube 22. The first hook teeth 261 and the second hook teeth 262 are connected by an elastic element, which is existing technology, such as a spring, to axially clamp the inner tube 21 and the outer tube 22, so that the first tube segment 211 is pressed against the high-temperature resistant filter cotton 25, and the first conical surface 2120 and the second conical surface 221 abut against each other and are pressed together.

[0074] like Figure 8 As shown, the outer tube 22 extends axially outward at its outlet end to form an extension section 223. The inner diameter of the extension section 223 is smaller than the inner diameter of the outer tube 22 at the outlet end of the first tube section 211. The outer wall of the outlet end of the extension section 223 bulges outward to form a conical or spherical surface to facilitate sealing connection.

[0075] like Figure 8 and 9 As shown, the second end of the second pipe section 212 extending outside the outer pipe 22 is connected to the first inlet 23, which is used to introduce a mixture of inert gas and ultrapure water, such as argon.

[0076] The interlayer cavity is connected to the second end of the second pipe section 212, and a second inlet 24 is connected to it for introducing oxygen to ensure complete combustion of the sample. The second inlet 24 avoids the bulge 2121, and the pipe connected to the second inlet 24 has an angle that is inclined from bottom to top in the direction of airflow. This can guide the oxygen entering from the second inlet 24 to diffuse axially along the outer pipe 22 and quickly reach the sample boat 73, which is beneficial to improving the completeness of combustion.

[0077] A method of using a combustion online ion chromatography system, employing the combustion online ion chromatography system as described above, characterized by comprising the following steps:

[0078] S1. Equipment preparation: Connect all pipes and fittings, check for gas leaks, initialize the equipment, and raise the temperature of the heating furnace 5 to the working temperature value; connect the absorption pipe containing the absorption liquid to the outlet end of the extension section 223.

[0079] S2. The transfer unit 10 completes the sample injection operation under the action of the third drive unit 101. In this embodiment, the second drive unit drives the sealing cylinder to open the feed port 413 first. Then, under the action of the third drive unit 101, the transfer unit 10 picks up the sample boat 73 containing the sample from the sample tray 8 and places it above the carrier boat 72. During the dropping process, the sample boat 73 automatically aligns and drops into the carrier boat 72 with good positional accuracy. After that, the second drive unit drives the sealing cylinder to slide and close the feed port 413.

[0080] S3. Remove residual gas, open the first inlet, and introduce a mixture of inert gas and ultrapure water into the inner tube; at the same time, another stream of inert gas enters the inner tube through the guide tube 7 and the sample boat chamber 4; simultaneously, open the second inlet and introduce oxygen into the jacketed cavity to remove residual gas in the inner tube and the jacketed cavity.

[0081] S4, the push rod 71, under the action of the first drive unit 6, pushes the sample boat 73 to the set position inside the combustion tube 2, and the heating furnace 5 preheats the sample inside the moving sample boat 73; wherein, a mixture of inert gas and ultrapure water continues to be introduced into the inner tube through the first inlet; at the same time, another stream of inert gas continues to enter the inner tube through the guide tube 7 and the sample boat chamber 4; at the same time, oxygen continues to be introduced into the jacket cavity through the second inlet to remove residual gas in the inner tube and the jacket cavity;

[0082] Along the airflow direction, from the second end of the second pipe section to the outlet end of the outer pipe, there are a first heating zone, a second heating zone, a third heating zone, and a maximum temperature heating zone. From the first heating zone to the maximum temperature heating zone, the heating power of the combustion furnace on the combustion tube 2 increases progressively. The residence time of the sample boat 73 in each heating zone can be set by the user according to their needs. Setting the residence time of the sample in different heating zones is beneficial for the slow, uniform, and complete pyrolysis of the sample, and also prevents the sample from directly entering the maximum temperature zone and causing deflagration.

[0083] S5 and push rod 71 continue to move forward under the action of the first drive unit 6. The sample goes through the preheating, heating, coking and combustion stages. Among them, the heating furnace 5 is designed so that the sample in the sample boat 73 cokes when it is close to the highest temperature zone and then enters the highest temperature zone. The sample boat 73 stays in the highest temperature zone for the longest time. The sample burns in the high temperature zone to form gas and diffuses. At this time, the air intake is adjusted. Inert gas carries ultrapure water into the inner tube through the first inlet. After the ultrapure water is fully vaporized in the inner tube 21, it comes into contact with the sample at the first tube section to form high temperature cracking gas. Another stream of oxygen enters the inner tube through the sample boat chamber 4 and the second inlet continuously introduces oxygen to ensure that the sample is fully combusted.

[0084] S6. The sample gas after high-temperature pyrolysis is discharged from the outlet of the outer tube and flows through the absorption liquid. The volume is adjusted and the absorption liquid is tested.

[0085] S7. The first drive unit 6 retracts the sample boat 73 from the combustion tube 2 into the sample boat chamber 4 via the push rod 71. Specifically, the slider slides axially along the guide tube 7, and the push rod 71 drives the sample boat 73 back into the sample boat chamber 4. Then, the second drive unit drives the sealing cylinder to move, first opening the feed port 413. Then, under the action of the third drive unit 101, the transfer unit 10 picks up the sample boat 73 from the carrier boat 72 and places it in a set position, facilitating the tracking and recording of the sample boat 73 and providing a more accurate reflection of the sample's condition before and after combustion. Throughout steps S1-S7, the cooling unit remains operational.

[0086] This cycle repeats itself.

[0087] Example 2

[0088] The difference between Example 2 and Example 1 is that, as Figures 10-13 As shown, the sealing assembly includes a sealing cap 43. The first end of the sealing cap 43 is hinged to the upper part of the sample inlet chamber body 41, and the second end of the sealing cap 43 is connected to the side of the sample inlet chamber body 41 via a locking member 44 to open or close the feed port 413. The locking member 44 is prior art, and those skilled in the art can select it according to their needs.

[0089] like Figure 11 As shown, the through hole on the sealing cap 43 is sealed to the movable cap 432. The movable cap 432 has an annular transparent window 433 for easy viewing of the sample injection status. The liquid inlet hole 431 is formed on the movable cap 432, which makes it easy to remove the movable cap for replacement of the elastic gasket.

[0090] like Figure 12 As shown, the bottom outer edge of the sample inlet chamber body 41 extends horizontally outward to form a flange, which increases the heat dissipation area and facilitates the installation of the cooling unit.

[0091] like Figure 12As shown, the cooling unit includes a Peltier module 45, heat dissipation fins 46, and a fan 47, which are fixedly arranged sequentially from the bottom of the sample inlet chamber body 41 downwards. The Peltier module 45 is fixedly connected upwards to the flange at the bottom of the sample inlet chamber body 41. The Peltier module 45 is existing technology and can be selected by those skilled in the art according to their needs. It can quickly cool down the sample. The heat dissipation fins 46 include several vertically arranged and parallel heat dissipation plates, which are fixedly connected upwards to the Peltier module 45, increasing the heat dissipation area and improving the heat dissipation effect. The fan 47 is fixedly arranged to accelerate the airflow around the heat dissipation fins 46 and improve the heat exchange efficiency.

[0092] The aforementioned sealing cover can be flipped and connected to the sample inlet body 41 for sample injection in liquid form. Before the injection begins, the sealing cover 43 is flipped to open the inlet 413. The mechanical gripper places the empty sample boat 73 at the front end of the push rod 71. Then, the sealing cover 43 is locked with the locking fastener 44. Then, the sample is injected through the injection needle through the liquid inlet 431. The sample boat 73 can be reused multiple times.

[0093] In this embodiment, the sample vial containing the sample liquid is placed in the sample tray 8. The sample tray 8 includes a temperature control unit, which includes a heating module and a cooling module. The heating module is such as an electric heating wire, and the cooling module is such as a Peltier module. This is existing technology used to heat or cool the sample liquid in the sample vial. Thus, when the sample liquid to be tested is a heavy liquid sample with high density or large molecular weight, appropriate heating can ensure good fluidity and facilitate sample injection. Conversely, when the sample to be tested is a light liquid sample with low density, small molecular weight, or high volatility, appropriate cooling can ensure the stability of the sample and reduce volatilization.

[0094] In this embodiment, the transfer unit 10 includes a sampling needle, which can extract sample liquid from the sample vial and inject it into the sample boat 73 under the action of the third driving unit 101. The third driving unit 101 is existing technology and can drive the sampling needle to move up and down, left and right, or forward and backward.

[0095] Thus, under the action of the third drive unit 101, the injection needle can inject the sample into the sample boat 73 through the liquid inlet 431 and the feed inlet.

[0096] The present invention has been described above by way of example, but the present invention is not limited to the specific embodiments described above. Any modifications or variations made based on the present invention shall fall within the scope of protection claimed by the present invention.

Claims

1. A user-friendly online combustion ion chromatography system, characterized in that, The system includes a workbench (1), a heating furnace (5), and a first drive unit (6). The workbench (1) is provided with a combustion tube (2), a sample boat chamber (4), and a guide tube (7) connected in sequence. The heating furnace (5) is located on the workbench (1) to heat the combustion tube (2). The sample boat can be placed inside the sample boat chamber (4). A push rod (71) is provided inside the guide tube (7). The first drive unit (6) is located on the workbench (1) and can drive the push rod (71) to slide axially along the guide tube (7) to push the sample boat out of the sample boat chamber (4). The sample boat is fed into the combustion tube (2) or transferred from the combustion tube (2) to the sample boat chamber (4). The sample boat chamber (4) includes a sample inlet body (41) and a sealing assembly. The sample inlet body (41) includes a through hollow cavity (412) to communicate with the inner cavity of the combustion tube (2) and the inner cavity of the guide tube (7). The hollow cavity (412) opens upward to form a feed inlet (413). The sealing assembly can open or close the feed inlet (413). The sealing assembly includes a liquid inlet hole (421, 431) that can communicate with the feed inlet (413). The push rod (71) is also provided with a support boat (72) for supporting the sample boat (73) upward. The support boat (72) is connected to the end of the push rod (71) and can swing left and right. The support boat (72) includes an upward-opening cavity (723) and the cavity (723) is larger at the top and smaller at the bottom. The sidewall of the support boat (72) forming the cavity (723) includes a notch (721) to facilitate the placement and removal of the sample boat (73); and the bottom of the support boat (72) includes several through holes (722). The push rod (71) includes a U-shaped connector (74) at its end. One free end of the U-shaped connector (74) passes vertically through the support boat (72) and is hinged to the support boat (72). The bottom surface of the U-shaped connector (74) is not higher than the bottom surface of the support boat (72) to avoid the support boat from forming a cantilever structure. The combustion tube (2) passes through the heating furnace (5) and includes an inner tube (21) and an outer tube (22). The inner tube (21) includes a second tube section (212) and a first tube section (211) arranged axially along the airflow direction. A relatively closed interlayer cavity is formed between the inner tube (21) and the outer tube (22). The interlayer cavity is connected to the inner cavity of the inner tube (21) through several through holes (2111) on the first tube section (211). The second end of the second tube section (212) extending outside the outer tube (22) is connected to a first inlet (23). The interlayer cavity is connected to a second inlet (24) near the second end of the second tube section (212).

2. The convenient-to-operate online combustion ion chromatography system according to claim 1, characterized in that, The sealing assembly can slide axially along the injection chamber body (41) to open or close the inlet (413); or the first end of the sealing assembly is hinged to the injection chamber body (41), and the second end of the sealing assembly is connected to the injection chamber body (41) via a locking member (44) to open or close the inlet (413).

3. The convenient-to-operate online combustion ion chromatography system according to claim 1, characterized in that, A cooling unit for cooling the sample inlet body and the sample boat therein is fixed below the sample inlet body (41). The cooling unit includes one or more of a fan (47), heat dissipation fins (46), or Peltier module (45).

4. The convenient-to-operate online combustion ion chromatography system according to any one of claims 1 to 3, characterized in that, It also includes a transfer unit (10) and a third drive unit (101). The transfer unit (10) can inject samples into the sample boat through the liquid inlet (421, 431) and / or the feed inlet (413) under the action of the third drive unit (101), or take the sample boat out and put it in through the feed inlet (413).

5. The convenient-to-operate online combustion ion chromatography system according to claim 4, characterized in that, It also includes a sample tray (8) for holding sample vials, the sample tray (8) including a temperature control unit for heating or cooling the sample vials, and the transfer unit (10) can extract sample liquid from the sample vials and inject it into the sample boat under the action of the third drive unit (101).

6. A method of using a combustion online ion chromatography system, employing the combustion online ion chromatography system as described in claim 5, characterized in that, Including the following steps: S1. Equipment preparation; S2. The transfer unit (10) completes the sample injection operation under the action of the third drive unit (101); S3. Remove residual gas, open the first inlet, and introduce a mixture of inert gas and ultrapure water into the inner tube (21). After a set time, close the first inlet (23). At the same time, another stream of inert gas enters the inner tube (21) through the guide tube (7) and the sample boat chamber (4). After a set time, close the guide tube (7). At the same time, open the second inlet (24) and introduce oxygen into the interlayer cavity to remove residual gas in the inner tube and the interlayer cavity. S4. The push rod (71) pushes the sample boat (73) to the set position inside the combustion tube (2) under the action of the first drive unit (6), and the heating furnace (5) preheats the sample inside the moving sample boat (73); S5. The push rod (71) continues to move forward under the action of the first drive unit (6). The sample goes through the preheating, heating, coking and combustion stages. At the same time, the inert gas carries ultrapure water into the inner tube (21) through the first inlet (25), another stream of oxygen enters the inner tube (21) through the sample boat chamber (4), and oxygen is continuously introduced through the second inlet. S6. The sample gas after high-temperature pyrolysis is discharged from the outlet of the outer tube and flows through the absorption liquid. The volume is adjusted and the absorption liquid is tested. S7. The first drive unit (6) uses a push rod (71) to retract the sample boat (73) from the combustion tube (2) into the sample boat chamber (4).

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