Analysis device
The analytical device employs a locking mechanism and sliding mechanism to prevent unintentional separation column removal, enhancing operational safety and efficiency by maintaining secure column connections.
Patent Information
- Application Number
- JP2025146593
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2021-04-23
- Filing Date
- 2025-09-04
- Publication Date
- 2025-11-18
AI Technical Summary
Existing analytical devices with multiple separation columns risk unintentional removal during operation, leading to sample leakage from the analysis flow path.
The analytical device incorporates a locking mechanism that restricts the removal of separation columns other than the one intended for replacement, along with a sliding mechanism to connect and disconnect columns from the analysis flow paths, and a control device to manage these mechanisms, ensuring secure column attachment and detachment.
Prevents unintentional removal of separation columns, maintaining the integrity of the analysis flow path and ensuring safe and efficient operation of the analytical device.
Smart Images

Figure 2025170424000001_ABST
Abstract
Description
[Technical Field]
[0001] The present disclosure relates to an analytical device. [Background technology]
[0002] Analytical instruments such as liquid chromatographs use a separation column packed with a packing material called a stationary phase to isolate analytes from contaminants or to separate multiple analytes from one another. In a separation, the sample is injected into a liquid flow called the mobile phase in the analytical instrument and moves through the stationary phase (packing material) in the separation column. As the sample moves through the stationary phase, the analytes are separated due to differences in the strength of interaction between the substances in the sample and the stationary phase.
[0003] The analytical device includes, for example, a liquid delivery pump that delivers the mobile phase, a degassing unit that removes dissolved air from the mobile phase, a sample injection unit that injects the sample into the mobile phase, a separation column where separation takes place, a column oven that controls the temperature of the separation column, and a detector that detects components in the column eluate. The detector may be a photometer, a mass spectrometer, or the like, and may be selected appropriately depending on the purpose of analysis, the sample, etc. The analytical device further includes, for example, a control device that analyzes the results detected by the detection unit.
[0004] To improve throughput, analytical instruments are sometimes equipped with multiple separation columns. In this case, by switching between the separation columns to be used using valves, analysis can be performed on the remaining separation columns while some of the separation columns are being washed and equilibrated. This allows for continuous analysis.
[0005] Patent Document 1 describes a separation column connecting device comprising: a column holder for holding a separation column; a first fitting holder mounting a first fitting having a seal part that connects to the upstream seal part of the separation column and to which an upstream piping is connected; a second fitting holder mounting a second fitting having a seal part that connects to the downstream seal part of the separation column and to which a downstream piping is connected; a main body member to which either the first fitting holder or the second fitting holder is fixed; a drive part that moves the first fitting holder or the second fitting holder that is not fixed to the main body member and the column holder relative to the main body member; a guide that guides the column holder in the direction of movement by the drive part; and an elastic body provided between the column holder and the second fitting holder. [Prior art documents] [Patent documents]
[0006] [Patent Document 1] Patent No. 6611398 (Claim 1) Summary of the Invention [Problem to be solved by the invention]
[0007] In the technology described in Patent Document 1, during operation, among the multiple separation columns (Fig. 25), the remaining separation columns may be unintentionally removed by the user, which may cause the sample to leak from the analysis flow path. The problem to be solved by the present disclosure is to provide an analytical device that can prevent unintentional removal of a separation column. [Means for solving the problem]
[0008] The analytical device of the present disclosure includes a plurality of removable separation columns connected in parallel, a plurality of analysis flow paths connected to each of the plurality of separation columns and allowing a sample to flow through each of the plurality of separation columns, a locking mechanism that restricts removal of the separation columns other than the separation column to be removed, a sliding mechanism that connects the separation columns to the analysis flow paths by sliding one of the separation columns or the analysis flow paths relative to the other structure that is placed on the separation column, and a control device that controls the locking mechanism, wherein releasing the locking mechanism releases the connection between the separation columns and the analysis flow paths and the locking mechanism restricts sliding of the other structure. Other solutions will be described later in the description of the invention. [Effects of the Invention]
[0009] According to the present disclosure, an analyzer capable of suppressing unintentional removal of a separation column can be provided. [Brief explanation of the drawings]
[0010] [Figure 1] FIG. 1 is a system diagram of a liquid chromatograph according to a first embodiment. [Figure 2] FIG. 10 is a diagram illustrating the state when the separation column is removed, with the analysis channel and the separation column still connected. [Figure 3] FIG. 2 is a block diagram of a slide mechanism. [Figure 4] FIG. 1 is a diagram illustrating a medium for identifying a separation column. [Figure 5] FIG. 10 is a diagram illustrating the removal of the separation column, showing the state in which the analysis channel is slid by releasing the locking mechanism. [Figure 6] FIG. 10 is a diagram illustrating the removal of the separation column, showing the state in which the analysis channel is locked while the lock is released. [Figure 7] 1 is a flowchart illustrating a method for removing a separation column. [Figure 8] 10A and 10B are diagrams illustrating light emission patterns of the LED switch. [Figure 9] FIG. 10 is a diagram illustrating the light emission pattern of the LED switch for each step when removing the separation column. [Figure 10] 1 is a flowchart illustrating a method for attaching a separation column. [Figure 11] FIG. 10 is a diagram illustrating the light emission pattern of the LED switch for each step when attaching the separation column. [Figure 12] FIG. 10 is a system diagram of a liquid chromatograph according to a second embodiment. [Figure 13] FIG. 10 is a diagram illustrating the state when the separation column is removed in the liquid chromatograph of the third embodiment, with the analysis flow path and the separation column still connected. [Figure 14] FIG. 10 is a diagram illustrating the removal of a separation column in the liquid chromatograph of the third embodiment, showing the state in which the analysis flow path is slid by pulling up the lever. [Figure 15] FIG. 10 is a diagram illustrating the state when a separation column is removed from the liquid chromatograph of the third embodiment, with the analysis flow path locked in a disconnected state. [Figure 16] 10 is a flowchart illustrating a method for removing a separation column in a liquid chromatograph according to a third embodiment. [Figure 17] 10 is a flowchart illustrating a method for attaching a separation column to a liquid chromatograph according to a third embodiment. [Figure 18] FIG. 10 is a diagram illustrating the state when the separation column is removed from the liquid chromatograph of the fourth embodiment, with the analysis flow path and the separation column still connected. [Figure 19] FIG. 10 is a diagram illustrating the removal of a separation column in the liquid chromatograph of the fourth embodiment in an unlocked state, with the analysis channel being slid. [Figure 20] FIG. 10 is a diagram illustrating the state when a separation column is removed from the liquid chromatograph of the fourth embodiment, with the analysis flow path locked in a disconnected state. DETAILED DESCRIPTION OF THE INVENTION
[0011] Hereinafter, modes for carrying out the present disclosure (hereinafter referred to as "embodiments") will be described with reference to the drawings. In the following description of one embodiment, other embodiments applicable to the one embodiment will also be described as appropriate. The present disclosure is not limited to the one embodiment below, and different embodiments can be combined with each other or modified as desired without significantly impairing the effects of the present disclosure. Furthermore, the same components will be given the same reference numerals, and redundant descriptions will be omitted. Furthermore, components having the same functions will be given the same names. The contents shown are merely schematic, and for convenience of illustration, changes may be made from the actual configuration within the scope of not significantly impairing the effects of the present disclosure, and some components may be omitted or modified between drawings.
[0012] 1 is a system diagram of a liquid chromatograph 100 according to the first embodiment. In the following example, a liquid chromatograph is used as an analytical device, but the analytical device may also be a gas chromatograph, an ultra-high performance liquid chromatograph, a clinical testing device equipped with a separation column, or the like.
[0013] Liquid chromatograph 100 includes multiple separation units 103, 104, and 105 connected in parallel, and separation units 103, 104, and 105 are defined as streams 1, 2, and 3, respectively. Separation units 103, 104, and 105 are connected to one mass spectrometer (detector) 119 by a flow path switching valve (flow path switching unit) 118. Note that the detector is not limited to mass spectrometer 119, and may be, for example, a visible / ultraviolet light absorbance detector, a photodiode array detector, a fluorescence detector, or the like.
[0014] Separation units 103, 104, and 105 are equipped with removable separation columns 115, 116, and 117, respectively. Thus, liquid chromatograph 100 is equipped with a plurality of removable separation columns 115, 116, and 117 connected in parallel. Liquid chromatograph 100 is equipped with a plurality of analysis flow paths 120, 121, 122, 123, 124, and 125. Analysis flow paths 120, 121, 122, 123, 124, and 125 are connected to the plurality of separation columns 115, 116, and 117, respectively, and allow the sample to flow through each of the plurality of separation columns 115, 116, and 117.
[0015] The separation unit 103 includes a liquid delivery pump 106 (liquid delivery unit), a sample injection valve 109 (sample injection unit), a connection unit 112, analysis flow paths 120 and 123, and an LED switch 201. The liquid delivery pump 106 delivers a plurality of different solvents while changing their concentrations. The sample injection valve 109 introduces the sample into the analysis flow path 120. A separation column 115 is installed in the connection unit 112. The analysis flow paths 120 and 123 are connected to the separation column 115 and allow the sample to flow through the separation column 115.
[0016] The separation unit 104 includes a liquid delivery pump 107 (liquid delivery unit), a sample injection valve 110 (sample injection unit), a connection unit 113, analysis flow paths 121 and 124, and an LED switch 202. The liquid delivery pump 107 delivers a plurality of different solvents while changing their concentrations. The sample injection valve 110 introduces the sample into the analysis flow path 121. A separation column 116 is installed in the connection unit 113. The analysis flow paths 121 and 124 are connected to the separation column 116 and allow the sample to flow through the separation column 116.
[0017] Separation unit 105 includes a liquid delivery pump 108 (liquid delivery unit), a sample injection valve 111 (sample injection unit), a connection unit 114, analysis flow paths 122 and 125, and an LED switch 203. Liquid delivery pump 108 delivers a plurality of different solvents while changing their concentrations. Sample injection valve 111 introduces the sample into analysis flow path 122. A separation column 117 is installed in connection unit 114. Analysis flow paths 122 and 125 are connected to separation column 117, and allow the sample to flow through separation column 117.
[0018] The LED switches 201, 202, and 203 (an example of an alarm device) are provided in the liquid chromatograph 100 and indicate which of the separation columns 115, 116, and 117 can be removed. By providing the LED switches 201, 202, and 203, the user can easily identify which separation columns 115, 116, and 117 should be removed.
[0019] The LED switches 201, 202, and 203 have LED lamp and switch functions, and in addition to providing notification of the removable separation columns 115, 116, and 117, their light emission state changes depending on the state of the connection parts 112, 113, and 114. The LED switches 201, 202, and 203 provide notification by, for example, lighting up, blinking, changing color, etc. The LED switches 201, 202, and 203 are connected to the control device 101 by electric signal lines (not shown), and are arranged near the separation columns 115, 116, and 117.
[0020] The notification devices are not limited to the LED switches 201, 202, and 203, and may be light sources other than LED lamps, speakers that emit sounds, or the like.
[0021] The liquid chromatograph 100 includes a control device 101, which controls the operations of the separation units 103, 104, and 105, the flow path switching valve 118, and the mass spectrometer 119. Furthermore, the control device 101 controls a lock mechanism 200 (FIG. 3), which will be described in detail later. The control device 101 may include, for example, a CPU (Central Processing Unit), RA (Reconfigurable Array), or the like, although these are not shown. The control device 101 is configured to include RAM (Random Access Memory), ROM (Read Only Memory), etc. A predetermined control program stored in the ROM is loaded into RAM and executed by the CPU, thereby realizing the control device 101.
[0022] The liquid chromatograph 100 includes a display device 102 (an example of an alarm device) connected to the control device 101, and the display device 102 displays various information such as analysis results and information related to the progress of the analysis. The display device 102, together with the LED switches 201, 202, and 203, also indicates which of the multiple separation columns 115, 116, and 117 are removable.
[0023] The liquid chromatograph 100 is equipped with an input device 1021 that is connected to the control device 101 and that, when operated with the separation columns 115, 116, and 117 placed thereon, releases the slide restriction imposed by the locking mechanism 200 (FIG. 3). The provision of the input device 1021 allows the user to release the slide restriction by operating the input device 1021, as will be described in detail later, thereby enabling the separation columns 115, 116, and 117 to be connected to the analysis flow paths 123, 124, and 125.
[0024] 2 is a diagram illustrating the removal of separation column 115, showing the state in which analysis channels 120, 123 and separation column 115 are connected. While FIG. 2 illustrates connection part 112, connection parts 113, 114 have the same structure except that separation columns 116, 117 are provided instead of separation column 115. Separation columns 116, 117 can also be removed and attached in the same manner as in FIGS. 2, 5, and 6, and therefore a description of the removal and attachment of separation columns 116, 117 will be omitted. Furthermore, although analysis channel 123 is slid by slide mechanism 700 in this specification, a slide mechanism (not shown) for sliding separation column 115 may also be provided.
[0025] The sample moves inside the analytical channels 120 and 123 in the direction of arrow 300, enters the separation column 115 through the analytical channel 120, and exits the separation column 115 through the analytical channel 123. Therefore, the analytical channels 120 and 123 are connected to one end (inlet) and the other end (outlet) of the separation column 115, respectively.
[0026] The liquid chromatograph 100 includes, at the connection portion 112, a stage 301, a heat block 302, a column heat block 303, a column cartridge 304, fitting holders 305 and 307, a compression spring 306, a heating device 309, a temperature sensor 310, a slide mechanism 700, an open detection sensor 312, a connection detection sensor 313, a reading device 314, and a support base 318.
[0027] The column heat block 303 is placed in an opening (not shown) formed in the column cartridge 304 and comes into contact with the heat block 302. That is, the heat block 302 comes into contact with the separation column 115 via the column heat block 303 placed in an opening (not shown) formed in the column cartridge 304. The heating device 309 heats the separation column 115. The temperature sensor 310 measures the temperature of the separation column 115. The temperature sensor 310 measures the temperature of the heat block 302, but may measure the temperature of any of the heat block 302, the column heat block 303, or the separation column 115.
[0028] 3 is a block diagram of the slide mechanism 700. The slide mechanism 700 connects the separation column 115 and the analysis channel 123 by sliding the analysis channel 123 (the other structure) relative to the placed separation column 115 (one of the structures), which is either the separation column 115 or the analysis channel 123. By providing the slide mechanism 700, the separation column 115 or the analysis channel 123 can be connected by sliding at least one of them. In the illustrated example, the slide mechanism 700 slides the analysis channel 123.
[0029] The slide mechanism 700 includes a motor 701, a crank arm 315, and a linear guide 308. The motor 701 is connected to the analysis channel 123 via the bendable crank arm 315, and the crank arm 315 converts the rotational driving force of the motor 701 into a propulsive force in the direction of the analysis channel 123 toward the separation column 115. The provision of the motor 701 allows the analysis channel 123 to be slid using the motor 701, thereby reducing the burden on the user.
[0030] The rotation speed, torque, rotation timing, etc. of the motor 701 are controlled by the control device 101. If it is desired to make the motor 701 smaller (to save power), a reduction mechanism (not shown) can be installed between the motor 701 and the crank arm 315, allowing a small motor 701 to obtain a large force.
[0031] The motor 701 includes a motor body 702 that rotates a rotary drive shaft (not shown), and a shaft fixing mechanism 703 that fixes the rotary drive shaft when the motor body 702 is not energized, as part of the locking mechanism 200. Although the rotary drive shaft can rotate even when the motor body 702 is not energized, the provision of the shaft fixing mechanism 703 allows the rotary drive shaft to be fixed when the motor body 702 is not energized, thereby limiting sliding of the analysis channel 123. In the first embodiment, the shaft fixing mechanism 703 fixes the rotary drive shaft of the motor body 702, which is connected to the separation columns 116 and 117. This maintains the connection between the separation columns 116 and 117 and the analysis channel 123, and prevents the separation columns 116 and 117 from being unintentionally removed.
[0032] The locking mechanism 200 restricts the removal of the separation columns 116, 117 (FIG. 1) other than the separation column 115 to be removed. During the replacement work of the separation column 115, the locking mechanism 200 allows the separation column 115 to be removed, while locking the separation columns 116, 117 other than the separation column 115 to be removed. This makes it possible to prevent the separation columns 116, 117 from being unintentionally removed.
[0033] The locking mechanism 200 restricts the sliding of the analysis channel 123 by the slide mechanism 700. This prevents the separation column 115 from being disconnected from the analysis channel 123 when locked by the locking mechanism 200, and prevents the separation column 115 from being unintentionally removed.
[0034] 4 is a diagram illustrating a medium 601 for identifying a separation column 115. The liquid chromatograph 100 includes a reader 314 (FIG. 2) that reads information recorded on the medium 601, which includes information for identifying the installed separation column 115. By including the reader 314, the separation column 115 can be identified, thereby preventing installation errors and the like. Although not shown, the separation columns 116 and 117 also include a medium (not shown).
[0035] In the illustrated example, the medium 601 is attached to the side surface of the column cartridge 304 that houses the separation column 115, but it may also be attached directly to the separation column 115. The medium 601 may be, for example, a one-dimensional code, a two-dimensional code, a symbol, an RFID tag, or the like, and the separation column 115 may be identified based on, for example, a unique number recorded on the medium 601 and a database (not shown) that indicates the relationship between numbers and identification information stored in the control device 101 (FIG. 1).
[0036] In the illustrated example, the medium 601 is an RFID tag that serves as an identifier. The medium 601 is read while the separation column 115 is placed thereon. When replacing the separation column 115, the reader 314 reads information such as the type of separation column 115 to which the medium 601 is attached, its serial number, and which of the connection parts 112, 113, and 114 (FIG. 1) the medium is attached to. The control device 101 counts the number of times the separation column 115 has been used and notifies the user via the display device 102 when it is time to replace the separation column 115. When replacing the separation column 115, a record of use is written on the medium 601 attached to the separation column 115 to be replaced, thereby preventing reuse.
[0037] The open detection sensor 312 (second sensor) detects disconnection of the analysis flow path 123 from the downstream side, which is the other end of the separation column 115. The connection detection sensor 313 (first sensor) detects connection of the analysis flow path 120 to the upstream side, which is one end of the separation column 115. The specific configurations of both the open detection sensor 312 and the connection detection sensor 313 are arbitrary, but for example, an optical sensor that can detect a structure by shading or reflection of light irradiated from below to above can be used.
[0038] The open detection sensor 312 detects the fitting holder 307 that is integral with the analysis channel 123. In the example shown, the open detection sensor 312 does not detect the fitting holder 307 because the fitting holder 307 is not located above the open detection sensor 312. On the other hand, as will be described in detail later with reference to FIG. 6, the open detection sensor 312 detects the fitting holder 307 when the fitting holder 307 is positioned at the farthest position from the separation column 115. This detection detects that the separation column 115 and the analysis channel 123 have been disconnected.
[0039] The connection detection sensor 313 detects the shaft 317 that protrudes laterally from the support base 318 due to the movement of the separation column 115 to the left in the drawing. In the illustrated example, the separation column 115 and the analysis channel 123 are arranged coaxially. Therefore, the shaft 317 arranged on the side of the separation column 115 pushes the compression spring 306 and protrudes laterally from the support base 318. As a result, the connection detection sensor 313 detects the shaft 317, and the connection between the separation column 115 and the analysis channel 123 is detected.
[0040] The control device 101 (FIG. 1) restricts the movement using the locking mechanism 200 when either the open detection sensor 312 or the connection detection sensor 313 detects. In this way, sliding is restricted in both the disconnected and connected states. This makes it easier to remove the separation column 115 in the disconnected state, and prevents unintentional removal of the separation column 115 in the connected state. In the illustrated example, the open detection sensor 312 is not detecting and the connection detection sensor 313 is detecting, so the separation column 115 is locked by the locking mechanism 200.
[0041] 5 is a diagram illustrating the removal of the separation column 115, showing the state in which the analysis channel 123 is slid by releasing the locking mechanism 200. In this state, the fitting holder 307 is not present above the open detection sensor 312, and the open detection sensor 312 is not detecting. Meanwhile, the restoring force of the compression spring 306 prevents the shaft 317 from protruding to the left of the support base 318, and the connection detection sensor 313 is not detecting. Therefore, since neither the connection detection sensor 313 nor the open detection sensor 312 is detecting, no restriction is imposed by the locking mechanism 200. When the locking mechanism 200 is released, the rotary drive shaft of the motor main body 702 (FIG. 3) becomes rotatable.
[0042] With the locking mechanism 200 (FIG. 3) released, energizing the motor main body 702 (FIG. 3) releases the connection between the separation column 115 and the analysis channel 123. This separates the separation column 115 from the analysis channel 123, and as will be described in detail later with reference to FIG. 7, the separation column 115 can be removed from the liquid chromatograph 100. In the illustrated example, energizing the motor main body 702 (FIG. 3) causes the analysis channel 123 to slide away from the separation column 115. This releases the connection between the separation column 115 and the analysis channel 123.
[0043] FIG. 6 illustrates the removal of the separation column 115, showing the analysis channel 123 locked in the unlocked state. When the analysis channel 123 is slid away from the separation column 115, the linear guide 308 eventually reaches the farthest position to which it can slide. At this time, the sliding by the slide mechanism 700 stops. The open detection sensor 312 detects the linear guide 308 and detects a disconnection. Meanwhile, the connection detection sensor 313 is not detecting a connection, as in the case shown in FIG. 5 above. Therefore, because the open detection sensor 312 is detecting a connection, the lock mechanism 200 restricts sliding. As a result, the analysis channel 123 is locked at the farthest position from the separation column 115, allowing the separation column 115 to be removed without being affected by the analysis channel 123.
[0044] In this manner, the locking mechanism 200 (FIG. 3) further restricts the sliding of the analysis channel 123 when the separation column 115 is disconnected from the analysis channel 123, as shown in FIG. 6. Because the sliding of the analysis channel 123 is restricted when the separation column 115 is disconnected from the analysis channel 123, the separation column 115 can be easily removed.
[0045] When installing the separation column 115, the process is reversed. That is, in the state shown in Figure 6, the user replaces the separation column 115 and presses one end of the new separation column 115 against the analysis channel 120. Next, the slide mechanism 700 slides the analysis channel 123 in the direction approaching the separation column 115, in the order shown in Figures 6, 5, and 2. This allows the separation column 115 and the analysis channel 123 to be connected.
[0046] 7 is a flowchart illustrating a method for removing the separation column 115 (a method for controlling the analyzer). The separation columns 116 and 117 (FIG. 1) can also be removed in the same manner as in FIG. 7. The description of FIG. 7 will be made with reference to FIG. 1 as appropriate. The method for removing the separation column 115 includes steps S1 to S12.
[0047] The control device 101 displays on the display device 102 a message indicating that the separation column 115 should be replaced due to the valid number of uses of the separation column 115, the expiration date being exceeded, etc. (Step S1). Alternatively, the user may instruct the control device 101 to replace the separation column 115 by using the input device 1021 (Step S1). The control device 101 notifies the user of the separation column 115 to be removed via at least one of the LED switch 201 indicating the connection part 112 and the display device 102 (Step S2).
[0048] Next, the control device 101 releases the restriction on removal imposed by the locking mechanism 200 (FIG. 3) when it detects the end of analysis in the separation column 115. In this way, the separation column 115 becomes removable upon completion of analysis, and therefore, the detection of the end of analysis allows the timing of removal of the separation column 115 to be known.
[0049] Specifically, the control device 101 releases the restriction on removal imposed by the locking mechanism 200 (FIG. 3) when at least one of the temperature of the separation column 115 and the internal pressure of at least one of the analysis channel 120 and the separation column 115 is equal to or lower than a predetermined value (step S3). The temperature can be, for example, a value measured by the temperature sensor 310 (FIG. 2).
[0050] When the temperature of the separation column 115 falls below a predetermined value, the control device 101 releases the restriction on removal imposed by the locking mechanism 200 (FIG. 3) (first half of step S3). This allows the completion of analysis to be determined based on the temperature of the separation column 115 when the temperature of the separation column 115, which was raised by the heating device 309 (FIG. 3) during operation, drops due to heating being stopped at the end of analysis. This allows removal to be performed at an appropriate time. Furthermore, by releasing the restriction when the temperature falls below a predetermined value, such as a temperature that is easy for an operator to touch, removal by an operator can be easily performed.
[0051] Furthermore, for example, the control device 101 releases the restriction on removal imposed by the locking mechanism 200 when the internal pressure of at least one of the analytical flow path 120 or the separation column 115 falls below a predetermined value (the latter half of step S3). This allows the end of analysis to be determined based on the pressure when the internal pressure of at least one of the analytical flow path 120 or the separation column 115, which is high during operation, drops due to the end of analysis, and removal can be performed at an appropriate time. For example, by releasing the restriction when the internal pressure falls below a predetermined value indicating a state close to atmospheric pressure, unintended sample leakage from at least one of the analytical flow path 120 or the separation column 115 can be sufficiently suppressed. The internal pressure of at least one of the analytical flow path 120 or the separation column 115 can be measured as the pressure of the liquid delivery pump 106, for example, as shown in the figure.
[0052] If the result of step S3 is "abnormal" because the result exceeds the predetermined value, the replacement work of the separation column 115 is stopped, and the control device 101 issues a system alarm using at least one of the LED switch 201 and the display device 102 (step S4). On the other hand, if the result of step S3 is "normal" because the result is equal to or less than the predetermined value, the control device 101 issues a notification to the user using at least one of the LED switch 201 and the display device 102 (step S5). This allows the user to know which separation column 115 needs to be replaced.
[0053] The user presses the LED switch 201 or a button on the display device 102 (step S6). This causes the control device 101 to release the shaft fixing mechanism 703 (FIG. 3), which is the locking mechanism 200 (FIG. 3) (step S7). The control device 101 then sends an electrical signal to the motor main body 702 (FIG. 3) to energize it and disconnect the separation column 115 from the analysis channel 123 (step S8). After disconnection, the control device 101 determines whether the open state is correct (step S9). Specifically, as shown in FIG. 6, the control device 101 determines that the open state is correct when the open detection sensor 312 detects that the analysis channel 123 is not connected. If the open state is incorrect (No), the replacement of the separation column 115 is stopped (step S10), as in step S4 above.
[0054] On the other hand, if the open state is correct (Yes), the control device 101 drives the shaft fixing mechanism 703, which is the locking mechanism 200 (FIG. 3) (step S11, locking step). This fixes the rotation drive shaft of the motor main body 702 (FIG. 3), restricting sliding. Step S11 is a step in which the locking mechanism 200 restricts removal of the separation columns 116, 117 other than the separation column 115 that is the target of removal, among the multiple separation columns 115, 116, 117 that are connected in parallel and are removable. Then, the disconnection is completed, and the user can remove the separation column 115 (step S12).
[0055] FIG. 8 is a diagram illustrating the light emission patterns of the LED switch 201. In steps S1 to S12 (FIG. 7), one of the light emission patterns A to E shown in FIG. 8 is appropriately selected and emitted. Light emission pattern A is extinguishment. Light emission pattern A is used while the connected separation column 115 is in use. Light emission pattern B is, for example, a flashing green light (the color of the LED switch 201 is not limited to green; the same applies below). Light emission pattern B is used when waiting for the user to press the LED switch 201 when replacing the separation column 115.
[0056] Light emission pattern C is, for example, a double green flash (the light goes out after flashing twice in a row). Light emission pattern C is used by the user during the replacement work when removing and installing the separation column 115 (described below). Light emission pattern D is, for example, a fast green flash. Light emission pattern D is used when a system alarm is issued. Light emission pattern E is a steady green light. Light emission pattern E is used when the liquid chromatograph 100 (Figure 1) is operating during the replacement work of the separation column 115.
[0057] 9 is a diagram illustrating the light emission patterns of the LED switch 201 for each of steps S1 to S12 when removing the separation column 115. Light emission pattern A is used in steps S1 and S12. Light emission pattern B is used in step S5. Light emission pattern C is used in step S11, and light emission pattern D is used in steps S4 and S10. Light emission pattern E is used in steps S2, S7, and S8.
[0058] In step S3, the light emission pattern E in step S2 continues to be used. In step S6, the light emission pattern B in step S5 continues to be used. In step S9, the light emission pattern E in step S8 continues to be used.
[0059] Figure 10 is a flowchart illustrating a method for installing the separation column 115. The separation columns 116 and 117 (Figure 1) can also be installed in the same manner as in Figure 10. Figure 10 will be described with reference to Figure 1 as appropriate. The method for installing the separation column 115 includes steps S21 to S32.
[0060] The control device 101 notifies the user of the separation column 115 to be replaced by at least one of the corresponding LED switch 201 and the display device 102 (step S21). At this point, the separation column 115 is not yet attached to the connection part 112. The shaft fixing mechanism 703 (FIG. 3) restricts the sliding by the slide mechanism 700 (FIG. 2). The user installs the separation column 115 on the connection part 112 to be replaced (step S22). After installation is complete, the user presses at least one of the LED switch 201 and a button (not shown) on the display device 102 (step S23). This causes the control device 101 to release the fixation by the shaft fixing mechanism 703 (FIG. 3) (step S24). At the same time, the control device 101 transmits an electrical signal to the motor main body 702 (FIG. 3) to energize the motor, thereby starting the sliding of the separation column 115 down the analysis channel 123 (step S25).
[0061] The control device 101 determines whether the connection state is correct (step S26). Specifically, the control device 101 determines that the connection state is correct when the connection detection sensor 313 (FIG. 2) detects the connection of the analysis flow path 123. If the connection state is incorrect (No), the replacement work of the separation column 115 is stopped (step S27), as in step S4 above. On the other hand, if the connection state is correct (Yes), the control device 101 determines whether the reading of the medium 601 (FIG. 3) of the separation column 115 is normal (step S28). If the reading is abnormal (No), for example, if the detection state is not a predetermined one, if the medium 601 cannot be read normally, or if the reading is not normal (No), the replacement work of the separation column 115 is stopped (step S29), as in step S4 above. On the other hand, if the connection state is correct (Yes), the control device 101 fixes the connection using the shaft fixing mechanism 703 (FIG. 3) (step S30). This completes the connection between the separation column 115 and the analysis flow path 123.
[0062] Next, the control device 101 starts the operation of the heating device 309 (FIG. 2) and the liquid delivery pump 106 (FIG. 1) (step S31), and starts equilibration of the separation column 115 (step S32).
[0063] 11 is a diagram illustrating the light emission patterns of the LED switch 201 in steps S21 to S32 (FIG. 10) when installing the separation column 115. The light emission patterns A to E shown in FIG. 11 are the same as the light emission patterns A to E shown in FIG. 8 above.
[0064] In step S32, light emission pattern A is used. In step S22, light emission pattern B is used. In step S21, light emission pattern C is used, and in step S27, light emission pattern D is used. In steps S24, S25, S30, S31, and S32, light emission pattern E is used.
[0065] In step S23, the light emission pattern B in step S22 continues to be used. In step S26, the light emission pattern E in step S25 continues to be used. In step S28, the light emission pattern D in steps S25 and S26 continues to be used. In step S29, the light emission pattern D in steps S27 and S28 continues to be used.
[0066] 11 of the above-mentioned Patent Document 1, the rotary drive shaft can rotate when not energized. However, according to the liquid chromatograph 100 of the first embodiment, after the separation columns 115, 116, and 117 are attached, the attached separation columns 115, 116, and 117 can be fixed using the shaft fixing mechanism 703 (locking mechanism 200) provided on the motor 701 (FIG. 3). This prevents the motor main body 702 from being unintentionally driven, and prevents the separation columns 115, 116, and 117 from being unintentionally removed.
[0067] 12 is a system diagram of a liquid chromatograph 1001 of the second embodiment. The liquid chromatograph 1001 is the same as the liquid chromatograph 100 (FIG. 1) except that it does not include the LED switches 201, 202, and 203 (FIG. 1). The liquid chromatograph 1001 includes a display device 102 as an alarm device, and the same information as that described above with reference to FIG. 8 is displayed on the display device 102.
[0068] The technology described in Patent Document 1 above does not mention, for example, displaying the removal status. However, with the liquid chromatograph 1001 of the second embodiment, the user can work while understanding the content displayed on the display device 102, making the work easier. Furthermore, since information can be conveyed to the user through the display device 102, increasing the amount of information displayed on the display device 102 can help the user understand the work. Furthermore, the number of parts can be reduced.
[0069] 13 is a diagram illustrating the removal of the separation column 115 from the liquid chromatograph 1002 of the third embodiment, with the analysis flow path 123 and the separation column 115 connected. Note that the installation can be performed in the order of FIGS. 15, 14, and 13, which will be described later.
[0070] Liquid chromatograph 1002 has a solenoid lock 311 as the locking mechanism 200 instead of shaft fixing mechanism 703 (FIG. 3). Furthermore, slide mechanism 700 provided in liquid chromatograph 1002 further has lever 316 that slides analytical flow path 123 (the other structure) when operated by the user. Other than these points, liquid chromatograph 1002 is the same as liquid chromatograph 100 (FIG. 1).
[0071] The solenoid lock 311 is disposed on the separation column 115 side of the linear guide 308, which is integral with the analysis channel 123. When not energized, the solenoid lock 311 protrudes from the side end of the linear guide 308 (the side opposite the separation column 115). This restricts the sliding of the slide mechanism 700. On the other hand, as will be described in detail later, when energized, the solenoid lock 311 retracts downward at the other end of the linear guide 308, thereby releasing the restriction on the sliding of the analysis channel 123. Therefore, the solenoid lock 311 can control whether the analysis channel 123 can slide, depending on whether or not it is energized.
[0072] 14 is a diagram illustrating the removal of the separation column 115 from the liquid chromatograph 1002 of the third embodiment, showing the state in which the analysis channel 123 is slid by pulling up the lever 316. The lever 316 is formed integrally with the crank arm 315. Pulling up the lever 316 rotates the pivots 331, 332, and 333, changing the direction of the force, and the analysis channel 123 slides away from the separation column 115. The lever 316 allows the user to slide the analysis channel 123 with a simple structure.
[0073] As described above, the sliding restriction on the analysis channel 123 is released by energizing the solenoid lock 311. When the user pulls up the lever 316 in this state, the analysis channel 123 slides away from the separation column 115, as shown in Figure 14. At this time, the open detection sensor 312 is not detecting anything, and the connection detection sensor 313 is also not detecting anything.
[0074] 15 is a diagram illustrating the removal of the separation column 115 from the liquid chromatograph 1002 of the third embodiment, with the analysis flow path 123 locked in a disconnected state. When the user fully pushes up the lever 316, the open detection sensor 312 detects the fitting holder 307. This causes the solenoid lock 311 to protrude, fixing the linear motion guide 308 on the separation column 115 side of the linear motion guide 308. Meanwhile, the restoring force of the compression spring 306 prevents the shaft 317 from protruding outside the support base 318. This causes the connection detection sensor 313 to go into non-detection mode.
[0075] 16 is a flowchart illustrating a method for removing the separation column 115 (a method for controlling the analyzer) in the liquid chromatograph 1002 of the third embodiment. In FIG. 16, the same steps as those in FIG. 7 above are assigned the same step numbers, and their explanations will be omitted.
[0076] After steps S1 to S6 are performed, the control device 101 (FIG. 1) energizes the solenoid lock 311 of the connection part 112, thereby releasing the locking by the locking mechanism 200 (FIG. 13) (step S37, corresponding to step S7 (FIG. 7)). Next, the user pulls up the lever 316, thereby releasing the connection between the analysis channel 123 and the separation column 115 (step S38, corresponding to step S8 (FIG. 7)). Then, after steps S9 and S10 are performed, the control device 101 (FIG. 1) deenergizes the solenoid lock 311 of the connection part 112, thereby locking the analysis channel 123 with the locking mechanism 200 (step S41, corresponding to step S11 (FIG. 7)). This prevents the analysis channel 123 from sliding unintentionally during the removal of the separation column 115. Finally, step S12 is performed.
[0077] 17 is a flowchart illustrating a method for attaching a separation column 115 to a liquid chromatograph 1002 according to the third embodiment. In FIG. 17, the same steps as those in FIG. 10 above are given the same step numbers, and their explanations will be omitted.
[0078] After steps S21 to S23 have been performed, the control device 101 (FIG. 1) energizes the solenoid lock 311 of the connection part 112, thereby releasing the locking by the locking mechanism 200 (FIG. 13) (step S44, corresponding to step S24 (FIG. 10)). Next, the user presses down the lever 316 to connect the analysis flow path 123 and the separation column 115 (step S45, corresponding to step S25 (FIG. 10)). Then, after steps S26 to S29 have been performed, the control device 101 (FIG. 1) deenergizes the solenoid lock 311 of the connection part 112, thereby locking the connection by the locking mechanism 200 (step S50, corresponding to step S30 (FIG. 10)). This secures the connection between the analysis flow path 123 and the separation column 115, preventing unintentional removal of the separation column 115. Then, steps S31 and S32 are performed.
[0079] The technology described in Patent Document 1 does not describe a specific method for removing a separation column. However, according to the liquid chromatograph 1002 of the third embodiment, by using the solenoid lock 311 as the locking mechanism 200, it is possible to prevent unintentional removal of the separation column 115 using the lever 316. Furthermore, by using the solenoid lock 311, which is locked when not energized, a fail-safe function can be achieved. Furthermore, by using the lever 316 for sliding, the device configuration can be simplified.
[0080] 18 is a diagram illustrating the removal of the separation column 115 from the liquid chromatograph 1003 of the fourth embodiment, with the analysis flow path 123 and the separation column 115 connected. Note that installation can be performed in the order of FIGS. 20, 19, and 18, which will be described later.
[0081] The liquid chromatograph 1003 is the same as the liquid chromatograph 100 (FIG. 1), except that it includes a solenoid lock 311 as the locking mechanism 200 instead of the shaft fixing mechanism 703 (FIG. 3). The rotation drive shaft (not shown) of the motor body 702 included in the motor 701 of the liquid chromatograph 1003 does not include the shaft fixing mechanism 703, and therefore can rotate even when not energized. Therefore, the solenoid lock 311 locks the linear guide 308, which is integral with the analytical flow path 123, thereby preventing sliding. This prevents unintentional disconnection and prevents unintentional removal of the separation column 115.
[0082] The solenoid lock 311 is driven in the same manner as in the third embodiment. For example, the solenoid lock 311 protrudes toward the separation column 115 of the linear guide 308, thereby preventing the analysis channel 123 from sliding toward the separation column 115.
[0083] 19 is a diagram illustrating the removal of the separation column 115 from the liquid chromatograph 1003 of the fourth embodiment, showing the state in which the analysis channel 123 is sliding in the unlocked state. When the locking mechanism 200 is unlocked, the rotation drive shaft (not shown) rotates due to the application of electricity to the motor body 702, and the analysis channel 123, which is integrated with the linear guide 308, slides toward the separation column 115.
[0084] 20 is a diagram illustrating the removal of the separation column 115 from the liquid chromatograph 1003 of the fourth embodiment, with the analysis channel 123 locked in the disconnected state. The solenoid lock 311 protrudes from the linear guide 308 on the separation column 115 side, thereby preventing the linear guide 308 from sliding toward the separation column 115.
[0085] 11 of the above-mentioned Patent Document 1, the rotary drive shaft can rotate when not energized. However, in the liquid chromatograph 1003 of the fourth embodiment, the solenoid lock 311 can be used to limit and lock the sliding of the motor.
[0086] The present invention is not limited to the above-described embodiments and includes various modifications. For example, the above-described embodiments have been described in detail to clearly explain the present invention, and the present invention is not necessarily limited to those including all of the described configurations. Furthermore, it is possible to replace part of the configuration of one embodiment with the configuration of another embodiment, or to add the configuration of another embodiment to the configuration of one embodiment. Furthermore, it is possible to add, delete, or replace part of the configuration of each embodiment with other configurations. [Explanation of symbols]
[0087] 1,2,3 Stream 100, 1001, 1002, 1003 Liquid chromatograph (analytical equipment) 101 Control device 102 Display device (alarm device) 1021 Input Device 103,104,105 Separation section 106,107,108 Liquid transfer pump 109,110,111 Sample injection valve 112,113,114 Connections 115,116,117 Separation columns 118 Flow path switching valve 119 Mass spectrometer 120,121,122,123,124,125 Analysis channel 200 Locking mechanism 201, 202, 203 LED switch (alarm device) Stage 301 302 Heat Block 303 Column Heat Block 304 Column Cartridge 305,307 Fitting holder 306 Compression Spring 308 Linear guide 309 Heating device 310 Temperature Sensor 311 Solenoid lock (locking mechanism) 312 Open detection sensor (second sensor) 313 Connection detection sensor (first sensor) 314 Reading device 315 crank arm 316 Lever 317 Shaft 318 Support stand 331, 332, 333 Rotating shaft 601 Medium 700 slide mechanism 701 Motor 702 Motor body 703 Axis fixing mechanism (locking mechanism)
Claims
[Claim 1] a plurality of removable separation columns connected in parallel; a plurality of analytical flow paths connected to the plurality of separation columns, respectively, for passing a sample through the plurality of separation columns; a locking mechanism that restricts removal of the separation columns other than the separation column to be removed; a slide mechanism that connects the separation column and the analysis flow path by sliding one of the structures, which is the separation column or the analysis flow path, relative to the other structure that is placed; a control device that controls the locking mechanism, Releasing the locking mechanism releases the connection between the separation column and the analysis channel; The locking mechanism restricts the sliding of the other structure. An analytical device characterized by:
Citation Information
Patent Citations
Separation column connection device, connection method, and analysis system
JP6611398B2