Analyzer and method for controlling analyzer
Patent Information
- Application Number
- JP2024217035
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2021-04-23
- Filing Date
- 2024-12-11
- Publication Date
- 2025-02-21
- Estimated Expiration
- 2042-02-03
AI Technical Summary
【0009】 本開示によれば、意図しない分離カラムの取り外しを抑制可能な分析装置及び分析装置の制御方法を提供できる。
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Figure 2025026688000001_ABST
Abstract
Description
[Technical field]
[0001] The present disclosure relates to an analysis device and a method for controlling an analysis device. [Background technology]
[0002] In analytical instruments such as liquid chromatographs, separation columns packed with a packing material called the stationary phase are used to isolate analytes from contaminants or to separate multiple analytes from one another. In a mutual 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 it moves through the stationary phase, the analytes are separated due to differences in the strength of interaction between the substance groups 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 a 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. As the detector, a photometer, mass spectrometer, or the like is appropriately selected depending on the purpose of analysis, the sample, etc. Furthermore, the analytical device includes, for example, a control device that analyzes the results detected by the detection unit.
[0004] In order to improve throughput, an analytical device may be equipped with multiple separation columns. In this case, the separation column to be used can be selected by switching using a valve, so that analysis can be performed using 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 connection device having: a column holder for holding a separation column; a first fitting holder mounting a first fitting having a seal part connecting to an upstream seal part of the separation column and connected to an upstream piping; a second fitting holder mounting a second fitting having a seal part connecting to a downstream seal part of the separation column and connected to a downstream piping; a main body member to which one of the first fitting holder and 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 other than the part to be removed may be removed unintentionally 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 and a method for controlling an analytical device that are capable of suppressing 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 and the analysis flow paths by sliding one of the structures that is the separation columns or the analysis flow paths relative to the other structure that is placed, and a control device that controls the locking mechanism, in which the connection between the separation columns and the analysis flow paths is released by releasing the locking mechanism, and the locking mechanism restricts the sliding of the other structure. Other solutions will be described later in the description of the embodiment of the invention. Effect of the Invention
[0009] According to the present disclosure, it is possible to provide an analyzer and a method for controlling an analyzer that can prevent unintentional removal of a separation column. [Brief description of the drawings]
[0010] [Figure 1] FIG. 1 is a system diagram of a liquid chromatograph according to a first embodiment. [Diagram 2] FIG. 13 is a diagram illustrating the state when the separation column is removed, with the analysis flow path and the separation column still connected. [Diagram 3] FIG. 4 is a block diagram of a slide mechanism. [Figure 4] FIG. 1 is a diagram illustrating a medium for identifying a separation column. [Diagram 5] FIG. 13 is a diagram illustrating removal of the separation column, showing the state in which the analysis channel is slid by releasing the locking mechanism. [Figure 6] FIG. 13 is a diagram illustrating the removal of the separation column, showing the state in which the analysis flow path is locked in the unlocked state. [Figure 7] 1 is a flow chart illustrating a method for removing a separation column. [Figure 8] 11A and 11B are diagrams illustrating light emission patterns of an LED switch. [Figure 9] FIG. 13 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 flow chart illustrating a method for attaching a separation column. [Figure 11] FIG. 13 is a diagram illustrating the light emission pattern of the LED switch for each step when attaching the separation column. [Figure 12] FIG. 11 is a system diagram of a liquid chromatograph according to a second embodiment. [Figure 13] FIG. 13 is a diagram for explaining the state when a 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. 13 is a diagram for explaining removal of a separation column in the liquid chromatograph of the third embodiment, in which the analysis flow path is slid by pulling up the lever. [Figure 15] FIG. 13 is a diagram for explaining removal of a separation column in the liquid chromatograph of the third embodiment, in which the analysis flow path is locked in a disconnected state. [Figure 16] 13 is a flowchart illustrating a method for removing a separation column in the liquid chromatograph of the third embodiment. [Figure 17] 13 is a flowchart illustrating a method for attaching a separation column in the liquid chromatograph of the third embodiment. [Figure 18] FIG. 13 is a diagram illustrating the liquid chromatograph of the fourth embodiment when a separation column is removed, showing a state in which the analysis flow path and the separation column are connected. [Figure 19] FIG. 13 is a diagram illustrating removal of a separation column in the liquid chromatograph of the fourth embodiment in an unlocked state, with the analysis flow path being slid. [Figure 20] FIG. 13 is a diagram for explaining removal of a separation column in the liquid chromatograph of the fourth embodiment, in which the analysis flow path is locked in a disconnected state. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0011] Hereinafter, a form for carrying out the present disclosure (referred to as an embodiment) 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 following one embodiment, and different embodiments can be combined with each other or modified as desired without significantly impairing the effects of the present disclosure. In addition, the same symbols will be used for the same members, and duplicate descriptions will be omitted. Furthermore, members 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 a range that does not significantly impair the effects of the present disclosure, and some members 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 exemplified as the analytical device, but the analytical device may 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 a plurality of 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] The separation units 103, 104, and 105 each include a removable separation column 115, 116, and 117. Thus, the liquid chromatograph 100 includes a plurality of removable separation columns 115, 116, and 117 that are connected in parallel. The liquid chromatograph 100 includes a plurality of analysis flow paths 120, 121, 122, 123, 124, and 125. The 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 the plurality of separation columns 115, 116, and 117, respectively.
[0015] The separation section 103 includes a liquid delivery pump 106 (liquid delivery section), a sample injection valve 109 (sample injection section), a connection section 112, analysis flow paths 120, 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 section 112. The analysis flow paths 120, 123 are connected to the separation column 115, and allow the sample to flow through the separation column 115.
[0016] The separation section 104 includes a liquid delivery pump 107 (liquid delivery section), a sample injection valve 110 (sample injection section), a connection section 113, analysis flow paths 121, 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 section 113. The analysis flow paths 121, 124 are connected to the separation column 116, and allow the sample to flow through the separation column 116.
[0017] The separation section 105 includes a liquid delivery pump 108 (liquid delivery section), a sample injection valve 111 (sample injection section), a connection section 114, analysis flow paths 122, 125, and an LED switch 203. The liquid delivery pump 108 delivers a plurality of different solvents while changing their concentrations. The sample injection valve 111 introduces the sample into the analysis flow path 122. A separation column 117 is installed in the connection section 114. The analysis flow paths 122, 125 are connected to the separation column 117, and allow the sample to flow through the separation column 117.
[0018] The LED switches 201, 202, and 203 (examples of notification devices) are provided in the liquid chromatograph 100 and notify the user of the removable separation columns 115, 116, and 117 among the multiple separation columns 115, 116, and 117. By providing the LED switches 201, 202, and 203, the user who has been notified can easily know which separation columns 115, 116, and 117 should be removed.
[0019] The LED switches 201, 202, and 203 have an LED lamp and a switch function, and in addition to notifying the state of the removable separation columns 115, 116, and 117, their light emission state changes according to the state of the connection parts 112, 113, and 114. The LED switches 201, 202, and 203 notify by, for example, turning on or off the LED lamp, changing the color tone, 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 device is not limited to the LED switches 201, 202, and 203, and may be a light source other than an LED lamp, a speaker that emits sound, 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, a flow path switching valve 118, and a mass spectrometer 119. The control device 101 also controls a lock mechanism 200 (FIG. 3), which will be described in detail later. The control device 101 includes, for example, a CPU (Central Processing Unit), a RA, and the like, neither of which are shown in the figure. The control device 101 is configured to include a random access memory (RAM), a read only memory (ROM), etc. A predetermined control program stored in the ROM is loaded into the 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 pieces of information such as analysis results and information related to the progress of the analysis. The display device 102, together with the above-mentioned LED switches 201, 202, and 203, also notifies which of the multiple separation columns 115, 116, and 117 are removable.
[0023] The liquid chromatograph 100 is provided 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, so that the separation columns 115, 116, and 117 can be connected to the analysis flow paths 123, 124, and 125.
[0024] 2 is a diagram for explaining the removal of separation column 115, in which analysis flow paths 120, 123 and separation column 115 are connected. FIG. 2 illustrates connection part 112, but 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 removal and attachment of separation columns 116, 117 will be omitted. In this specification, analysis flow path 123 is slid by slide mechanism 700, but a slide mechanism (not shown) for sliding separation column 115 may be provided.
[0025] The sample moves inside the analysis channels 120, 123 in the direction of arrow 300, enters the separation column 115 through the analysis channel 120, and exits the separation column 115 through the analysis channel 123. Therefore, one end (inlet) and the other end (outlet) of the separation column 115 are connected to the analysis channels 120, 123, 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, 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 is in contact with the heat block 302. That is, the heat block 302 is in 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 structure), which is one of the structures being 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 bending crank arm 315, and the rotational driving force of the motor 701 is converted by the crank arm 315 into a propulsive force in the direction of the separation column 115 of the analysis channel 123. 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] For example, the rotation speed, torque, rotation timing, etc. of the motor 701 are controlled by the control device 101. In addition, when 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, so that even a small motor 701 can 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 the locking mechanism 200. The rotary drive shaft can rotate even when the motor body 702 is not energized, but by providing the shaft fixing mechanism 703, the rotary drive shaft can be fixed when not energized, and the sliding of the analysis channel 123 can be restricted. In the first embodiment, the rotary drive shaft of the motor body 702 connected to the separation columns 116, 117 is fixed by the shaft fixing mechanism 703. This maintains the connection between the separation columns 116, 117 and the analysis channel 123, and prevents the separation columns 116, 117 from being unintentionally removed.
[0032] The locking mechanism 200 restricts removal of the separation columns 116, 117 (FIG. 1) other than the separation column 115 to be removed. During replacement of the separation column 115, the locking mechanism 200 allows the separation column 115 to be removed to be removed, while the separation columns 116, 117 other than the separation column 115 to be removed are locked. This makes it possible to prevent unintentional removal of the separation columns 116, 117.
[0033] The locking mechanism 200 restricts the sliding of the analysis channel 123 by the slide mechanism 700. This makes it possible to prevent the separation column 115 from being disconnected from the analysis channel 123 when locked by the locking mechanism 200, and thus to prevent 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 a medium 601 that includes information for identifying an installed separation column 115. By including the reader 314, the separation column 115 can be identified, thereby making it possible to prevent 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 may 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) indicating the relationship between the number and identification information stored in the control device 101 (FIG. 1).
[0036] In the illustrated example, the medium 601 is an RFID tag that is an identifier. The medium 601 is read when the separation column 115 is placed thereon. When replacing the separation column 115, the reader 314 reads various pieces of information such as the type of separation column 115 to which the medium 601 is attached, the serial number, and which connection part 112, 113, 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 of the time to replace the separation column 115 via the display device 102. When replacing the separation column 115, a record of use is written in the medium 601 attached to the separation column 115 to be replaced, thereby preventing reuse.
[0037] The open detection sensor 312 (second sensor) detects the disconnection of the analysis flow path 123 to the downstream side, which is the other end side, of the separation column 115. The connection detection sensor 313 (first sensor) detects the connection of the analysis flow path 120 to the upstream side, which is one end side, 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 the shading, reflection, etc. 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 present 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 placed at the farthest position from the separation column 115. This detection detects the disconnection of the separation column 115 and the analysis channel 123.
[0039] The connection detection sensor 313 detects the shaft 317 that protrudes to the side of the support base 318 due to the movement of the separation column 115 to the left in the drawing. In the example shown, the separation column 115 and the analysis channel 123 are arranged coaxially. Therefore, the shaft 317 arranged to the side of the separation column 115 pushes the compression spring 306 and protrudes to the side of 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) performs a restriction by the locking mechanism 200 when either the open detection sensor 312 or the connection detection sensor 313 detects. In this manner, sliding is restricted in both the disconnected and connected states. This makes it possible to easily 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 for explaining removal of separation column 115, in which analysis channel 123 is slid by releasing locking mechanism 200. In this state, fitting holder 307 is not present above open detection sensor 312, and open detection sensor 312 is not detecting. Meanwhile, shaft 317 does not protrude to the left of support base 318 due to the restoring force of compression spring 306, and connection detection sensor 313 is not detecting. Therefore, since both connection detection sensor 313 and open detection sensor 312 are not detecting, no restriction is imposed by locking mechanism 200. By releasing the lock by locking mechanism 200, the rotary drive shaft of motor body 702 (FIG. 3) becomes rotatable.
[0042] With lock mechanism 200 (FIG. 3) released, the connection between separation column 115 and analysis flow path 123 is released by energizing motor body 702 (FIG. 3). This separates separation column 115 from analysis flow path 123, and separation column 115 can be removed from liquid chromatograph 100, as will be described in detail later with reference to FIG. 7. In the illustrated example, energizing motor body 702 (FIG. 3) causes analysis flow path 123 to slide in a direction away from separation column 115. This releases the connection between separation column 115 and analysis flow path 123.
[0043] FIG. 6 is a diagram for explaining removal of the separation column 115, in which the analysis channel 123 is locked in an unlocked state. When the analysis channel 123 is slid in a direction away from the separation column 115, the linear guide 308 eventually reaches the farthest position to which it can slide. At the same time, the sliding by the slide mechanism 700 stops. In addition, the open detection sensor 312 detects the linear guide 308 and detects a disconnection. On the other hand, the connection detection sensor 313 is not detecting, as in the case of referring to FIG. 5 above. Therefore, since the open detection sensor 312 is detected, the sliding is restricted by the lock mechanism 200. As a result, the analysis channel 123 is locked at the farthest position from the separation column 115, so that the separation column 115 can be removed without being affected by the analysis channel 123.
[0044] Thus, further, the locking mechanism 200 (FIG. 3) restricts the sliding of the analysis channel 123 as shown in FIG. 6 when the separation column 115 is disconnected from the analysis channel 123. Since 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 attaching the separation column 115, the process is reversed from the above. That is, in the state shown in Fig. 6, the user replaces the separation column 115, and one end of the new separation column 115 is pressed against the analysis flow path 120. Next, the slide mechanism 700 slides the analysis flow path 123 in the direction approaching the separation column 115, in the order of Figs. 6, 5, and 2. This allows the separation column 115 and the analysis flow path 123 to be connected.
[0046] Fig. 7 is a flow chart for explaining a method for removing the separation column 115 (a method for controlling the analytical device). The separation columns 116, 117 (Fig. 1) can also be removed in a manner similar to that shown in Fig. 7. Fig. 7 will be described 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, or the like (step S1). Alternatively, the user instructs the control device 101 to replace the separation column 115 by instructing the input device 1021 (step S1). The control device 101 notifies the user of the separation column 115 to be removed through 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 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 when the analysis is completed, so that the time to remove the separation column 115 can be known by detecting the end of the analysis.
[0049] Specifically, the controller 101 releases the restriction on removal by the lock 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 end of analysis to be known 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, falls due to heating being stopped upon completion 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 by the locking mechanism 200 when the internal pressure of at least one of the analysis flow path 120 or the separation column 115 falls to a predetermined value or less (the latter half of step S3). As a result, when the internal pressure of at least one of the analysis flow path 120 or the separation column 115, which is high during operation, drops due to the end of analysis, the end of analysis can be determined based on the pressure, and removal can be performed at an appropriate time. For example, by releasing the restriction when the internal pressure is equal to or less than a predetermined value indicating a state close to atmospheric pressure, unintended leakage of sample from at least one of the analysis flow path 120 or the separation column 115 can be sufficiently suppressed. The internal pressure of at least one of the analysis 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 it is determined in step S3 that the separation column 115 is "abnormal" because it exceeds the predetermined value, the replacement work of the separation column 115 is stopped, and the control device 101 notifies the user by at least one of the LED switch 201 and the display device 102 as a system alarm (step S4). On the other hand, if it is determined in step S3 that the separation column 115 is "normal" because it is equal to or less than the predetermined value, the control device 101 notifies the user by 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 is to be replaced.
[0053] The user presses the LED switch 201 or the 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 lock mechanism 200 (FIG. 3) (step S7). The control device 101 energizes the motor body 702 (FIG. 3) by sending an electric signal, and disconnects the separation column 115 from the analysis flow path 123 (step S8). After disconnection, the control device 101 judges whether the open state is correct or not (step S9). Specifically, the control device 101 judges that the open state is correct when the open detection sensor 312 detects the disconnection of the analysis flow path 123 as shown in FIG. 6. If it is not correct (No), the replacement work of the separation column 115 is stopped as in step S4 above (step S10).
[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 process). This fixes the rotation drive shaft of the motor main body 702 (FIG. 3) and restricts 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 for explaining the light emission patterns of the LED switch 201. In steps S1 to S12 (FIG. 7), any one of the light emission patterns A to E shown in FIG. 8 is appropriately selected and emitted. Light emission pattern A is off. 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 flash of green light (turning off after flashing twice in a row). Light emission pattern C is used when the user is performing replacement work when removing and installing the separation column 115 (described below). Light emission pattern D is, for example, a rapid flash of green light. 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 in operation during the replacement work of the separation column 115.
[0057] 9 is a diagram illustrating the light emission patterns of the LED switch 201 in 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] Fig. 10 is a flow chart for explaining a method for attaching the separation column 115. The separation columns 116, 117 (Fig. 1) can also be attached in a similar manner to that shown in Fig. 10. Fig. 10 will be explained with reference to Fig. 1 as appropriate. The method for attaching the separation column 115 includes steps S21 to S32.
[0060] The control device 101 notifies the user of the separation column 115 to be attached 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 attached to the connection part 112. In addition, 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 completing the installation, the user presses at least one of the LED switch 201 and the button (not shown) of 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 starts sliding toward the separation column 115 of the analysis flow channel 123 by energizing the motor body 702 (FIG. 3) by transmitting an electric signal to the motor body 702 (FIG. 3) (step S25).
[0061] The control device 101 judges whether the connection state is correct (step S26). Specifically, when the connection detection sensor 313 (FIG. 2) detects the connection of the analysis flow path 123, the control device 101 judges that the connection state is correct. If the connection state is not correct (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 judges whether the reading of the medium 601 (FIG. 3) of the separation column 115 is normal (step S28). If the reading is not normal (No), for example, if the detection state is not a predetermined one, if the medium 601 cannot be read normally, or the like, 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 by 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 controller 101 starts the operation of the heater 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.
[0064] In step S32, the light emission pattern A is used. In step S22, the light emission pattern B is used. In step S21, the light emission pattern C is used, and in step S27, the light emission pattern D is used. In steps S24, S25, S30, S31, and S32, the light emission pattern E is used.
[0065] In step S23, the light emission pattern B in step S22 is continued to be used. In step S26, the light emission pattern E in step S25 is continued to be used. In step S28, the light emission pattern D in steps S25 and S26 is continued to be used. In step S29, the light emission pattern D in steps S27 and S28 is continued to be used.
[0066] In the motor shown in Fig. 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, 117 are attached, the attached separation columns 115, 116, 117 can be fixed using the shaft fixing mechanism 703 (lock mechanism 200) provided in the motor 701 (Fig. 3). This makes it possible to prevent the motor body 702 from being unintentionally driven, and to prevent the separation columns 115, 116, 117 from being unintentionally removed.
[0067] Fig. 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 displays on the display device 102 the same content as that described with reference to Fig. 8 above.
[0068] The technology described in the above Patent Document 1 does not, for example, mention displaying the removal state. However, according to the liquid chromatograph 1001 of the second embodiment, the user can work while grasping the contents displayed on the display device 102, making the work easier. Also, since information can be conveyed to the user through the display device 102, the user's understanding of the work can be supported by increasing the amount of information displayed on the display device 102. Also, the number of parts can be reduced.
[0069] 13 is a diagram for explaining removal of separation column 115 in liquid chromatograph 1002 of the third embodiment, in which analysis flow path 123 and separation column 115 are connected. Note that installation can be performed in the order of Figures 15, 14, and 13, which will be described later.
[0070] Liquid chromatograph 1002 includes a solenoid lock 311 as lock mechanism 200 instead of shaft fixing mechanism 703 (FIG. 3). Slide mechanism 700 included in liquid chromatograph 1002 further includes lever 316 that slides analysis flow channel 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. The solenoid lock 311 protrudes from the side end of the linear guide 308 (the side opposite the separation column 115) when not energized. This restricts the sliding of the slide mechanism 700. On the other hand, the solenoid lock 311 retracts downward at the other end of the linear guide 308 when energized, as will be described in detail later, and the restriction on the sliding of the analysis channel 123 is released. Therefore, the solenoid lock 311 can control whether the analysis channel 123 can slide or not depending on whether or not electricity is applied.
[0072] 14 is a diagram illustrating the removal of separation column 115 from liquid chromatograph 1002 of the third embodiment, in which lever 316 is pulled up to slide analysis flow path 123. Lever 316 is formed integrally with crank arm 315. Pulling up lever 316 causes rotation of pivots 331, 332, and 333 to change the direction of force, causing analysis flow path 123 to slide away from separation column 115. Lever 316 allows the user to slide analysis flow path 123 with a simple structure.
[0073] As described above, the restriction on the sliding of 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, and the connection detection sensor 313 is also not detecting.
[0074] 15 is a diagram for explaining removal of separation column 115 in liquid chromatograph 1002 of the third embodiment, in which the analysis flow path 123 is locked in a disconnected state. When a user pushes lever 316 all the way up, open detection sensor 312 detects fitting holder 307. This causes solenoid lock 311 to protrude, and fixes linear motion guide 308 on the separation column 115 side of linear motion guide 308. Meanwhile, shaft 317 does not protrude outside support base 318 due to the restoring force of compression spring 306. This causes connection detection sensor 313 to go into non-detection.
[0075] 16 is a flow chart for explaining a method for removing the separation column 115 (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 are given the same step numbers, and the explanation thereof will be omitted.
[0076] After steps S1 to S6 are performed, the controller 101 (FIG. 1) energizes the solenoid lock 311 of the connection part 112 to release the locking by the locking mechanism 200 (FIG. 13) (step S37, which corresponds to step S7 (FIG. 7)). Next, the user pulls up the lever 316 to release the connection between the analysis channel 123 and the separation column 115 (step S38, which corresponds to step S8 (FIG. 7)). Then, after steps S9 and S10 are performed, the controller 101 (FIG. 1) deenergizes the solenoid lock 311 of the connection part 112 to perform locking by the locking mechanism 200 (step S41, which corresponds to step S11 (FIG. 7)). This makes it possible to prevent the analysis channel 123 from sliding unintentionally during the removal of the separation column 115. Finally, step S12 is performed.
[0077] Fig. 17 is a flow chart for explaining a method for attaching a separation column 115 in a liquid chromatograph 1002 of the third embodiment. In Fig. 17, the same steps as those in Fig. 10 above are given the same step numbers, and the explanation thereof will be omitted.
[0078] After steps S21 to S23 are performed, the controller 101 (FIG. 1) energizes the solenoid lock 311 of the connection part 112 to release the lock by the lock 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 to the separation column 115 (step S45, corresponding to step S25 (FIG. 10)). Then, after steps S26 to S29 are performed, the controller 101 (FIG. 1) deenergizes the solenoid lock 311 of the connection part 112 to lock the connection by the lock mechanism 200 (step S50, corresponding to step S30 (FIG. 10)). This fixes the connection between the analysis flow path 123 and the separation column 115, making it possible to prevent unintentional removal of the separation column 115. Then, steps S31 and S32 are performed.
[0079] The technology described in the above Patent Document 1 does not describe a specific method for removing the 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. In addition, by using the solenoid lock 311 that is locked in a non-energized state, a fail-safe function can be achieved. Furthermore, by using the lever 316 for sliding, the device configuration can be simplified.
[0080] Fig. 18 is a diagram for explaining removal of separation column 115 in liquid chromatograph 1003 of the fourth embodiment, in a state in which analysis flow path 123 and separation column 115 are 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 has a solenoid lock 311 as the lock mechanism 200 instead of the shaft fixing mechanism 703 (FIG. 3). The rotation drive shaft (not shown) of the motor body 702 provided in the motor 701 of the liquid chromatograph 1003 does not have the shaft fixing mechanism 703, and therefore can rotate even when not energized. Therefore, the solenoid lock 311 locks the linear guide 308 formed integrally with the analysis flow path 123, thereby making it possible to suppress sliding. This makes it possible to suppress unintended disconnection and unintended 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 side of the linear motion guide 308, thereby preventing the analysis channel 123 from sliding toward the separation column 115.
[0083] 19 is a diagram for explaining removal of separation column 115 from liquid chromatograph 1003 of the fourth embodiment, in which analysis channel 123 is slid in an unlocked state. When lock mechanism 200 is unlocked, a rotating drive shaft (not shown) rotates due to energization of motor body 702, and analysis channel 123 integrated with linear guide 308 slides toward separation column 115.
[0084] 20 is a diagram illustrating the removal of the separation column 115 in the liquid chromatograph 1003 of the fourth embodiment, in which the analysis flow path 123 is locked in a disconnected state. The solenoid lock 311 protrudes from the separation column 115 side of the linear motion guide 308, thereby preventing the linear motion 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, according to 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 modified examples. 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 configurations described. It is also possible to replace a part of the configuration of one embodiment with the configuration of another embodiment, and it is also possible to add the configuration of another embodiment to the configuration of one embodiment. It is also possible to add, delete, or replace a part of the configuration of each embodiment with another configuration. [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 delivery 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 flow path 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 (lock mechanism)
Claims
1. a plurality of removable separation columns connected in parallel; a plurality of analysis 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 on the separation column; A control device for controlling the lock mechanism, Releasing the locking mechanism releases the connection between the separation column and the analysis flow path; The locking mechanism restricts the sliding of the other structure.
1. An analytical device comprising:
2. Furthermore, the locking mechanism restricts the sliding of the other structure in a state in which the separation column is disconnected from the analysis flow path.
2. The analysis device according to claim 1 .
3. The apparatus further includes an input device that is connected to the control device and that is operated with the separation column placed thereon to release the restriction on the slide.
3. The analysis device according to claim 2 .
4. The slide mechanism includes: Sliding the other structure; A motor connected to the other structure The analysis device according to any one of claims 1 to 3.
5. The motor is A motor body that rotates a rotary drive shaft; The lock mechanism includes a shaft fixing mechanism that fixes the rotation drive shaft when the motor body is not energized.
5. The analysis device according to claim 4.
6. The slide mechanism includes: Sliding the other structure; A lever is provided for sliding the other structure by the user's operation. The analysis device according to any one of claims 1 to 3.
7. a notification device for notifying a removable separation column among the plurality of separation columns; The analysis device according to any one of claims 1 to 3.
8. A reading device is provided for reading information recorded on a medium including information for identifying the installed separation column. The analysis device according to any one of claims 1 to 3.
9. a locking step of restricting removal of the separation columns other than the separation column to be removed by a locking mechanism among a plurality of removable separation columns connected in parallel, Releasing the locking mechanism releases the connection between the separation columns and a plurality of analysis flow paths that are connected to the plurality of separation columns, respectively, and allow samples to flow through the plurality of separation columns, respectively; and The lock mechanism restricts sliding of one of the structures, which is the separation column or the analysis flow path, relative to the other structure placed thereon by a slide mechanism connecting the separation column and the analysis flow path. A method for controlling an analytical device.
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