JP5515096B2 - Automatic analysis pretreatment device and automatic analysis device equipped with automatic analysis pretreatment device - Google Patents

Description

  The present invention relates to an automatic analysis pretreatment device and an automatic analysis device including the automatic analysis pretreatment device.

  In order to perform measurement with high accuracy in the analysis of minute substances, pretreatment such as separation, concentration and purification of the sample is essential. Conventionally, this pretreatment has been performed manually in a state of being completely isolated from the external environment. Therefore, when the number of samples of the sample increases, the burden on the operator becomes considerable. Therefore, automation has been strongly desired. Regarding automation, Japanese Patent Application Laid-Open No. 2010-60474 (Patent Document 1) discloses a mass spectrometer that can perform sample pretreatment and analytical measurement fully automatically.

JP 2010-60474 A

  In order to analyze a sample having a high matrix such as a rock sample, analysis by a mass spectrometer or high performance liquid chromatography (HPLC) is performed. In the pretreatment of this analysis, an operation of separating and extracting necessary elements using an open column (column) is required. In this pretreatment, a sample dissolving solution (sample solution) in which a sample is dissolved is injected into an ion exchange resin sealed in a column, and a reagent is injected into the ion exchange resin into which the sample solution has been injected. . However, the conventional pretreatment apparatus as shown in Patent Document 1 does not include a mechanism for moving a nozzle for injecting a sample solution or a reagent into the column. Therefore, when the sample solution is injected, if the sample solution rebounds and adheres to the tapered part of the column, the attached sample solution cannot be injected into the ion exchange resin, and the amount of the sample solution to be measured decreases. This results in a problem that correct analysis results cannot be obtained. In addition, because the sample solution discharge position in the column and the reagent discharge position are the same, when the reagent is injected, the sample solution previously injected into the column rebounds, and the sample is injected into the nozzle for injecting the reagent. When the solution adheres, there arises a problem that the reagent is contaminated. Furthermore, since the position in the column where the reagent is discharged cannot be changed in the conventional apparatus, if the reagent discharge speed is too high, the reagent accumulates in the column, thereby disturbing the stability of the enclosed ion exchange resin. In addition, there is a problem that a sufficient reaction cannot be obtained in the ion exchange resin due to an increase in the speed of the reagent passing through the ion exchange resin.

  An object of the present invention is to provide an automatic analysis pretreatment apparatus capable of analyzing all of the injected sample solution.

  Another object of the present invention is to provide an automatic analysis pretreatment apparatus capable of preventing nozzles from being soiled.

  Another object of the present invention is to provide an automatic analysis pretreatment apparatus capable of discharging a sample solution or a reagent at a speed at which the steady state of the ion exchange resin is not disturbed.

  Another object of the present invention is to provide an automatic analysis pretreatment apparatus capable of rotating a nozzle along the inner peripheral wall of the column without contacting the nozzle with the inner peripheral wall of the column.

  The automatic analysis pretreatment apparatus of the present invention includes a dispensing stage including a nozzle, a nozzle moving mechanism, and a liquid dispensing apparatus, a column stage, and a command generator. The nozzle moving mechanism moves the nozzle in the XYZ directions according to the movement command generated by the command generation device. The liquid dispensing device discharges a predetermined amount of liquid from the nozzle at a discharge speed determined according to the dispensing command generated by the command generation device. The column stage includes one or more columns into which liquid is dispensed from nozzles. The command generator generates a movement command and a dispensing command. In particular, the command generation device of the automatic analysis pretreatment apparatus of the present invention dispenses a predetermined amount of liquid into the column while rotating the nozzle along the inner peripheral wall of the column without contacting the inner peripheral wall of the column. The movement command and dispensing command necessary for the operation are generated in synchronization. Here, the generation of the movement command and the dispensing command in synchronization means that the movement command and the dispensing command are generated in a time-related manner. If comprised in this way, since a nozzle does not contact the inner peripheral wall of a column, a nozzle will not be contaminated with the substance adhering to the inner peripheral wall of a column. Further, when the liquid is discharged while moving the nozzle so as to circulate along the inner peripheral wall of the column, the liquid is not concentrated and injected into a specific part in the column. Therefore, the steady state of the ion exchange resin enclosed by the reagent excavating a part of the ion exchange resin is not disturbed. In addition, since a predetermined amount of liquid is dispensed into the column while rotating the nozzle along the inner peripheral wall, it is possible to prevent the speed of the reagent passing through the ion exchange resin from increasing, Can sufficiently react the reagent. Therefore, a good analysis result can be obtained.

  The command generator generates a movement command and a discharge speed for commanding the position and moving speed of the nozzle necessary to prevent the liquid discharged from the nozzle from rebounding while the nozzle is orbiting along the inner peripheral wall. Generates a dispensing command to be issued in synchronization. With this configuration, the liquid discharged from the nozzle does not rebound and adheres to the nozzle, and therefore, the rebound liquid attached to the nozzle does not mix with the same kind of liquid sucked and discharged by the same nozzle. .

  The column used in the present invention includes a cylindrical portion having an opening into which a nozzle is inserted, a small-diameter cylindrical portion having a smaller diameter than that of the cylindrical portion and filled with an ion exchange resin, and the cylindrical portion and the small-diameter cylinder. And a tapered cylindrical portion located between the two. In this case, the command generation device is configured to generate a movement command so that the liquid discharged from the nozzle spouts the liquid onto the inner peripheral wall of the tapered cylindrical portion. If comprised in this way, the sample solution which adhered and remained to the taper-shaped cylindrical part can be washed away with another solution, for example, a reagent injected after sample solution injection, and can be made to inject into ion exchange resin. Therefore, when the sample solution is injected into the small-diameter cylindrical portion filled with the ion exchange resin, even if the sample solution adheres to the tapered cylindrical portion due to rebound of the sample solution or retention in the tapered cylindrical portion. Since the adhering sample solution can be flowed with the liquid discharged from the nozzle, the entire sample solution injected into the column can be analyzed.

  The nozzle may be composed of a nozzle body and a replaceable pipette tip attached to the tip of the nozzle body. With this configuration, even when the discharged liquid rebounds and adheres to the pipette tip, it is possible to contaminate other types of sample reagents and solutions simply by replacing the pipette tip attached to the tip of the nozzle. It can be easily prevented.

  In a more specific configuration of the present invention, the command generation device includes a discharge speed setting unit, a dispensing amount setting unit, a dispensing command generation unit, a distance setting unit, and a movement command generation unit. . The discharge speed setting unit commands the discharge speed from the pipette tip. The dispensing volume setting unit commands the dispensing volume from the pipette tip. The dispensing command generating unit generates a dispensing command based on the set discharge speed and dispensing amount. The distance setting unit commands a distance from the center position of the column. The movement command generation unit determines the movement speed of the nozzle based on the set discharge speed, dispensing amount, and distance from the center position of the column. The movement command generation unit generates a movement command including the determined movement speed so as to be synchronized with the dispensing command. With this configuration, the nozzles required to prevent the liquid ejected from the nozzles from bouncing even if there is a change in the size of the column to be used, the amount of liquid to be injected, the ejection speed or the analysis target, etc. The position and moving speed can be easily set.

  The present invention can also be grasped as an automatic analyzer including any of the above-described automatic analysis pretreatment apparatuses.

It is the schematic of an example of embodiment of the automatic analysis pre-processing apparatus of this invention. It is a figure which shows an example of the column used by embodiment of FIG. It is a figure which shows an example of the image displayed on the display part of a controller. It is a block diagram which shows a part of structure of the principal part of the signal processing circuit of the command generation device arrange | positioned divided | segmented inside a controller and a control part. It is a figure which shows the flowchart which shows an example in the case of performing a pre-analysis process. (A) And (B) is a figure which shows an example of the height which discharges a sample solution. It is a figure which shows the state in which a nozzle discharges a solution to a column, circling along an inner peripheral wall, without making it contact with the inner peripheral wall of a column.

  Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is a schematic view of an example of an embodiment of an automatic analysis pretreatment apparatus according to the present invention. In order to facilitate understanding, a part of the automatic analysis processing apparatus is omitted in FIG. As shown in FIG. 1, the automatic analysis preprocessing apparatus 1 includes a controller 3 having a display unit D, a control unit 5, and an apparatus body 7. The controller 3 displays items to be set for the operation of each unit of the apparatus body 7 on the display unit D. The controller 3 is provided with a setting input unit (not shown). The control unit 5 controls the operation of each unit of the apparatus body 7 according to the items set by the controller 3. The apparatus body 7 of the present embodiment includes a nozzle unit 11, rails 13 extending in the X-axis direction shown in the lower left region of FIG. 1, a pair of rails 15 extending in the Y-axis direction, a reagent stage 17, and a sample stage. 19, a pipette tip rack 21, a column stage 23, and a liquid recovery stage 25.

  The nozzle unit 11 is attached to the rail 13 so as to be movable in the X-axis direction by a drive source (not shown). The rail 13 is provided on the rail 15 so as to be movable in the Y-axis direction along the pair of rails 15 by a driving source (not shown). The nozzle unit 11 includes a nozzle 31 including a nozzle body 27 and a pipette tip 29 that is replaceably attached to the tip of the nozzle body 27. The nozzle 31 is attached to the rail 32 so as to be movable in the Z-axis direction by a drive source (not shown). In addition, a liquid dispensing device 35 (see FIG. 4) including a pump for discharging liquid from the nozzle is provided inside the nozzle unit 11. With such a configuration, the nozzle unit 11 can move in a plane (XY plane) surrounded by the rails 13 and 15, and can move in the XYZ directions in combination with the rails 32. Further, not only the nozzle unit 11 is moved to a predetermined position, but also the operation of rotating the nozzle unit 11 during the operation of discharging the liquid from the nozzle 31 is possible. In the present embodiment, the nozzle moving mechanism 33 is configured by the nozzle unit 11, the rail 13, the rail 15, and the rail 32. A known linear motion mechanism such as a linear motor or a rack and pinion can be used as the drive source for the nozzle unit 11, the drive source for the rail 13, and the drive source for the nozzle 31.

  The reagent stage 17 is configured so that a maximum of eight reagent bottles 37 can be placed. A reagent is contained in the reagent bottle 37. Note that the reagent stage 17 of the present embodiment is configured such that two of the eight reagent bottles 37 can be heated.

  A sample container 39 is disposed on the sample stage 19. The sample stage 19 of the present embodiment has one row of 10 sample container holes (not shown) in which 10 sample containers 39 can be arranged at the maximum. Inside the sample container 39, a sample solution (sample solution) obtained by decomposing a sample to be measured into powder using a high concentration mixed acid is preliminarily contained. The sample stage 19 is disposed above the liquid recovery stage 25 via two vertical plates 24.

  A large number of replacement pipette tips 29 are arranged in the pipette tip rack 21. The column stage 23 is provided with a column for dispensing liquid from a pipette tip 29 attached to the tip of the nozzle body 27. FIG. 1 shows a state where the column 43 (see FIG. 2) is not arranged on the column stage 23. The column stage 23 of the present embodiment has one row of ten column insertion holes 45 in which ten columns 43 can be arranged. The column stage 23 is formed integrally with the sample stage 19 and is disposed above the liquid recovery stage 25. The column stage 23 is configured such that the row of sample container holes and the row of column insertion holes 45 are parallel. As will be described later, the ten column insertion holes 45 are aligned with the collection container 47 of the liquid collection stage 25 in the vertical direction. In the present embodiment, the sample stage 19 and the column stage 23 are integrally formed, but it goes without saying that they may be configured as separate stages.

  FIG. 2 is a diagram showing the outer shape of the column 43 used in the present embodiment. The column 43 used in the present embodiment includes a cylindrical portion 43a having an opening into which the pipette tip 29 of the nozzle 31 is inserted, and a small-diameter cylindrical shape having a diameter smaller than that of the cylindrical portion 43a and filled with an ion exchange resin. A portion 43b, and a tapered tubular portion 43c positioned between the tubular portion 43a and the small-diameter tubular portion 43b.

  In the liquid recovery stage 25, 30 recovery containers 47 for recovering the liquids respectively passing through the ten columns 43 installed on the column stage 23 are arranged in three rows. The column stage 23 and the liquid recovery stage 25 are configured such that one recovery container 47 is positioned under one column 43. The liquid recovery stage 25 may be provided with a waste liquid tank that collects waste liquid that becomes unnecessary and is not recovered. In the present embodiment, the liquid recovery stage 25 recovers the liquid that has passed through the column 43 to the recovery containers 47 arranged in three rows, and facilitates the operation of recovering and exchanging the recovered recovery containers 47. In addition, it is configured to be slidable in the Y-axis direction.

  Further, the liquid recovery stage 25 of the present embodiment further moves in the Z-axis direction so that the tip of the column 43 can be inserted into the recovery container 47 in order to reliably recover the liquid that has passed through the column 43 into the recovery container 47. It is configured to be possible. When inserting the tip of the column 43 into the recovery container 47, the liquid recovery stage 25 is displaced to the upper position in the Z-axis direction, and when recovering the recovery container 47, the liquid recovery stage 25 is moved in the Z-axis direction. Displace to the lower position. Since the configuration for moving the liquid recovery stage 25 in the Y-axis direction and the Z-axis direction can adopt a known configuration regardless of the gist of the present invention, description thereof will be omitted.

  FIG. 3 is a diagram illustrating an example of a display image displayed on the display unit D of the controller 3. This display part D is comprised by the liquid crystal touch panel, and selection is performed by touching the inside of the button frame on a display part. A numerical value is set using a numeric keypad (not shown) after selection. In the present embodiment, the case of setting for the first process is shown. As shown in the left column of FIG. 3, in the suction side process, the setting on the suction side is selected by touching the inside of the “suction side” button frame. The number “1” below the “sample container” button frame indicates that the reagent bottle is selected as the first bottle. The following items can be set.

  “Selection of container”: A reagent bottle 37 for sucking a reagent from the pipette tip 29 of the nozzle 31 or a sample container 39 for sucking a sample solution is selected.

  “Dispensing amount”: the total amount of the target liquid (sample solution, reagent) injected into the column 43 in one process.

  “Suction speed”: the speed at which the pipette tip 29 sucks liquid from the reagent bottle 37 or the sample container 39.

  “Suction height”: the distance from the bottom of the sample container 39 to the tip of the pipette tip 29 during suction.

  “Agitation amount” of agitation before aspiration: Aspiration and discharge amount during agitation by sucking (repeating suction and discharge).

  “Agitation speed” of agitation before suction: the suction discharge speed during agitation by sucking.

  “Number of agitation” of agitation before suction: Number of times of sucking.

  Further, as shown in the right column of FIG. 3, the following items can be set in the discharge-side process.

  “Selection of container”: Selection of waste tank, collection container row or sample container. When the column of the waste liquid tank or the collection container is selected, the column of the waste liquid tank or the collection container is arranged under the column, and the liquid sucked into the column is discharged. When the sample container is selected, the liquid sucked into the sample container is discharged.

“Discharge rate”: average dispensing speed of the total amount of target liquid (sample solution, reagent) injected into the column 43 in one process “split dispensing amount”: dispensing per one discharge operation from the pipette tip 29 amount.

  “Discharge height”: distance between the tip of the pipette tip 29 and the ion exchange resin in the column 43 (height of the tip of the pipette tip 29 from the resin surface in the column). Alternatively, the distance between the tip of the pipette tip 29 and the bottom of the sample container 39.

  “Discharge position”: the position of the tip of the pipette tip 29 that is laterally offset from the center position of the column 43.

  “Tip change”: Whether or not the pipette tip is changed for each dispensing operation.

  “Column height”: the depth at which the tip of the column 43 is inserted into the collection container 47 or the like.

  In carrying out the present invention, it is only necessary to set at least the discharge speed, the dispensing amount, and the distance from the center position of the column, but it is needless to say that other items may be set. Therefore, it goes without saying that the controller may be configured so that items other than those described above can be set.

  FIG. 4 is a block diagram illustrating a main part of the configuration of the command generation device 50 in which the components are arranged separately in the controller 3 and the control unit 5 of the automatic analysis preprocessing apparatus 1 of the present embodiment. The command generator 50 includes at least a discharge speed setting unit 51, a dispensing amount setting unit 53, and a distance setting unit 55 in the controller 3. Although not shown in FIG. 4, a similar setting unit is configured for all the setting items. The control unit 5 includes at least a dispensing command generation unit 57 and a movement command generation unit 59. In the present embodiment, the discharge speed setting unit 51 outputs a command for instructing the “discharge speed” shown in FIG. 3 to the dispensing command generation unit 57 and the movement command generation unit 59. The dispensing amount setting unit 53 outputs a command for instructing the “dispensing amount” shown in FIG. 3 to the dispensing command generation unit 57 and the movement command generation unit 59. The distance setting unit 55 outputs a command for instructing the “discharge position” in FIG. The dispensing command generation unit 57 generates a dispensing command based on the discharge speed commanded from the discharge speed setting unit 51 and the dispensing volume commanded from the dispensing volume setting unit 53. Specifically, the liquid dispensing device 35 drives a pump (not shown) so as to discharge the dispensed amount of liquid commanded from the dispensed volume setting unit 53 at the discharge speed commanded from the discharge speed setting unit 51. To do. In addition, when the dispensing volume set by the controller 3 is large, the set dispensing volume exceeds the volume that can be sucked by the pipette tip, and the set dispensing volume cannot be dispensed by one dispensing operation. There is. In addition, when the set dispensing volume is large, if the dispensing volume set in one operation is dispensed, the discharge speed becomes too fast, causing the steady state of the resin in the container to be dispensed. May be. Therefore, the dispensing command generation unit 57 of the present embodiment reduces the dispensing amount to be dispensed by one dispensing operation when the dispensing amount commanded from the dispensing amount setting unit 53 is large. A dispensing command for dispensing a plurality of times may be generated. In this case, the dispensing operation may be repeated by the number of times obtained by dividing the commanded dispensing amount by the divided dispensing amount to be discharged in one dispensing. For example, when the dispensing amount is 7000 μl and the divided dispensing amount is set to 200 μl, the number of divided dispensings is 35. A liquid dispensing device 35 provided in the nozzle unit 11 discharges a dispensing amount or a divided dispensing amount of liquid from a pipette tip 29 attached to the tip of the nozzle at a discharge speed determined in accordance with a dispensing command. A pump (not shown) is driven.

  The movement command generation unit 59 is based on the discharge speed commanded from the discharge speed setting unit 51, the dispensed volume commanded from the dispensing volume setting unit 53, and the distance (discharge position) commanded from the distance setting unit 55. Generate a movement command. Specifically, the movement command generating unit 59 generates a first movement command for moving the nozzle from the center of the container to be discharged by the distance set by the distance setting unit 55 (the radius R of the orbiting operation). . In particular, when the container to be discharged is a column as shown in FIG. 2, (the inner diameter of the cylindrical portion 43a−the outer diameter of the pipette tip)> the set distance> the outer diameter of the small-diameter cylindrical portion 43b. When the numerical value of “discharge position” is set to, the liquid is discharged onto the inner peripheral wall of the tapered cylindrical portion 43 c of the column 43. Further, the movement command generation unit 59 of the present embodiment is a nozzle required to prevent the liquid ejected from the nozzle from rebounding while the nozzle 31 circulates along the inner peripheral wall of the column 43. The second movement command for instructing the position and the movement speed (circulation speed of the nozzle) is output to the nozzle movement mechanism 33 following the first movement command. In the present embodiment, the position of the nozzle is determined by the set values of “discharge height” and “discharge position” shown in FIG. The moving speed (circulation speed) is determined based on the discharge speed set by the discharge speed setting unit 51, the dispensing amount commanded from the dispensing amount setting unit 53, and the distance commanded from the distance setting unit 55 (discharge position). Is done. As a specific example, assuming that the set nozzle discharge speed is V, the set dispensing amount or divided dispensing amount is L, and the set distance is R, the moving speed = 2πR · (V / L). it can. Then, the movement command generation unit 59 is a second movement command for rotating the nozzle along the inner peripheral wall without contacting the inner peripheral wall of the column 43 when the nozzle 31 (pipette tip 29) discharges the liquid. Is output to the nozzle moving mechanism 33. In the controller 3 shown in FIG. 3, when “0” is set as the “ejection position”, the nozzle moving mechanism 33 fixes the nozzle 31 to the center of the column 43 without rotating. The movement command generator 59 generates the second movement command so as to synchronize with the dispensing command. Therefore, when the dispensing command generating unit 57 has generated a dispensing command that dispenses a column multiple times, the movement command generating unit 59 has the same movement command as many times as the number of divided dispensings. Is generated. The command generation device 50 used in the present embodiment generates various commands necessary for performing other operations necessary for pre-analysis processing such as replacement of the pipette tip 29 and suction of liquid by the pipette tip. Can do.

  FIG. 5 is a flowchart showing an operation flow when performing the pre-analysis process using the automatic analysis pre-processing apparatus of the present embodiment. In the example of FIG. 5, teaching is first performed in step ST1. Teaching refers to the position information about the positions of the column 43, the pipette tip 29 in the pipette tip rack 21, the reagent bottle 37, the sample container 39, and the recovery container 47 previously arranged in the apparatus main body 7 in FIG. This is an operation for storing in the memory unit 33. Teaching is also performed on the position of each recovery container or waste liquid tank of the liquid recovery stage 25. Next, the setting items displayed on the display unit of the controller 3 are set (step ST2). Next, the liquid recovery stage 25 is moved in the Y-axis direction and the Z-axis direction according to the contents set in “Discharge side container selection” and “Column height” (step ST3). When the movement of the liquid recovery stage 25 is completed, the nozzle unit 11 is moved onto the pipette tip rack 21, and the pipette tip 29 is attached to the tip of the nozzle body 27 (step ST4). The nozzle unit 11 equipped with the pipette tip 29 moves immediately above the container selected in “Selection of container”, and inserts the tip of the pipette tip into the liquid in the selected container. The pipette tip is inserted at the center of the selected container up to the height set in “aspiration height” when the sample container is selected, and below the reagent liquid level when the reagent bottle is selected (step ST5). In addition, if the stirring of the solution before suction is specified by “Agitating amount before stirring”, “Agitating speed before suction” and “Agitating speed before suction” and “Number of stirring before suction”, the liquid is stirred before suction. . The pipette tip 29 inserted into the liquid in the container aspirates the amount of liquid (sample solution or reagent etc.) set in the “split dispensing amount” (step ST6). When the pipette tip 29 sucks the liquid, the nozzle unit 11 moves immediately above the column 43, or when “sample container” is selected in “discharge side container selection”. Here, when a value other than “sample container” is selected in “Discharge side container selection” and a value other than 0 is set in “Discharge position”, the value is set to the outside of the set value from the center of the column 43. The nozzle 31 is moved to the shifted position. When 0 is set in the “ejection position”, the nozzle is moved to the center of the column or sample container. Then, the tip of the pipette tip 29 is inserted into the selected column or sample container up to the height set in “Discharge height” (step ST7). The height set in “Discharge height” can be appropriately set according to the shape of the column or sample container to be selected, the substance contained in the selected column or sample container, and the nature of the liquid to be discharged. For example, as shown in FIG. 6A, when a sample solution is discharged, a position as close as possible to the ion exchange resin, that is, a discharge height, so that all of the discharged sample solution is introduced into the ion exchange resin. Set the position as low as possible. As shown in FIG. 6B, when the reagent is discharged, the sample solution adhered to the tapered cylindrical portion 43c due to the sample solution rebounding when the sample solution is introduced into the ion exchange resin. Is discharged so as to be discharged onto the inner peripheral wall of the tapered cylindrical portion 43c away from the ion exchange resin so that it can be washed away with a reagent and introduced into the ion exchange resin. By discharging onto the inner peripheral wall on the tapered cylindrical portion 43c, the droplet from the pipette tip 29 does not hit the ion exchange resin and the surface of the ion exchange resin is not disturbed.

  From the pipette tip 29 inserted in the container, the sucked liquid is discharged at the discharge speed set by the discharge speed setting unit 51. When a value other than “sample container” is selected in “Discharge side container selection” and a value other than 0 is set in “Discharge position”, the numerical value set in “Discharge position” as shown in FIG. The liquid is discharged while the nozzle 31 rotates along the peripheral wall of the column 43 so as to draw a circle having a radius R from the center (step ST8). When the discharge of the liquid is completed and “tip exchange” is set to “present” in the display unit D of FIG. 3, the pipette tip is moved to a pipette tip OFF position (not shown) to remove the tip ( Step ST9). Note that when “chip replacement” is set to “none”, the chip is not replaced. If the pre-analysis process has not ended, step ST3 to step ST9 are repeated to perform the next step. Further, the contents set in the setting item may be changed during the pre-analysis process. Moreover, you may perform the setting of the setting item about a process of multiple times collectively.

  In the above description, the sample solution is poured into the column as an example. However, when a reagent is poured into the column, the same procedure as described above may be used. Of course, the sample solution injection and the reagent injection may be performed continuously.

  In this embodiment, as the column, a cylindrical portion having an opening, a small diameter cylindrical portion filled with an ion exchange resin, and a tapered cylindrical shape located between the cylindrical portion and the small diameter cylindrical portion. However, the shape of the column used in the present invention is not limited to the shape of the column used in the above examples.

  According to the present invention, a movement command and a dispensing command necessary for dispensing a predetermined amount of liquid into the column while rotating around the inner circumferential wall of the column without contacting the nozzle with the inner circumferential wall of the column. Occurs in synchronization. Therefore, since the nozzle does not contact the inner peripheral wall of the column, the nozzle is not contaminated by the substance attached to the inner peripheral wall of the column. Further, since the liquid can be discharged while moving the nozzle so as to circulate along the inner peripheral wall of the column, the liquid is not concentrated and injected into a specific portion in the column. Therefore, the steady state of the ion exchange resin enclosed by the reagent excavating a part of the ion exchange resin is not disturbed. Moreover, since it can prevent that the speed | rate of the reagent which passes the inside of an ion exchange resin becomes high, a reagent can fully be made to react within an ion exchange resin. Therefore, a good analysis result can be obtained.

DESCRIPTION OF SYMBOLS 1 Automatic analysis pretreatment apparatus 3 Controller 5 Control part 7 Apparatus main body 11 Nozzle unit 13 Rail 15 Rail 17 Reagent stage 19 Sample stage 21 Pipette tip rack 23 Column stage 24 Vertical plate 25 Liquid recovery stage 27 Nozzle main body 29 Pipette tip 31 Nozzle 32 Rail 33 Nozzle moving mechanism 35 Liquid dispensing device 37 Reagent bottle 39 Sample container 43 Column 45 Column insertion hole 47 Recovery container 50 Command generating device 51 Discharge speed setting unit 53 Dispensing amount setting unit 55 Distance setting unit 57 Dispensing command generating unit 59 Movement command generator

Claims (6)

A nozzle, a nozzle moving mechanism that moves the nozzle in the X, Y, and Z directions according to a movement command; and a liquid dispensing device that discharges a predetermined amount of liquid from the nozzle at a discharge speed determined according to the dispensing command. Dispensing stage,
A column stage comprising one or more columns into which the liquid is dispensed from the nozzle;
An automatic analysis pre-processing device comprising a command generator for generating the movement command and the dispensing command,
The command generation device is configured to move the nozzle along the inner peripheral wall without contacting the inner peripheral wall of the column, and to move the predetermined amount of liquid into the column. And an automatic analysis pretreatment apparatus, wherein the dispensing commands are generated in synchronization.   The command generator commands the position and moving speed of the nozzle necessary to prevent the liquid ejected from the nozzle from rebounding while the nozzle circulates along the inner peripheral wall. The automatic analysis preprocessing device according to claim 1, wherein the movement command and the dispensing command for commanding the discharge speed are generated in synchronization. The column includes a cylindrical part having an opening into which the nozzle is inserted, a small-diameter cylindrical part having a smaller diameter than the cylindrical part and filled with an ion exchange resin, the cylindrical part, and the small-diameter cylinder. A tapered cylindrical portion located between the two, and
The pre-automatic analysis according to claim 1, wherein the command generation device generates the movement command so that the liquid discharged from the nozzle discharges the liquid onto an inner peripheral wall of the tapered cylindrical portion. Processing equipment. The nozzle is composed of a nozzle body and a pipette tip attached to the tip of the nozzle body.
The automatic analysis pretreatment device according to claim 1, wherein the pipette tip is replaceable. The nozzle is composed of a nozzle body and a pipette tip attached to the tip of the nozzle body.
The pipette tip is replaceable,
The command generator is
A discharge rate setting unit for commanding a discharge rate from the pipette tip;
A dispensing volume setting unit for commanding a dispensing volume from the pipette tip;
A dispensing command generating unit that generates the dispensing command based on the set discharge speed and the dispensing amount;
A distance setting unit that commands a distance from the center position of the column;
A movement command generation unit that determines the movement speed of the nozzle based on the set discharge speed, the dispensing amount, and the distance and generates the movement command in synchronization with the dispensing command. The automatic analysis pretreatment apparatus according to 2.   The automatic analyzer provided with the automatic analysis pre-processing apparatus as described in any one of Claims 1-5.

Images