JP3024375B2 - Automatic pretreatment device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic pretreatment apparatus, and more particularly, to an automatic pretreatment apparatus capable of automatically performing pretreatments in analytical operations such as dissolution, extraction, filtration, dilution, and reagent reaction of a sample liquid. The present invention relates to an automatic pretreatment device capable of automatically performing a constant volume operation on a volumetric flask.

[0002]

2. Description of the Related Art Dissolution, extraction, filtration, dilution,
Pre-processing work for analysis work such as reagent reaction and preparation of standard solution is extremely troublesome work requiring precision and great effort, and when these are performed manually, enormous processing time is required. In addition to the necessity, various inconveniences such as a processing error and sample contamination may occur. For this reason,
There is a need for an automatic pre-processing device that automatically performs these operations. For example, an apparatus described in Japanese Patent Application Laid-Open No. 1-200711 by the present applicant has been proposed.

[0003] However, in the apparatus proposed above, the accuracy of the constant volume operation for injecting while measuring the amount of the solution according to the set value was insufficient.

[0004] Generally, in the analysis work such as a standard test, the dissolution volume of a sample solution is set by a constant volume operation using a measuring flask. When these operations are performed manually, the operator visually and manually observes the marked line circumferentially printed on the cylindrical capillary portion of the volumetric flask and the center of the lower meniscus of the liquid level of the injection solution. The goal is achieved by matching hands. These workloads are large, and there were some difficulties in performing the same operation fully automatically, and it could not be easily realized.

When the constant volume operation is performed automatically, the liquid level of the solution to be injected into the volumetric flask and the mark are detected, and a detecting means for judging the coincidence is provided. Control means for the injection of the solution to be stopped are required.
The detection means needs to have a function of eliminating characteristics such as the transparency of the sample solution, the size and damage of the volumetric flask, and the effects of water droplets attached to the wall surface of the volumetric flask. In addition, in the control means, when the constant volume point is reached, the injection operation is immediately stopped, the flow of the residual liquid into the volumetric flask tube is suppressed, and the constant volume point is set to more accurately perform the constant volume operation. Before reaching the temperature, it is necessary to adjust the solution injection speed, and a washing process for washing away the sample powder attached to the tube is also required.

As a method that can be applied to the detection of the liquid level of a liquid injected into a measuring flask, there are known techniques, for example, JP-A-61-149825 (Abbott) and JP-A-63-149825. 154917 (filed by Murako Medical Co., Ltd.) or JP-A-60-200126 (filed by Suntory Ltd.).

[0007]

SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for quickly and extremely accurately charging a liquid up to the marked line of a volumetric flask, in addition to a pretreatment operation for ordinary analytical work, An object of the present invention is to provide an automatic pretreatment device capable of easily performing a constant volume operation on a flask.

[0008]

SUMMARY OF THE INVENTION According to the present invention, an object of the present invention is to provide a turntable means on which a plurality of containers including a volumetric flask can be placed, and a stationary position which is separate from the turntable means. The rack means on which the plurality of containers can be placed, and a predetermined amount of liquid are sampled and discharged into a volumetric flask placed on the turntable means, and the level is lowered to a level below the marked line of the volumetric flask. A probe means for injecting the sampled liquid, separately sampling one of the liquid and the dilution, and discharging the liquid and the dilution to the volumetric flask so as to inject one of the liquid and the diluent up to the marked line of the volumetric flask, Along with the rack means, it is possible to place a volumetric flask into which the liquid has been injected to a level below the mark, and
A mounting means movable in the vertical direction, a light source which is arranged on one side of the mounting means, has a substantially uniform brightness in a vertical band, and is arranged on the other side of the mounting means. Supporting means for supporting the supporting portion movably in the vertical direction, and the supporting portion for receiving light from a light source transmitted through a volumetric flask mounted on the mounting means and outputting a video signal. And a video signal output from the sensor means when one of the separately sampled liquid and diluent is being discharged from the probe means into the volumetric flask placed above. Detecting means for detecting coincidence between the marked line of the volumetric flask and one of the liquid levels of the liquid and the diluent injected into the volumetric flask, and outputting a coincidence detection signal; and container Robot means configured to be able to transfer the probe means between the turntable means, the rack means and the mounting means, and a transfer operation of the robot means, and a vertical movement of the mounting means. Controls the operation, the vertical movement of the support part, and the sampling and discharging operations of the probe means, and responds to the coincidence detection signal from the detection means in response to the coincidence detection signal from the detection means. Control means for controlling the operation of the probe means so as to stop one of the discharges.

The probe means may include a probe needle capable of inserting a tip into each of the containers, and a micro syringe pump for sucking and discharging a predetermined amount of liquid through the probe needle. More desirable.

Further, it is more preferable that the probe needle has a plurality of fine holes at its tip end, on the inner wall surface of the inserted container, for discharging the liquid almost uniformly in a shower shape.

Further, a three-way switching valve capable of switching the liquid flowing from a single inlet into one of the two outlets and allowing the liquid to flow out is provided on the discharge side of the probe means, and the sampled liquid is It is more desirable that the three-way switching valve be switched to control the discharge of the liquid and the stop of the discharge when the discharge into the volumetric flask and the stop of the discharge.
Further, an image sensor using a one-dimensional CCD camera is employed as the sensor means, and the detection means converts a video signal output from the sensor means into a digital signal by binarizing the video signal. A circuit for generating a falling pulse, and a signal processing means having a first-in first-out memory circuit, a pulse width extraction circuit, a storage circuit for storing a mark width and a liquid level defined between the top and bottom of the liquid level meniscus, And a calculation means including a movement determination circuit.

Further, the control means moves the placing means up and down to a predetermined position in accordance with the volume of the volumetric flask into which the liquid has been injected to a level below the marked line, thereby positioning the placing means. It is more desirable to configure to control

Further, the control means moves the support means attached to the support part to a predetermined position in accordance with the volume of the volumetric flask into which the liquid has been injected to a level below the mark. It is more desirable that the positioning means be moved up and down to control the positioning operation of the support means.

Further, Vo is placed in a stationary position separate from the turntable means, the rack means, and the placing means.
It is more desirable to provide a stirring means employing a rtex mixer and to configure the robot means so that each container can be transferred between the stirring means and the turntable means, the rack means, and the placing means described above. .

[0015]

In the automatic pretreatment apparatus according to the present invention, the sensor means is attached to the supporting portion so as to receive the light from the light source transmitted through the measuring flask mounted on the mounting means and output a video signal. And detecting means, when the separately sampled liquid is being discharged from the probe means into the measuring flask placed above, based on the video signal output from the sensor means, Detects coincidence with the concave bottom formed on the liquid surface of the liquid injected into the volumetric flask, outputs a coincidence detection signal,
Since the control means controls the probe means to stop discharging the sampled liquid from the probe means in response to the coincidence detection signal from the detection means, the automatic pretreatment device of the present invention It can be injected quickly and very accurately up to the marked line of the volumetric flask.

Further, in the automatic pretreatment apparatus of the present invention, a vertically movable mounting means is provided near the rack means, and the liquid is injected to a level below the marked line of the measuring flask. A light source having a substantially uniform brightness in a band shape in the vertical direction is arranged on one side with respect to the mounting means, and the sensor means is attached and the support portion is moved in the vertical direction. Freely supporting support means is disposed on the other side with respect to the mounting means;
The robot means is configured to be able to transfer each container including the volumetric flask and the probe means to and from the turntable means, the rack means, and the mounting means, respectively. Since the vertical movement of the means and the vertical movement of the support means are controlled, the sensor means can be quickly positioned with respect to the marked lines of the measuring flasks of various sizes. Can easily perform a constant volume operation.

[0017]

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a block diagram of an automatic pretreatment apparatus according to the present invention.

FIG. 1 is a perspective view schematically showing the structure of an embodiment of the present invention, FIG. 2 is a plan view of the same, and FIG. 3 is a partial cross-sectional view of FIG.

The apparatus of this embodiment mainly includes a turntable means 10, a rack means 11, a probe means 12, a robot means 13, a filter robot means 14, and a liquid level measuring means 7.
0 and control means for controlling them (not shown in FIG. 1)
have.

As shown in FIGS. 1 and 2, the liquid level measuring means 70 is provided close to the rack means 11, and is provided with a mounting means 7 on which a measuring flask is mounted and which can be moved vertically.
2 and one side of the mounting means 72,
A light source 71 having a substantially uniform luminance in a band shape in the vertical direction,
A supporting means 74 disposed on the other side of the mounting means 72 for supporting the supporting portion movably in the vertical direction; and a light from the light source 71 transmitted through the measuring flask mounted on the mounting means 72. A sensor unit 73 attached to the support unit for receiving a video signal and outputting a video signal; and a signal processing unit (not shown in FIGS. 1 and 2) for processing the video signal output from the sensor unit 73. It is constituted by a detecting means including an arithmetic unit for detecting a liquid level waveform or the like.

The liquid level measuring means 70 includes a mounting means 7.
Vortex as stirring means provided adjacent to
mixer 90 is also included.

FIG. 4 shows a schematic configuration for detecting the marked line of the measuring flask and the liquid level of the injected solution in the apparatus according to one embodiment of the present invention. FIG. 5 is an explanatory diagram of a liquid level detecting operation of the apparatus according to one embodiment of the present invention.

In FIGS. 4 and 5, reference numeral 72a denotes a measuring flask, which is provided with a mark 72b which is a mark indicating a set amount to be injected. 72d is an injection nozzle, and 72c is a liquid level. A light source 71 is arranged on one side of the measuring flask 72a, and a one-dimensional CCD camera 73 is arranged on the other side in opposition to the light source 71. In this embodiment, a 1024-bit image sensor is used for a one-dimensional CCD camera. A waveform 73a is a waveform output from the image sensor according to the brightness of each bit. The signal is output at the L level when the image is bright and at the H level when the image is dark. Mark 7
Since the light 2b and the liquid surface 72c block light, the waveform 73a is observed as waveforms 73b and 73c, respectively. 73e is a waveform obtained by binarizing the waveform 73a at a certain slice level 73d. In the waveform 73e, a waveform 73g is obtained by binarizing a waveform based on a liquid level, and a waveform 73f is obtained by binarizing a waveform based on a reference line. It is a thing.

The values of the widths of the rising and falling times of each of the waveforms 73f and 73g are written in a first-in first-out memory, and the width of the waveform is measured by a pulse width determination circuit of an arithmetic unit. And the position of the liquid level are recognized. The liquid is injected from the injection device (not shown) into the injection nozzle 72.
As the liquid is injected through d, the liquid level 72c rises and approaches the mark 72b, but the first-in first-out memory is used to record the time-varying state at high speed.

Therefore, the position of the liquid surface is recognized by continuously measuring the waveform widths of the above-mentioned waveforms 73f and 73g, so that the injection stop signal is generated at an appropriate time before the liquid surface reaches the mark position. By outputting, it becomes possible to make the injection amount exactly constant. As an example for realizing this operation, L-SER / MODEL, WL manufactured by Koden Kogyo Co., Ltd.
D-3 can be used.

FIG. 6 is an explanatory diagram showing the inflow path of the solution in the liquid level measuring means of this embodiment. A solution bottle 80,
A syringe pump 79 for sucking a liquid from the solution bottle 80 and discharging the liquid to the other side, and a three-way discharging the liquid discharged from the syringe pump to one of two outlets according to a control signal by switching a valve to one of two outlets. A switching valve 78, a probe needle 77 connected to one output side of the three-way switching valve 78, and a level below a marked line in which the tip of the probe needle 77 is inserted and which is attached to the cylindrical thin tube portion. Flask 7 into which the solution has already been injected
There is a discharge bottle 81 connected to the other output side of the two-way and three-way switching valve 78. At the tip of the probe needle 77, a plurality of pores are provided on the inner wall surface of the inserted container to discharge the liquid almost uniformly in a shower shape.

FIG. 7 is a diagram showing a schematic configuration of a signal processing section and an arithmetic section for detecting the liquid level of the liquid level measuring means and the reference line in the present embodiment. CCD as sensor means
A signal processing unit 75 to which a video signal output from the camera 73 is input is provided with a signal processing binarization circuit for binarizing the video signal at a certain slice level, and a rising and falling position based on binarized waveform data. , A rising and falling pulse generation circuit that generates a pulse by detecting the pulse data, a first-in first-out memory that stores the pulse data at high speed as time passes, a clock circuit and a counter that generates signal processing timing, and the like. The arithmetic unit 76 receives the pulse data from the first-in first-out memory of the signal processing unit 75 in the order of storage, extracts a pulse width from the pulse data, a pulse position detection circuit that detects a pulse position, A mark width liquid level width storage circuit for storing a pulse width of the mark, a liquid level pulse judgment circuit for judging whether or not the pulse corresponds to the liquid level, a movement judgment circuit for judging the movement of the liquid level, a mark And a water level determination circuit for determining that the concave bottom of the liquid surface has risen to the mark line.

The turntable means 10 is provided with a turntable 15 on which a plurality of container housings (four in this embodiment) are provided. As clearly shown in FIG. 2, a plurality of (32 in this embodiment) containers (for example, containers 16) for the filtrate are stored in the outermost row (filtration row) of the container storage sections 16.
a) is placed, and a plurality (32 in this embodiment) of containers (for example, containers 17a) for liquids being processed are placed in the container storage section 17 in the second row (transfer row) from the outermost periphery. It is configured to be. Further, a plurality (eight in this embodiment) of sample flasks or sample containers 18a for sample liquid are placed in the container storage portions 18 in the third row (sample row) from the outermost circumference, and the innermost row (Dilution column)
A plurality of containers for dilution (8 in this embodiment)
) (For example, the container 19a). Note that FIG. 1 shows only a part of the container storage part and the container for easy understanding, and many of them are omitted.

Containers 16a respectively placed in the container storage section 16 of the filtration row and the container storage section 17 of the transfer row
And 17a have a maximum capacity of about 20 ml, but the volume of the volumetric flask or the sample container 18a placed in the container storage section 18 of the sample row can be set to a maximum of about 150 ml. In addition, the diluent container storage unit 19
The capacity of the container 19a placed in the container 19a can be about 50 ml at the maximum. The number of containers that can be placed in the container storage units in each row is not limited to the number described above, and may be any number.

As shown in FIG. 3, the turntable 15 is mounted on a rotating shaft 20 and is configured to be rotated together with the rotating shaft 20 in a horizontal plane so that the turntable 15 can be accurately stopped at a desired position. . The rotation of the rotating shaft 20 is performed by rotating a driving disk 21 provided below the rotating shaft 20 with an electric motor 22. In this embodiment, the rubber ring 21 a provided on the outer periphery of the driving disk 21 is driven to rotate by the roller 22 a of the electric motor 22. In addition to the combination of the rubber ring and the roller, a combination of a gear and a belt drive may be used. Electric motor 2
When a normal AC motor is used as 2, in order to control the position of the turntable 15, a position mark disk 23 fixed to the rotating shaft 20 is detected by an optical sensor 24 and feedback control is performed. Electric motor 22
If a step motor is used, the sensor 24 can be omitted.

The rack means 11 is provided stationary at a predetermined position different from that of the turntable 15, and is configured to accommodate a large number of measuring flasks or sample containers. The rack means 11 is configured so as to be removable from the apparatus and transportable. For this reason, when a series of processes is completed, a large number of measuring flasks or sample containers can be replaced at the same time. In FIG. 1, only a part of the container storage part and the container are shown for easy understanding, and many of them are omitted.

The probe means 12, as shown in FIG.
For example, a probe needle 26 for sampling and injecting a predetermined amount of a sample solution, dilution water and the like in a container 25 and a micro syringe pump (diluter) 2 connected to the probe needle 26 via a three-way switching valve 7.
8 is provided. The syringe pump 28 is a known one, and performs suction and discharge of a predetermined amount of liquid. A dilution water tank 29 is further connected to the three-way switching valve 27.

As shown in FIGS. 1 and 3, in this embodiment, for example, four types of probe needles 26a, 26b, 26c, and 26d having different needle portions are prepared. One is configured to be used selectively. Which probe needle is selected depends on the liquid properties of the sample solution. When used for injection into a chromatography system described later, a probe needle having a small diameter is selected. The probe needles 26a, 26b, 26c and 26d are connected to the small syringe pumps 28a and 28b and the large syringe pump 28c via a flexible pipe and a switching valve (not shown). The selection of the probe needles 26a, 26b, 26c, and 26d and the movement in the horizontal and vertical directions are performed by being gripped by the robot means 13 as described later.

When a constant volume operation is performed on the volumetric flask, the probe needle is used to discharge the liquid to the inner wall surface of the volumetric flask almost uniformly in a shower shape.
A plurality of pores are provided at the tip.

The robot means 13, as shown in FIG.
By gripping the volumetric flask or sample container 30 with a finger 31 as an attachment, the container is transferred between the container storage section 18 on the turntable 15 and the container storage section on the rack means 11 and the probe needle is moved to a desired horizontal position. It is for moving to the position, up and down position. Further, the robot means 13 is used for selecting one of a plurality of types of filters as described later. In this embodiment, the robot means 13 can precisely control the position of a desired two-dimensional (X-axis, Y-axis) position within the reach of the arm, and can also control the position in the vertical direction (Z-axis direction). A simple horizontal two-joint robot is used. In general, a horizontal two-joint robot has characteristics of high compliance in the horizontal direction and high rigidity in the vertical direction. As the robot means 13, a three-dimensional orthogonal coordinate robot can be used instead of the horizontal two-joint robot.

FIG. 10 is a cross-sectional view of the horizontal two-joint robot. Reference numeral 32 denotes a first arm, and reference numeral 33 denotes a second arm. The first arm 32 includes a support shaft 34 having a motor 35.
, Can be rotated in the horizontal direction. The second arm 33 is rotatably supported by the distal end of the first arm 32, and is rotatable in a horizontal direction around a support shaft 38 by being driven by a motor 37 via a drive system 36 such as a belt. . The entire horizontal two-joint robot is driven vertically by a motor 39. Two chuck members 40a and 40 for chucking a finger for gripping a sample container or a probe needle are provided at the distal end of the second arm 33.
b is detachably attached. These chuck members 40 a and 40 b are configured such that the distance between the chuck members is controlled by driving a motor 41 provided in the second arm 33.

Although not shown, the robot means 13 has an encoder for detecting the rotational position of the motor 35 for the first arm 32 and the rotational position of the motor 37 for the second arm 33. And sensors for detecting the horizontal overrun and the origin of the first arm 32 and the second arm 33, respectively, and sensors for detecting the vertical overrun and the origin of the first arm 32 and the second arm 33, respectively.

FIG. 11 shows an example of a finger which is an attachment for gripping a sample container, and is configured such that tips of chuck members 40a and 40b are inserted into holes 42a and 42b, respectively. Chuck member 4
When driven in the direction in which the distance between 0a and 40b increases and decreases, the members 44a and 44b rotate around the fulcrums 43a and 43b, and the sample container 45 is gripped and released, respectively. FIG. 12 shows an example of a finger which is an attachment for holding the probe needle, and the chuck members 40a and 40a are similar to the case of FIG.
0b is configured to be inserted into holes 46a and 46b, respectively. Chuck members 40a and 40
When driven in the direction in which the distance b is increased and decreased,
Each member 48a and 4 around the fulcrum 47a and 47b
The probe needle rotates by 8 bg, and the probe needle is gripped and released, respectively. Each finger includes chuck members 40a and 40a.
It is placed at a predetermined position 49 (FIG. 2) within the movable range of b, and the chuck members 40a and 40b move as required and are automatically connected.

As shown in FIG. 3, the filter robot means 14 mainly includes a column 14a extending vertically and an arm 14b extending horizontally from the top of the column 14a. The support 14a also serves as a rotation axis, and the rotation of the support 14a causes the arm 14 to rotate.
b also rotates. The support 14a is driven by rotating a drive disk 50 provided below the support 14a with an electric motor (not shown). In this embodiment, the driving disk 50
The rubber ring 50a provided on the outer periphery of the motor is driven to rotate by rollers of an electric motor. In addition to the combination of the rubber ring and the roller, a gear may be combined or a belt and a pulley may be used. When a normal AC motor or DC motor is used as the electric motor, the filter robot means 14
In order to control the rotational position of the optical disc, a position mark disk 51 fixed to the support 14a is detected by an optical sensor and feedback control is performed. If a step motor is used as the electric motor, the sensor can be omitted.

The arm 14b rotates by a predetermined angle in a vertical plane centering on a portion attached to the support 14a, in addition to the rotation in the horizontal plane around the support 14a, and the arm 14b The tip is configured to be able to move up and down. With such a configuration, there is no inconvenience such that the tip (outlet end) of the filter described later is inserted into the inside of the container during the filtering operation, and as a result, a part of the filtered liquid flows out of the container. This pivoting operation of the arm 14b is performed by an air cylinder (not shown) that moves back and forth by pressurized air by applying a rotational moment to the arm 14b.

A filter holding mechanism for detachably holding a disposable filter 52, which is a disposable molded filter, is provided at the tip of the arm 14b.
A sealing mechanism for forming a sealed chamber on the sample liquid injection side of No. 2,
A mechanism for feeding a pressurized gas into the sealed chamber is provided.

The filter holding mechanism is provided on a part of the lower surface of the disposable filter 52 supplied from the filter supply unit 53 (FIG. 1) through an insertion hole 54 provided on the upper surface of the tip of the arm 14b. It is configured to hold this. A holding member 55 connected via a rod to an air cylinder movable in the front-rear direction supports a part of the lower surface of the disposable filter 52. When disposing the disposable filter 52, when the holding member 55 is moved, the disposable filter 52 falls by its own weight.

Regarding the structure of the filter holding mechanism, the sealing mechanism, and the mechanism for sending the pressurized gas into the sealing chamber,
This is described in detail in Japanese Patent Application Laid-Open No. 1-200711 proposed by the present applicant.

The filter robot means 14 includes a sensor for detecting the horizontal rotation position of the arm 14b, a sensor for detecting the vertical rotation position of the arm 14b, and a disposable filter 52. Although not shown, a sensor or the like for detecting whether or not it is held is provided.

The arm part 14 of the filter robot means 14
b can be rotated in the horizontal direction by the rotation of the support portion 14a, but its stop position is set at four positions in this embodiment. One is the processing position (on the X-axis) shown in FIGS. 1 and 2 and is stopped at this position during the filtering process of the sample. In this case, the outlet end of the disposable filter 52 is positioned just above the container housing 16 of the filtration row. Further, it can be stopped at the position of the filter storage magazine 53a of the filter supply unit 53 shown in FIG. In this embodiment, the filter supply unit 53 includes six filter storage magazines 53a to 53f, and each of the filter storage magazines 53a to 53f includes a plurality of different types of unused disposable disposable filters (in the present embodiment, a plurality of disposable disposable filters). 16) can be stored.

When a disposable filter is mounted on the filter robot means 14, first, the filter storage magazine 53
The insertion hole 54 of the arm portion 14b is moved to a position directly below "a". Then, the disposable filter is lowered from the filter storage magazine 53a through the insertion hole 54, and is held by the filter holding mechanism. When another type of disposable filter is mounted, the filter supply unit 53 is rotated to move a desired filter storage magazine to the currently indicated position of the filter storage magazine 53a. This movement of the filter supply unit 53 is performed by the arm of the robot means 13 pushing and rotating the filter supply unit 53.

Still other stop positions of the arm portion 14b include a position of a discharge port 56 for discharging the filtered diluent and a position of a disposal port 57 for discarding the used filter in a multi-stage filtration process described later. (FIGS. 1 and 2).

As shown in FIG. 3, the rotary shaft 20 of the lower part of the turntable 15 and the filter robot
The container storage section 16 of the filtration row, the container storage section 17 of the transfer row, the container storage section 18 of the sample row, and the container storage section of the dilution row, between (with respect to the X axis) the rotating shaft which is the support section 14a of the fourth column Just below 19, the stirrers 58, 59, 6
0 and 61 are arranged respectively. These stirrers 58, 59, 60, and 61 are well-known magnetic stirrers for stirring the sample in the container when the container is in each container storage unit. That is, S and N magnetic poles are provided at the diametrical ends of the upper portions of these stirrers, respectively, and the magnetic poles (stirrers) placed in the container are rotated by rotating the magnetic poles by the electric motor 62 to stir. Is what you do.

The rotary shaft 20 and the support 1 of the filter robot means 14 are located below the turntable 15.
An ultrasonic vibrator 63 is provided immediately below the container housing portion 18 of the sample row on the extension line (on the X-axis line) of the sample line 4a (on the X-axis line), that is, directly below the housing portion of the sample container. Can be

As shown in FIG. 3, the turntable 15 is provided between a container storage section 16 of the filtration row and a container storage section 17 of the transfer row and a container storage section 18 of the sample row and a container storage section 19 of the dilution row. A partition 15a is provided to separate the two. A heating resistance coil 64 is provided between the sample row and the dilution row, and a cooling liquid circulation pipe 65 for cooling is provided on the outer circumference of the outermost filtration row.
Is provided. Since the sample solution and the diluted solution are stored in the container storage section 18 of the sample row and the container storage section 19 of the dilution row, respectively, the extraction efficiency can be improved by heating them (heating). Tank section). Since the filtered solution and the solution being processed are stored in the container storage section 16 of the filtration row and the container storage section 17 of the transfer row, the partition 15a and the partition 15a are so heated that they are not heated together and concentration occurs. A cooling liquid circulation pipe 65 is provided to cool this part (cooling tank part). Since the heating tank section and the cooling tank section are separated from each other as described above, the heating and cooling effects are very high.

The apparatus of this embodiment further comprises reagent stations 66 and 67 (FIGS. 1 and 2)
At a stationary position outside the
(Up to 1000 ml) and large capacity (150 ml) reagent containers 67a to 67c.

The probe needles 26a, 26b,
A cleaning mechanism 68 is provided at the storage positions of 26c and 26d. The cleaning mechanism 68 includes the probe needle 26
a, 26b, 26c, and 26 and the elements communicating therewith are to be cleaned. At least at the time of cleaning, a cleaning liquid is supplied from a cleaning liquid supply and discharge system (not shown).

Further, an automatic six-way switching valve 69, which is an input port for injecting a sample into the liquid chromatography system, is provided. Although the figure shows an example in which only one input port is provided, a plurality of input ports may be provided as needed.

The control means includes a microcomputer in which a sequence relating to desired pre-processing and constant-volume operation is programmed. According to instructions from the microcomputer, the turntable means 10, the probe means 12, the robot means 13. Filter robot means and liquid level measuring means 70 (mounting means 72 and support means 74)
It is configured to control the driving of.

In the constant volume operation, in addition to controlling the transfer operation of the robot means 13 and the sampling operation of the probe means 12, the control means responds to the coincidence detection signal from the detection means of the liquid level measurement means 70 to control the probe. The discharge operation of the probe means is controlled to stop the discharge of the sampled liquid from the means.

FIG. 13 is a block diagram schematically showing an electric configuration of the control means in this embodiment. As is clear from the figure, in this embodiment, the central processing unit (CPU) 1
A microcomputer including a read only memory (ROM) 101, a random access memory (RAM) 102, input / output interfaces 103 and 104, a display device 105, a teaching unit 106, and a bus 107 for connecting these components is used. .

The input / output interface 103 includes a sensor 108 for detecting a horizontal rotation position of the arm portion 14B of the filter robot means 14, a sensor 109 for detecting a vertical rotation position, and a filter robot means. 14, a sensor 110 for detecting whether the filter is held, a horizontal overrun detection sensor 111 for the arm of the robot means 13, a horizontal origin detection sensor 112, a vertical overrun for the arm of the robot means 13, A detection sensor 113 and a vertical origin detection sensor 114 are connected, and a detected information signal is input to the microcomputer. Further connected to the input / output interface 103 are the ultrasonic transducer 63, the three-way switching valve 27 (78), the six-way switching valve 69 of the liquid chromatography system, and the syringe pumps 28a, 28b, and 28c. Controlled. In addition, the encoders 115 and 116 of the robot unit 13 are connected to the input / output interface 103, and the position of the robot unit 13 is controlled.

A control unit 117 for controlling the rotation of the step motor 22 for the turntable 15 is connected to the input / output interface 104, and the position of the turntable 15 is controlled by a microcomputer. The input / output interface 104 further includes a control unit 118 for controlling the rotation of the motor 68 for the agitators 58, 59, 60, and 61, and a control unit 12 for controlling the motor 119 of the cleaning liquid drive pump of the cleaning mechanism 68.
Injection motor 12 for 0, 6-way switching valve 69
1, a control unit 124 for controlling a motor 123 for driving the arm 14b of the filter robot means 14 in the horizontal direction, and a control unit 1 for controlling a motor 125 for driving the arm 14b in the vertical direction.
26, a motor 35 for driving the first arm of the robot means 13, a motor 37 for driving the second arm,
A control unit 127 for controlling a motor 39 for driving in the vertical direction, a motor 41 for chucking the fingers, and a motor 72 for moving the mounting means 72 up and down.
f and a control unit 128 for controlling a motor 74a for vertically moving the support section of the support means 72, and a signal processing section 75 and an arithmetic section 76 constituting detection means are connected. These are controlled.

Next, the operation of this embodiment will be described. FIG. 14 is a flowchart schematically showing an example of a control program of the microcomputer.

When the power is turned on (step S1), C
The PU 100 clears the RAM 102 and other memories (Step S2), and then returns all the driving elements to their home positions (origin positions) (Step S3). this is,
The turntable means 10 is to return the container to be started to the processing position (on the X-axis), the robot means 13 is to position each arm at a predetermined origin, and the filter robot means 14 is ,
This means that the arm 14b is rotated to the position of the filter supply unit 53.

Next, it is determined whether or not the teaching process is to be performed (step S4). If the teaching process is to be performed, a teaching mode routine is to be performed (step S5).
If the teaching process is not performed, the process proceeds to the automatic mode routine (step S6).

The teaching process is for setting an address for the moving position of the robot means 13 and is executed by the teaching unit 106.

As the horizontal teaching process, address setting for the position of the sample container storage section in the rack means 11 will be described first. As shown in FIG. 15, the rack means 11 has sample container storage units arranged in a matrix. The center of the finger attached to the tip of the second arm 33 of the robot means 13 is manually moved to the four corners A, B, C, and D in this matrix arrangement, and the respective addresses are stored in memory. Thus, the address of the center position of each of the remaining sample container storage sections can be obtained by calculation.

As shown in FIG. 16, the teaching processing of the container storage section on the turntable 15 in the horizontal direction is performed at points E and F, which are the container storage sections in each row at the processing position (on the X-axis). , G and H, the tip of the robot means 13 is manually moved to store the respective addresses. Thus, the address of the center position of the container storage section on the turntable 15 can be obtained by calculation.

As a teaching process of the vertical position, as shown in FIG. 17, the second arm 33 of the robot means 13 is placed in the container 130 disposed on the turntable 15 and the container storage section on the reagent stations 66 and 67.
The probe needle attached to the tip of the head is lowered by driving the motor by manual operation, and the addresses in the vertical direction (Z-axis direction) at the suction position I and the discharge position J are stored. This is performed for each type of container.

The automatic mode routine includes (a) a filtration dilution mode in which a sample container is filtered and then diluted,
(b) a dilution filtration mode in which the sample solution is diluted and then filtered, (c) a filtration mode in which only the sample solution is filtered, (d) a multi-stage filtration mode in which the sample solution is multi-stage filtered, (e) Primary dilution mode and secondary dilution mode in which only the sample solution is diluted, (f) Reaction mode for examining the reagent reaction of the sample solution, (G) Dissolution filtration mode in which the sample is dissolved and filtered, (h) Sample solution Injection mode to automatically inject into the input port of the liquid chromatography system,
(i) A mode in which a creamy sample is extracted, filtered, and automatically injected into the input port of the liquid chromatography system. (j) A specified liquid volume for measuring the level of the liquid to be injected into the volumetric flask and charging a fixed amount. Although there are charging modes and the like, a dissolution-extraction-dilution-
The filtration-injection mode will be described.

FIG. 18 is a flow chart showing the flow of the dissolution-extraction-dilution-filtration-injection mode, and FIG. 19 shows the operation sequence.

This mode is used for a tablet purity test, a content uniformity test and the like. First, in step S10,
Sample container 2 in the sample row of turntable 15
At 00, a tablet as a sample is put. Next, in step S11, initial processing of the syringe pump is performed,
In step S12, the origin of the arm of the robot means 13 is checked. In the next step S13, after the arm of the robot means 13 is moved to a predetermined position where the finger is placed and the finger for gripping the probe needle is chucked, A probe needle of a desired system is selected and gripped.

In step S14, the solution is sampled from the extra large volume solution container 202 into the syringe pump. A pipe is directly connected to the solution container 202 from a syringe pump via a three-way switching valve or the like.
The sampled solution is dispensed by a predetermined amount into the sample container 200 in the next step S15. This dispensing is performed by moving the probe needle to the position of the sample container 200 by the robot means 13.

Next, in step S16, the turntable 15 is rotated to position the sample container 200 directly above the stirrer 60, and the sample container 200 is stirred and melted. The position of 200 is positioned right above the ultrasonic transducer 63 and is dispersed by ultrasonic driving. In FIG. 19, reference numeral 200a denotes a stirrer.

After the sample container 200 is sufficiently stopped,
In step S17, the supernatant is sampled via the probe needle. In the next step S18, the probe needle is moved to the position of the dilution container 203 in the dilution row of the turntable 15, and the sampled supernatant is dispensed into the dilution container 203 by a set amount. In step S19, the probe needle is moved to the position of the internal standard solution container 204 stored in the reagent station 67 of the turntable 15, and the internal standard solution is sampled. In the next step S20, the probe needle is moved to the position of the dilution container 203, and the sampled internal standard solution is transferred to the dilution container 20.
Dispense only the set amount into 3. Next, in step S21, after stirring is performed, a set amount of the diluted solution in the dilution container 203 is sampled.

In the next step S22, the probe needle is moved to the position of the filter 205 of the filter robot means 14, and a set amount of the diluted solution sampled is injected into this filter. Note that a desired filter 205 is supplied to the filter robot means 14 in advance from the filter supply unit 53 and set. Further, the filter robot means 14 is rotated so that the filtration vessel 206 of the filtration row of the turntable 15 is located below the filter 205. In step S23, the diluted solution is filtered under pressure and injected into the filtration container 206.

In the next step S24, the filter robot means 14 rotates from the processing position, and the filter vessel 206
The probe needle moves to the position of and samples the filtrate. Further, the probe needle moves to the position of the input port 69a of the switching valve 69 of the liquid chromatography system, and the sampled filtrate is transferred to the input port 6a.
Inject into 9a.

In the next step S25, it is determined whether or not the processing in this mode has been completed for the set number of sample containers stored on the turntable 15 (in this embodiment, a maximum of eight). If the number of processed samples is smaller than the set number, the process returns to step S14 and returns to steps S14 to S14.
The process of S24 is repeated. If the number of processed samples has reached the set number, the process proceeds to step S26, and it is determined whether or not the number of processed samples has reached the total set number to be processed. If the total number has been reached, the processing in this mode is terminated.

If the number of samples to be processed has not reached the total set number, the sample containers on the turntable 15 and new sample containers in the rack means 11 are exchanged. First, in step S27, the arm of the robot means 13 is advanced to a predetermined position where the finger is placed, and the finger for holding the probe needle is replaced with the finger for holding the container. Next, in step S28, the turntable 1
The sample container stored on the container 5 is chucked by a container gripping finger and transferred to a predetermined storage unit in the rack means 11. A predetermined number of sample containers are transferred in the same manner.

In the next step S29, the rack means 11
A new sample container containing the sample set therein is chucked by a container gripping finger and transferred to the container storage section of the sample row on the turntable 15.
Also in this case, a predetermined number of sample containers are transferred in the same manner. Then, the process returns to step S14, and the processes of steps S14 to S24 described above are repeated.

During the processing mode of FIG. 18, the probe needle is cleaned by the cleaning mechanism 68 as needed. Since the cleaning method is known, the description is omitted.

Next, two-stage filtration of the sample solution is performed.
The step filtration mode will be described.

FIG. 20 is a flowchart showing the flow of the two-stage filtration mode. FIG. 21 is a flow chart showing the probe means 12, robot means 13 and filter robot means 14 at that time.
FIG. 22 shows the behavior of the liquid in the probe needle at that time.

In this mode, in order to prevent some of the components in the sample from adsorbing to the filter membrane during filtration, the first filtration liquid is discarded and the second filtration liquid is collected. Is what you do. First, in step S30, the filter robot means 14 is rotated to the position of the filter supply unit 53, and the filter 52 of a desired type is
Is set (the state of FIG. 21A). Next, in step S31, the filter robot means 14 is rotated on the X axis.

In the next step S32, the robot means 1
The probe needle 26 is moved to the position of the filter 52 of the filter robot means 14 by 3 and a set amount of the sampled first-stage diluent is injected into the filter 52 (the state of FIG. 21B). Then, step S3
3 to rotate the filter robot means 14 and
2 is positioned directly above the outlet 56, and under this condition, the solution is filtered under pressure and the filtrate is discharged to the outlet 56 (FIG. 21).
(State of (C)).

Next, in step S34, the filter robot means 14 is rotated so that the filtration vessels of the filtration row of the turntable 15 are positioned on the X axis, that is, directly below the filter 52. In the next step S35, the probe needle 26 is moved to the position of the filter 52 of the filter robot means 14 by the robot means 13, and a set amount of the sampled second-stage diluent is injected into the filter 52, and pressure filtration is performed. Then, the diluent is injected into the filtration container (the state shown in FIG. 21D).

Next, in step S36, the filter robot means 14 is rotated to remove the filter 52 from the disposal port 5.
7 and the filter 52 is placed in this state.
Is dropped and discarded (state of FIG. 21E).

In this mode, the probe needle 2
In 6, the liquid is sucked and discharged as shown in FIG. In the initial state, air and dilution water are contained as shown in FIG. Next, 200 ul of the anti-dilution liquid is inhaled (FIG. (C)). Then, the diluent is injected into the filter 52 (FIG. 2D). Next, 1500 ul of the second stage diluent is sucked in (FIG. (E)), and this diluent is injected into the filter 52 (FIG. (F)).

The multi-stage filtration of the present invention is not limited to the above-described two-stage filtration, but may be a three-stage filtration or a filtration in which the number of stages is larger. In that case, the above-mentioned first-stage filtration is repeated.

Next, a mode in which a creamy sample is extracted, filtered, and automatically injected into the input port of the liquid chromatography system will be described.

FIG. 23 is a plan view showing the structure of the automatic pretreatment device in this mode, and FIG. 24 is a diagram for explaining the structure and operation of the plunger pump. The difference between the configuration of the automatic pre-processing device of FIG. 23 and the configuration of the automatic pre-processing device of FIG. 2 is only the following, and the others are exactly the same. That is, in the present automatic pretreatment device, a rack table 301 for accommodating a plurality of sample containers and an automatic balance 302 are installed as rack means 300, and a plunger pump 303 for sampling cream is provided. ing.

As shown in FIG. 24, the plunger pump 303 has a disposable disposable housing composed of a cylinder portion 304 and a piston portion 305 detachably attached to the automatic pretreatment device side by a housing holder 306. The piston 305 is configured to be slid downward by the motor 307 and the drive system 308. The tip of the cylinder 304 has a thin needle shape, and has a disposable disposable tip 309 attached thereto. Further, a discharge needle 310 for pressurized air (about 0.3 kg / cm ² ) is provided in parallel with the disposable chip 309. The tip of the discharge needle 310 is located behind the tip of the disposable tip 309.

The cream 31 in the sample collection container 311
2 is sampled in the plunger pump 303, as shown in FIG.
9 is inserted so that the tip of the nozzle 9 is located outside the inner lid 313 in the sample collection container 311, and pressurized air is discharged from the discharge needle 310. As a result, the inner lid 313 is pressed, and the cream 312 is injected into the cylinder 304 via the disposable chip 309.

FIG. 25 is a flow chart showing the flow of the automatic injection mode for the creamy sample.

First, in step S40, the disposable housing and the disposable tip 309 are set in the plunger pump 303. In the next step S41, the empty sample container of, for example, 50 ml in the rack table 301 is moved to the position of the automatic balance 302 by the robot means 13 and the tare is weighed. The weighed result is output to the microcomputer described above.

Next, at step S42, the sample collection container 311 is set to the operating position of the plunger pump 303 by the robot means 13. That is, after the sample collection container 311 is horizontally moved directly below the plunger pump 303, as shown in FIG. The sample collection container 311 is moved upward so that the inserted and the tip of the discharge needle 310 is inserted outside the inner lid 313.

Thereafter, in step S43, pressurized air is discharged from the discharge needle 310 to make about 3 g of the cream 312.
Is injected into the cylinder part 304. Next, step S4
In step 4, the robot 13 is operated to return the sample collection container 311 to the original position.

In the next step S45, the empty sample container in which the tare is weighed is moved to the position of the plunger pump 303 by the robot means 13, and the flow proceeds to step S46.
The motor 307 of the plunger pump 303 is driven to slide the piston 305 downward,
A portion (about 1 g) is poured into an empty sample container. Next, in step S47, the robot means 13 is operated to remove the sample container containing the cream from the automatic balance 3.
02, and weighing is performed in the next step S48. The weighed result is also output to the microcomputer described above.

After the disposal chip 309 and the like are discarded in step S49, in step S50, the weighed sample container is moved to the container storage section of the sample row of the turntable 15 by the robot means 13.

In the next step S51, injection of the extraction solvent into the sample container, dispersion by stirring and application of ultrasonic waves in step S52, filtration in step S53,
The automatic injection into the input port of the liquid chromatography system in step S54 is exactly the same as in the case of the previously described mode, and therefore the description is omitted.

Next, a description will be given of a prescribed liquid charging mode in which the level of the liquid to be injected into the volumetric flask is measured and a fixed amount is charged. FIG. 8 is a flowchart showing a liquid level detection operation for measuring the liquid level in this mode. Hereinafter, description will be made with reference to FIG. 8 and FIGS. 4 to 7 showing the configuration and the like of the liquid level detecting means.

First, in step S70 of FIG. 8, the measuring flask whose liquid level is to be measured is transferred to the mounting means 72 by the robot means. The mounting means 72 is configured to be vertically movable with the measuring flask mounted thereon. In response to a control signal corresponding to the size of the measuring flask and the like sent from a control means (not shown), the mounting means 72 moves up and down to a predetermined position while the measuring flask 72a is mounted.

On the other hand, in step S71, the support means 74 for vertically supporting the sensor means 73 attached to the support part also moves in accordance with a control signal from the control means. The sensor means 73 is moved up and down to the position.

In step S72, the measuring flask 7
2a is illuminated by a light source 71 disposed on the opposite side of the mounting means 72 from the sensor means 73. At this time, the sensor unit 73 receives the transmitted light transmitted through the measuring flask 72a and outputs the video signal to the signal processing unit 75. Then, the signal processing unit 75 and the arithmetic unit 76
The pulse corresponding to the mark 72b, which is a mark indicating the set amount to be injected, attached to the volumetric flask 72a is recognized, and its position is stored. That is, in FIG. 5, in the waveform 73a of the video signal output from the one-dimensional CCD camera 73 as the sensor means, the reference line 72b is observed as the waveform shown in 73b because it blocks light. Waveform 73
The waveform obtained by binarizing a at a certain slice level 73d is 7
3e, and in this waveform 73e, a waveform 73f is a binarized waveform of a mark line. This waveform 73f
The value of the time width of the rise and fall of the waveform is written in the first-in first-out memory, and the width of the waveform is measured by the pulse width determination circuit of the arithmetic unit 76, and the position of the reference line is recognized.

Next, in step S73, the robot means moves the probe needle 77 under the control of the control means.
Is transferred to the measuring flask 72a, and the tip is inserted into the measuring flask. Then, in step S74, the syringe pump 79 is driven,
The liquid is started to be injected into the volumetric flask 72a through the three-way switching valve 78 switched to the probe needle 77 side. At this time, since a plurality of pores are provided at the distal end of the needle 77, the liquid is almost uniformly discharged to the inner wall surface of the volumetric flask 72a in a shower shape, and is flushed down along the tube wall.

As the liquid is injected in this way,
The liquid level in the measuring flask 72a rises. Then, in step S75, it is determined whether the liquid level has risen to the vicinity of the marked line 72b of the measuring flask 72a. That is,
In FIG. 5, in the waveform 73a of the video signal output from the one-dimensional CCD camera 73 as the sensor means, the reference line 72b and the liquid level 72c (the meniscus portion) correspond to the reference line 72.
b and to reduce the amount of light passing through the liquid level 72c,
The waveform 73a is observed as waveforms 73b and 73c, respectively. The waveform 73a is converted to a certain slice level 73.
The waveform binarized by d is 73e, and this waveform 73e
In the figure, the waveform 73g is a binarized waveform of the liquid level, and the waveform 73f is a binarized waveform of the marked line. The values of the rise and fall time widths of each of the waveforms 73f and 73g are written in a first-in first-out memory, and the width of the waveform is measured by the pulse width determination circuit of the arithmetic unit 76, and the position of the marked line And the position of the concave bottom of the liquid level. As the liquid is injected from the probe needle 77, the liquid level 72c rises and approaches the marked line 72b. Since the position of the liquid level is recognized by continuously measuring the waveform widths of the waveforms 73f and 73g, an appropriate time before the liquid level reaches the mark position is determined. Therefore, when the liquid does not transmit light, the liquid level cannot be measured by this method.

When the liquid level 72c rises to the vicinity of the marked line 72b (Yes at Step S75), Step S76 is performed.
In, a control signal is sent from the control means to the syringe pump 79 so as to switch the driving speed to a low speed. Then, by this speed switching, the liquid is injected into the volumetric flask 72a at a lower speed, and the rising speed of the liquid level 72c becomes slower.

In this state, in step S78, it is determined whether the liquid level 72c matches the marked line 72b. The operation of the determination is the same as that in step S75 described above, and a description thereof is omitted.

When the coincidence between the liquid surface 72c and the reference line 72b is detected (Yes at Step S78), a coincidence detection signal is sent from the detection means constituted by the signal processing section 75 and the arithmetic section 76 to the control means, and Step S79 is performed. In the above, a control signal is sent from the control means, which has received the coincidence detection signal from the detection means, to the three-way switching valve 78 so that the flow path is switched to the discharge bottle 81 side, and the three-way switching valve 78 operates according to this control signal. To change the flow path.

Then, in step S80, the syringe pump 79 stops after the remaining amount of the liquid in the pump is completely depressed. At this time, the remaining liquid is discharged to the discharge bottle 81 by the switching of the flow path by the three-way switching valve 78. In this way, a fixed amount of liquid is correctly charged into the measuring flask 72a.

When the charging of the liquid into the volumetric flask 72a is completed, the probe needle 77 is pulled out of the volumetric flask 72a and moved by the robot under the control of the controller in step S81. Further, in step S82, the measuring flask 72a is transferred to the port of the next processing step by the robot means under the control of the control means.

As described above, the liquid injection speed is switched to the low speed when the liquid level rises to the vicinity of the mark line, and the completion of the quantitative charging is detected by judging the coincidence between the mark line and the liquid level. When the flow path is changed by the three-way switching valve at the time when the liquid level is measured, the liquid level measurement becomes more accurate, and the constant volume operation is performed with high accuracy.

In the embodiment described above, the rack means is configured to store only the volumetric flask or the sample container, or to store the sample container and the automatic balance. May be stored. For example, in addition to a volumetric flask and a sample container, small containers such as a filtration container, a transfer container, and a dilution container may be stored and exchanged with those on a turntable by robot means, or may be replaced with a flat surface by a conveyor or the like. Automatic replacement may be performed. Even if the rack means is configured to circulate three-dimensionally, automatic replacement is possible.

The robot means can be realized by various robot means other than the configuration of the embodiment described above. It is also effective to provide a plurality of these robot means.

[0111]

As described in detail above, the automatic pretreatment apparatus according to the present invention uses the marked line of the measuring flask and the level of the liquid charged in the measuring flask based on the video signal output from the sensor means. And detecting means for outputting a match detection signal upon detecting a match with the control means, and controlling the probe means to stop discharging the sampled liquid from the probe means in response to the match detection signal from the detection means. Therefore, the liquid can be quickly and extremely accurately charged to the mark line of the measuring flask. Further, since the positioning of the mounting means and the sensor means for the volumetric flask are automatically performed according to the volume of the volumetric flask, an automatic pretreatment device capable of easily performing a constant volume operation for volumetric flasks of various volumes is provided. Can be provided.

[Brief description of the drawings]

FIG. 1 is a perspective view schematically showing a configuration of an automatic pretreatment device according to an embodiment of the present invention.

FIG. 2 is a plan view of the automatic pretreatment device in the embodiment of FIG.

FIG. 3 is a partial cross-sectional view of FIG.

FIG. 4 is a diagram showing a schematic configuration of a liquid level detecting means of the apparatus according to one embodiment of the present invention.

FIG. 5 is an explanatory diagram of a liquid level detecting operation of the apparatus according to the embodiment of the present invention.

FIG. 6 is a view showing a liquid inflow path of the apparatus according to one embodiment of the present invention.

FIG. 7 is a diagram illustrating a schematic configuration of a signal processing unit and a calculation unit of a liquid level detecting unit of the apparatus according to one embodiment of the present invention.

FIG. 8 is a flowchart showing a liquid level detecting operation of the apparatus according to the embodiment of the present invention.

FIG. 9 is an explanatory view of a probe means in the embodiment of FIG.

FIG. 10 is a sectional view of the horizontal two-joint robot in the embodiment of FIG.

FIG. 11 is a diagram showing an example of a finger which is an attachment for holding a sample container.

FIG. 12 is a diagram illustrating an example of a finger that is an attachment for gripping a probe needle.

FIG. 13 is a block diagram schematically showing an electric configuration of a control unit in the embodiment of FIG.

14 is a flowchart schematically showing an example of a control program of the microcomputer in the embodiment of FIG.

FIG. 15 is a diagram illustrating a teaching process in the embodiment of FIG.

FIG. 16 is a diagram illustrating a teaching process in the embodiment of FIG.

FIG. 17 is a diagram illustrating a teaching process in the embodiment of FIG. 1;

FIG. 18 is a flowchart showing the flow of a dissolution-extraction-dilution-filtration-injection mode in the embodiment of FIG.

FIG. 19 is a diagram illustrating an operation sequence in the mode of FIG. 18;

FIG. 20 is a flowchart showing a flow in a two-stage filtration mode in the embodiment of FIG. 1;

21 is a diagram illustrating the operation of the probe unit, the robot unit, and the filter robot unit in the mode of FIG.

FIG. 22 is a diagram illustrating behavior of a liquid in a probe needle.

FIG. 23 is a plan view showing a configuration of an automatic pretreatment device when a mode relating to pretreatment of a creamy sample is performed.

FIG. 24 is a diagram illustrating the configuration and operation of a plunger pump.

FIG. 25 is a flowchart showing a flow of a mode relating to pretreatment of a creamy sample.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 Turntable means 11 Rack means 12 Probe means 13 Robot means 14 Filter robot means 15 Turntable 16, 17, 18, 19 Container storage part 16a, 17a, 19a Container 18a, 30 Female flask (sample container) 26, 77 Probe needle 27, 78 Three-way switching valve 28 Micro syringe pump 31 Finger 70 Liquid level measuring means 71 Light source 72 Mounting means 73 Sensor means (CCD camera) 74 Support means 75 Signal processing unit 76 Operation unit 79 Syringe pump 100 CPU 101 ROM 102 RAM 103 , 104 input / output interface 105 display device 106 teaching unit 107 bus

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. ⁷ , DB name) G01N 35/00-35/10 G01F 23/28 B01L 3/08

Claims (8)

(57) [Claims] 1. A turntable means on which a plurality of containers including a volumetric flask can be placed, and a rack means which is at a stationary position separate from the turntable means and on which the plurality of containers can be placed; The sampled liquid is sampled and discharged into a volumetric flask placed on the turntable means, and the sampled liquid is injected up to a level below the mark of the volumetric flask, and up to the mark of the volumetric flask. A probe means for separately sampling one of the liquid and the diluent and discharging the liquid and the diluent to the volumetric flask so as to inject one of the liquid and the diluent; and The measuring flask loaded with the liquid can be placed to a level below, and the placing means is movable in the vertical direction. A light source having a substantially uniform brightness in a strip shape in the vertical direction; and a support means disposed on the other side of the mounting means for supporting the support portion movably in the vertical direction. Sensor means attached to the support portion for receiving light from a light source transmitted through a measuring flask mounted on the mounting means and outputting a video signal; and one of the separately sampled liquid and diluent While is being discharged from the probe means into the volumetric flask placed as described above, based on the video signal output from the sensor means, the marked line of the volumetric flask and the liquid injected into the volumetric flask and Detecting means for detecting the coincidence of the diluent with one of the liquid levels and outputting a coincidence detection signal; each container including the volumetric flask and the probe means being connected to the turntable means and the rack. Robot means configured to be transferable between each of the means and the mounting means, a transfer operation of the robot means, a vertical movement operation of the mounting means, a vertical movement operation of the support portion, And controlling the sampling operation of the probe means,
Control means for controlling a discharge operation of the probe means so as to stop discharge of one of the sampled liquid and the diluent from the probe means in response to a coincidence detection signal from the detection means. And an automatic pretreatment device. 2. The apparatus according to claim 1, wherein said probe means includes a probe needle capable of inserting a tip into each of said containers, and a micro syringe pump for sucking and discharging a predetermined amount of liquid through said probe needle. The automatic pretreatment device according to claim 1, wherein 3. The probe needle has a tip at its tip,
3. The automatic pretreatment apparatus according to claim 2, wherein a plurality of fine holes for discharging one of the liquid and the diluent almost uniformly in a shower shape are provided on an inner wall surface of the inserted container. 4. A three-way switching valve, which is capable of switching a liquid flowing from a single inlet to one of two outlets and allowing the liquid to flow out, is disposed on the discharge side of the probe means. 2. The discharge device according to claim 1, wherein when the one of the diluting liquid is discharged into the measuring flask and the discharging is stopped, the three-way switching valve is switched to control the discharging and the discharging of one of the liquid and the diluting liquid. The automatic pretreatment device according to any one of claims 1 to 4. 5. An image sensor using a one-dimensional CCD camera is adopted as said sensor means, and said detecting means converts a video signal output from said sensor means into a digital signal by binarization. A circuit for generating a rising and falling pulse of a waveform, and a signal processing unit having a first-in first-out memory circuit; The automatic pretreatment device according to claim 1, wherein the automatic pretreatment device is provided. 6. The positioning operation of the placing means by vertically moving the placing means to a predetermined position in accordance with the volume of the volumetric flask into which the liquid has been injected to a level below the marked line. The automatic pre-processing device according to any one of claims 1 to 5, wherein 7. The sensor means moves the support means attached to the support part to a predetermined position in accordance with the volume of the volumetric flask into which the liquid has been injected to a level below the mark. 7. The automatic pre-processing apparatus according to claim 1, wherein the automatic pre-processing apparatus controls the positioning operation of the supporting means by moving the supporting means up and down. 8. The Vortex m in a stationary position separate from the turntable means, the rack means, the placing means and the like.
A stirring means employing an ixer is provided, and the robot means is configured to be capable of transferring the containers together with the turntable means, the rack means, and the placing means together with the stirring means. Claims 1 to 7
The automatic pretreatment device according to any one of the above.