JPH05164761A - Automatic preprocessor for chemical analysis - Google Patents

Abstract

PURPOSE:To automatically and efficiently perform a series of preprocessing operations for chemical analysis, such as the filtration of sample liquids, dilution of the filtered sample liquids, transfer of containers, stirring of the sample liquids, etc., and, at the same time, to simplify and miniaturize the title preprocessor. CONSTITUTION:An automatic filtering device section 10 filter sample liquids by using marketable filter units 2 fed one piece one piece from a filter stocker 16. Then an automatic diluting/container transferring device section 16 dilutes the filtered sample liquids while the section 16 transfers the sample containers 24 containing the sample liquids from a rack 26 to a shaking device 18.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION The present invention relates to a solid preparation in various solvents in dissolution test for measuring the degree of dissolution of preparation components when the solid preparation such as tablets, granules and capsules is immersed in the solvent. After collecting a part of the solution in which the main drug is eluted by immersing in the sample solution, and before conducting the chemical analysis of the sample solution collected, the sample solution is filtered so that the sample solution contains solids and dust. In such a case, the present invention relates to a device for automatically performing a series of pretreatment operations for removing them and diluting and adjusting the sample liquid after filtration.

[0002]

2. Description of the Related Art The dissolution test of solid preparations such as tablets, granules and capsules has recently been regarded as important as one of the quality evaluation methods for preparations. This dissolution test is to examine the dissolution rate of the main drug when the solid preparation is dipped in various solvents. It is injected into a sample container in a predetermined amount and solidified in various solvents kept at a temperature of about 37 ° C. Put the formulation in, take a part of the solution several times over the course of time, and perform absorptiometric analysis of each of the sample liquids with a spectrophotometer to record the change over time in the elution amount of the main drug. It is done by Further, in the case of simultaneous measurement of multiple components in a preparation, a sample liquid is collected and liquid chromatographic analysis is performed.

In this dissolution test, if the sample liquid sent to the analyzer contains solids or dust, an error will occur in the measured value, and the reliability of the analysis result will be significantly lost. Prior to subjecting the sample solution to chemical analysis, the sample solution is filtered to completely remove solids and the like in the sample solution. Further, when the sample liquid is introduced into the analytical instrument, the filtered sample liquid is diluted and adjusted to an appropriate concentration.

The above-mentioned filtration operation of the sample liquid has been conventionally performed.
A part of the sample solution in which the solid preparation is dissolved in a solvent is manually separated into an injection cylinder, and a commercially available filter unit 2 as shown in FIG. 9 is attached to the tip of the injection cylinder, and the sample solution is removed from the injection cylinder. Was extruded and passed through the filter unit 2 to filter the sample liquid. In the filter unit 2 shown in FIG. 9, a large-diameter tubular protrusion 6 ′ having a connection port 6 is formed in the center of the upper surface of the disk-shaped body 4, and the connection port is formed in the center of the lower surface of the body 4. 8 has a small diameter tubular protrusion 8'having an outer diameter equivalent to the inner diameter of the large diameter tubular protrusion 6 ', and the filter material is housed inside the body 4 of the package. Have

When the filtered sample liquid is diluted with a diluting liquid such as pure water to an appropriate concentration, an automatic diluting device equipped with moving mechanisms for moving the diluting nozzle in the vertical direction and in the X and Y directions, respectively. Is used. That is, the dilution nozzle is moved by each of the X-direction and Y-direction movement mechanisms, the dilution nozzle is positioned and stopped immediately above one of the many containers stored in parallel in the rack, and the dilution nozzle is moved by the vertical movement mechanism. After lowering and inserting the lower end of the dilution nozzle into the sample container, drive control the syringe connected to the dilution nozzle and the flow path switching valve, and pass pure water together with the sample liquid through the dilution nozzle into the sample container. To be discharged. Then, the sample container in which the sample liquid and pure water are dispensed is transferred from the rack to the stirring device by an automatic transfer device attached to the automatic diluting device or manually, and the sample container is rocked by the stirring device. By stirring the liquid contained inside, a sample liquid adjusted to an appropriate concentration can be obtained.

[0006]

As in the prior art, after manually filtering the sample liquid, pure water is added to the filtered sample liquid by an automatic diluter, and then by an automatic transfer device or manually. The sample container is transferred from the rack to the stirrer by using the stirring device to prepare the sample liquid by stirring and mixing the liquid in the sample container. The transfer of the sample container containing the sample solution and the stirring and mixing operation are performed individually, and some operations are performed manually, so a series of pretreatment operations for chemical analysis takes time, and the dissolution test The work efficiency in operation also deteriorates. In addition, manually performing the filtering operation of the sample liquid is very troublesome and requires a lot of labor at a business office such as a pharmaceutical company that needs to repeatedly perform dissolution tests on various solid preparations. Furthermore, since an automatic transfer device is provided separately from the automatic diluter to transfer the sample container from the rack to the stirring device, the overall device configuration and drive / control mechanism become complicated,
Further, there is a problem that a large space is required for the entire device.

The present invention has been made in view of the above circumstances, and is required for a series of pretreatment operations for chemical analysis, such as filtration of a sample solution, dilution of a filtered sample solution, transfer of a container, and stirring. An automatic pretreatment device that can improve work efficiency by shortening time, does not require any human hands, can simplify the device configuration and drive / control mechanism, and can save space for the entire device. It is a technical issue to provide.

[0008]

According to the present invention, an automatic pretreatment device for chemical analysis is constructed as follows. That is,
The apparatus according to the present invention includes an automatic filtration device section for performing a filtering operation of a sample liquid, a sample container rack for accommodating a plurality of sample containers in which the filtered sample liquid is dispensed in parallel, a sample liquid and a diluting liquid. A sample container rack that stores a plurality of sample containers that are injected and stirred and mixed in parallel, an automatic dilution / container transfer device section that performs the dilution operation of the sample liquid after filtration, and transfers the sample container, and the sample The container is configured to include a stirring device that rocks the container to stir and mix the sample liquid and the diluent contained in the container. The automatic filtering device section accommodates a plurality of filter units, each of which has a filter material housed inside a package having connection ports formed on the upper side and the lower side, in a vertically stacked state, and has a lower end opening surface. One of the cylindrical filter stocker that is the outlet and the connection port of the filter unit that is sequentially supplied one by one from the outlet of the filter stocker is connected to the sample liquid supply source. A filter unit setting device that connects and disconnects the liquid tube and the drain tube to the drain tube and the drain tube are connected to each other, and flow into the filter unit from the sample solution supply source through the tube. Then, the sample liquid that has been filtered while flowing through the filter unit and flows out into the drain tube is supported. It is composed of a sample liquid dispensing device having a discharge nozzle for discharging the pull vessel.
Further, the automatic dilution / container transfer device section is connected to the diluent supply source by a flow path, and sucks the filtered sample liquid contained in the sample container contained in the sample container rack from the lower end port and inhales the same. A diluting nozzle that discharges the sample liquid with the diluting liquid into the sample container stored in the sample container rack from the lower end port, suction of the sample liquid into the diluting nozzle, and dilution from the diluting liquid supply source to the diluting nozzle A syringe and a flow path switching valve for driving and controlling the operations of feeding the liquid and discharging the sample liquid and the diluting liquid from the diluting nozzle into the specimen container, and a movable holding for holding the diluting nozzle so that it can reciprocate in the vertical direction. Body and a sample which is held by the movable holder so as to be reciprocally movable in the vertical direction, and which is located immediately below the dilution nozzle among the sample containers stored in the sample container rack. Container holding device having a holding arm for detachably holding the container, a holding arm elevating mechanism and a nozzle elevating mechanism for vertically reciprocating the container holding device and the dilution nozzle, and the movable holding body in the X direction. It is composed of an X and Y direction moving mechanism for moving in the Y direction. The stirring device is arranged within the movable range of the container gripping device.

When the apparatus having the above-mentioned configuration is used, the sample solution is filtered, the filtered sample solution is diluted, the container is transferred, and the like, which is carried out when a sample is chemically analyzed using an analytical instrument such as a spectrophotometer in a dissolution test. A series of pretreatment operations such as stirring will be automatically performed.

[0010]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT A preferred embodiment of the present invention will be described below with reference to the drawings.

FIGS. 1 to 3 respectively show the overall structure of an automatic pretreatment system for chemical analysis according to one embodiment of the present invention. FIG. 1 is a side view showing a state in which a side cover is removed, and FIG. Is a front view showing a state in which a front cover is removed, and FIG. 3 is an external perspective view.

This device comprises an automatic filtering device section 10 and a dispensing section 1.
2, the container storage unit 14, the automatic diluting / container transfer device unit 16 and the stirrer 18 are configured, and the container storage unit 14 includes
A sample container rack 22 that accommodates a plurality of sample containers 20 arranged in parallel in the X and Y directions and a sample container rack 26 that accommodates sample containers 24 arranged in parallel in the X and Y directions are arranged. There is. Reference numeral 28 in FIG. 3 is an operation panel.

As shown in FIG. 4, which is a perspective view of a main part of the automatic filter device unit 10 in a partially broken state, the automatic filter unit unit 10 includes a filter accommodating unit 110, a filter take-out unit 112, and a filtering operation unit 114. , The device shown in the figure is a 6-unit type,
In the filter housing portion 110, six cylindrical filter stockers 116 are arranged side by side. Filter stocker 1
A plurality of commercially available filter units 2 as shown in FIG.
The small-diameter tubular projection 8'is inserted into and fitted into the large-diameter tubular projection 6'of the filter unit 2 located on the lower side, and is accommodated in a state of being connected in the vertical direction.

In the filter take-out section 112, a pair of block bodies 118 and 120 are arranged below the filter stocker 116. One of the block bodies 118 has a planar shape at a position corresponding to each filter stocker 116, as shown in a perspective view of only a part (the front end in FIG. 4) of the automatic filtering device section 10 in FIG. U-shaped support / removal claws 122 are respectively provided to project in the horizontal direction. In addition, the other block body 120 has the support / removal claws of the one block body 118.
At a position corresponding to 122, a concave portion 124 having a U-shaped planar shape and into which the support / removal pawl 122 is fitted is formed. Then, the support / removal claw 122 of the one block body 118
Has a bearing surface for bearing the barrel portion 4 of the filter unit 2 on the upper surface, and has a tapered cam surface 128 on the surface facing the other block body 120. Further, the other block body 120 has an upper surface serving as a bearing surface 130 for supporting the body portion 4 of the filter unit 2, and a surface facing the one block body 118 is formed in a tapered shape to serve as a cam surface 132.

On the other hand, in the filtering operation unit 114, a pair of block bodies 134, 1 adjacent to the pair of block bodies 118, 120 of the filter take-out unit 112 and parallel to the block bodies 118, 120.
36 are provided. Then, one block body 134 has a U-shaped planar shape at a position corresponding to each upper flow path connector 146, which will be described later, disposed adjacent to each filter stocker 116, and the other block body. Detachment claws 138 each having a tapered cam surface 142 are horizontally projected on the surface facing the 136. Further, in the other block body 136, a concave portion 140 into which the release claw 138 is fitted and which has a U-shaped planar shape is formed at a position corresponding to each release claw 138 of the one block body 134, A surface of the other block body 136 facing the one block body 134 is formed in a tapered shape to form a cam surface 144.

The pair of block bodies 118 and 120 of the filter take-out section 112 are centered on the take-out port of the filter stocker 116 and the pair of block bodies 13 of the filtration operation section 114.
4, 136 are supported so as to approach and separate from each other symmetrically about the upper flow path connector 146, and further, the pair of block bodies 118, 120 of the filter take-out section 112 and the filtering operation section 114. A pair of block bodies 134, 13
6 and 6 are interlocked with each other, so that when one side approaches, the other side separates, and when one side separates, the other side approaches, so that they are driven so as to perform opposite operations of approaching and separating. It has become. That is, as shown in FIG. 5, the four block bodies 118, 120, 134, 136 are
One end of each of them is slidably engaged with the common guide rod 148, and one block body 118 of the filter take-out section 112 and one block body 134 of the filtration operation section 114 are respectively arranged. The end face is fixed to a common large connecting plate 150, and the other block body 120 of the filter take-out part 112 and the other block body 136 of the filtering operation part 114 are common small connecting plates at their one end faces. It is fixed to 152. Further, one end of each of the connecting arms 154 and 156 is pivotally attached to the large connecting plate 150 and the small connecting plate 152, and the other end of each of the connecting arms is attached to the mounting member.
It is pivotally attached to both ends of an interlocking arm 158 fixed to 160. Then, the rotation shaft 162 to which the mounting member 160 is fixed
Is rotated forward and backward by a drive motor (not shown), so that the pair of block bodies 11 of the filter take-out portion 112
The mechanism is such that 8, 120 and the pair of block bodies 134, 136 of the filtering operation unit 114 are interlocked with each other, and the opposite operations of approaching and separating are performed respectively.

Upper flow path connectors 146 are arranged in the filtering operation section 114 adjacent to the respective filter stockers 116, and each upper flow path connector 146 is fixed to a fixed table 164 as shown in FIG. It is fixed to. Upper flow path connector 146
A flow path through which the sample liquid flows is formed inside, and a liquid supply tube 166 is communicatively connected to one end of the flow path, and the other end of the flow path has a large-diameter tubular protrusion of the filter unit 2. 6'is in communication with a nozzle 168 which is inserted into the connection port 6 and engages with the large-diameter tubular projection 6 '.

Further, as shown in FIG. 6, the liquid supply tube 166 is communicatively connected to a liquid delivery syringe 172 via a three-way switching valve 170, and the liquid delivery syringe 172 is connected to the three-way switching valve 170.
Through, for example, a solid preparation dissolution operation section in the dissolution test apparatus. Then, the liquid delivery syringe 17
By driving 2 and controlling the switching of the three-way switching valve 170, a part of the solution in which the solid preparation is dissolved in a solvent is collected, and the sample solution is supplied from the liquid-feeding syringe 172 through the three-way switching valve 170. It is adapted to be fed to the upper flow path connector 146 through the liquid tube 166.

Below the block bodies 118, 120, 134 and 136, a lower flow path connector 174 is arranged. The lower flow path connector 174 includes a horizontal moving table 176 arranged so as to be capable of reciprocating in the horizontal direction, an elevating member 178 supported by the horizontal moving table 176 so as to be able to move up and down, and a liquid feed held by the elevating member 178. It is composed of a member 180 and a compression coil spring 182 for urging the liquid feeding member 180 upward. Incidentally, FIG.
4 is a diagram schematically showing the basic structure of the lower flow path connector 174 for easy understanding, and does not necessarily correspond to the structure shown in FIG. 4, but the same reference numerals as those in FIG. These are the same members that perform the same function.

As shown in FIG. 5, the horizontal moving table 176 is configured to be reciprocally moved in the horizontal direction by being guided by the guide rod 186 by driving the drive motor 184 in forward and reverse directions. Further, the elevating member 178 and the liquid feeding member 180 held by the elevating member 178 are horizontally moved by driving the drive motor 188 held by the horizontal moving table 176 through the elevating drive mechanism 190 supported by the horizontal moving table 176. It is adapted to reciprocate vertically with respect to the table 176. A supporting recess 192 for supporting the filter unit 2 is formed at the upper end of the liquid feeding member 180 and has an insertion opening into which the small-diameter tubular protrusion 8 ′ of the filter unit 2 is inserted. Liquid channel 1 penetrating into

Then, the elevating member 178 is raised while the filter unit 2 is supported in the supporting recess 192 of the liquid feeding member 180, and the upper flow path connector is connected to the connection port 6 of the large-diameter tubular projection 6'of the filter unit 2. The nozzle 168 of 146 is inserted, and the connection port 8 of the small-diameter tubular protrusion 8 ′ of the filter unit 2 is pressed against the insertion port of the support recess 192 of the liquid feeding member 180 by the elastic force of the compression coil spring 182. ..
In the state shown in FIG. 6, when the sample sending liquid is sent to the upper flow path connecting device 146 through the liquid supply tube 166 by the liquid sending syringe 172, the sample liquid flows through the internal flow path of the upper flow path connecting device. Through the nozzle 168, into the filter unit 2, and is filtered while passing through the filter material contained in the body 4 of the filter unit 2, and the filtered sample liquid is the small-diameter tubular protrusion 8 ′ Through the connection port 8 into the liquid delivery member 180, flows through the internal liquid flow path 194, enters the drainage tube 196, and passes through the drainage tube 196 and the discharge nozzle 202 of the dispensing unit 12. Will be sent to.

3 is a filter stopper, and this filter stopper 198 pushes the stopper piece 200 to a position below the unused filter stocker 116 among the six filter stockers 116, and the stopper piece 200 By supporting the filter unit 2 with 200, the filter stocker 11
6 This is to prevent the filter unit 2 from falling through the outlet at the bottom.

The discharge nozzle 202 of the dispensing unit 12 is supported by a dispensing arm 204 which is reciprocally held in the vertical direction, and the dispensing arm 204 is moved in the vertical direction and X by a dispensing arm drive mechanism 206. It is movable in the Y direction and the Y direction. Illustration and description of the configuration of each of these moving mechanisms are omitted. The discharge nozzle 202 of the pipetting unit 12 is moved in the X direction and the Y direction to stop the positioning immediately above one of the empty sample containers 20 stored in the sample container rack 22, and then the discharge nozzle 202 is discharged. And lower end thereof is inserted into the sample container 20 as shown in FIG. 6, and the filtered sample liquid 100 is added to the sample container 20.
To be injected inside. The operation of the automatic filtering device section 10 having the above-described configuration will be described. First, the filter unit 2 at the lowest position in the filter stocker 116 is described.
Is supported by the liquid feeding member 180, the pair of block bodies 118 and 120 of the filter take-out section are separated from each other, and the pair of block bodies 134 and 136 of the filter operation section are brought close to each other, and Of the pair of block bodies 118 and 120 by horizontally moving the block bodies 118 and 120 in the direction of approaching each other and moving the pair of block bodies 134 and 136 of the filtering operation unit in the direction of separating from each other. The filter unit 2 at the lowest position in the plane is separated from the other filter units 2 above it. At this time, the separated filter unit 2
The liquid feeding member 180 supporting the pair of block members 118,
Since the filter unit 2 is interposed from both cam surfaces of 120 to receive a downward force, the compression coil spring 182 is pushed downward against the elastic force. On the other hand, the plurality of filter units 2 remaining in the filter stocker 116 are supported by the bearing surfaces of the upper surfaces of the pair of block bodies 118 and 120, and are retained in the filter stocker 116. Next, by moving the elevating member 178 downward with respect to the horizontal moving table 176, one filter unit 2 is taken out below the pair of block bodies 118 and 120 while being supported by the liquid feeding member 180. Be done.

Next, the horizontal moving table 176, on which the lifting member 178 is supported, is moved in the horizontal direction to move the liquid feeding member 180, which is held by the lifting member 178 and supports the filter unit 2, to the upper flow path of the filtering operation section. It is moved to a position directly below the connector 146 and stopped. Then, by moving the elevating member 178 upward with respect to the horizontal moving table 176, the nozzle 168 of the upper flow path connector 146 is inserted into the connection port of the large-diameter tubular protrusion of the filter unit 2, and
The connection opening of the small-diameter tubular projection of the filter unit 2 is elastically pressed by the compression coil spring 182 to the insertion opening of the support recess of the liquid feeding member 180. This state corresponds to the state shown in FIG. 6, and in this state, the sample liquid is filtered as described above.

When the sample liquid filtering operation is completed, the elevating member 178 is moved downward with respect to the horizontal moving table 176. With this operation, the used filter unit 2 is left behind above the liquid feeding member 180 in a state where the large-diameter tubular projection is engaged with the nozzle 168 of the upper flow path connector 146. Then, by moving the horizontal moving table 176 in the horizontal direction, the empty liquid feeding member 180 is moved to a position directly below the filter stocker 116 of the filter take-out section and stopped. Then, the elevating member 178 is moved upward with respect to the horizontal moving table 176, and at the same time, the pair of block bodies 118 and 120 of the filter take-out section are separated from each other, and the pair of block bodies 134 and 1 of the filtering operation section are arranged.
Horizontally move the 36 toward each other. As a result of these operations, the used filter unit 2 is moved upward by the cam surfaces of the pair of block bodies 134 and 136 to form the upper flow path connector.
Remove from the nozzle 168 of 146. At the same time, a plurality of unused filter units 2 in the filter stocker 116 drop, and the lowermost filter unit 2 is supported by the liquid feeding member 180. Then, by repeating the above series of operations again, the filtering operation proceeds.

Next, the respective components of the automatic diluting / container transferring device section 16 and the stirring device 18 will be described with reference to FIG. Figure 7
FIG. 3 is a perspective view showing a partially broken configuration of a main part of an automatic diluting / container transfer device section 16, wherein the device section 16 includes a dilution nozzle device 210, a container gripping device 212, and a horizontal movement holding device for holding them. It is composed of a plate 214 and a movable part including a horizontal movement mechanism 216 for moving the horizontal movement holding plate 214 in the X direction and the Y direction in a horizontal plane.

The diluting nozzle device 210 holds the diluting nozzle 222 and the upper end of the diluting nozzle 222 to fix and hold the diluting nozzle 222 in a vertical posture, and a vertical connecting plate 226 fixedly connected to a horizontal moving holding plate 214. A nozzle holding portion 224 that is engaged with a guide rail 228 fixed to the guide rail 228 and is reciprocally movable in the vertical direction by being guided by the guide rail 228, and a moving nut that is integral with the nozzle holding portion 224.
230, a nozzle drive shaft 232 that rotates by screwing with the moving nut 230, and raises and lowers the nozzle holding portion 224 and the dilution nozzle 222 by the rotation operation, and a power transmission roller fixed to the upper end of the nozzle drive shaft 232. 234, a drive motor 236 attached to the horizontal movement holding plate 214, a drive pulley 238 fixed to the rotation shaft of the drive motor 236, and a belt 240 wound around the drive pulley 238 and the power transmission roller 234. It is composed of a nozzle lifting drive device. Dilution nozzle 222
As shown in the schematic cross-sectional view of the schematic structure of the flow path in FIG. 8, a liquid feed for dilution composed of a sample liquid measuring syringe 278, a pure water measuring syringe 280, a flow path switching valve 282, etc. A flow path connection is made to the device. And the drive motor 23
By driving 6 forward and reverse, the drive pulley 23
8, the nozzle drive shaft 232 is rotated clockwise and counterclockwise via the belt 240 and the power transmission roller 234, and the nozzle holding part 224 and the dilution nozzle 222 are guided along the guide rail 228 by the rotation operation of the nozzle drive shaft 232. It can be raised and lowered.

Further, the container gripping device 212 includes an elevating and lowering drive shaft 242 having an upper end portion rotatably engaged with a horizontal movement holding plate 214, a moving nut 244 screwed to the elevating and lowering drive shaft 242, and a moving nut 244. A pair of gripping arms 248, 248, which are integrally fixed and slidably engaged with the guide rail 228, each of which has two abutting rods 250 and which are capable of expanding and contracting, and a pair of gripping arms thereof. A container transfer robot 246 having a driving mechanism for driving the arms 248, 248, a power transmission roller 252 fixed to the lower end of the elevation drive shaft 242, and a horizontal holding plate 254 fixedly connected to the vertical connecting plate 226. Lifting drive motor 2 attached
56, a robot elevating and lowering drive device including a drive pulley 258 fixed to the rotary shaft of the elevating and lowering drive motor 256, and a belt 260 wound around the drive pulley 258 and the power transmission roller 252. The container transfer robot 246 is provided immediately below the dilution nozzle 222 of the plurality of sample containers 24 stored in the plurality of storage holes 262 formed in parallel in the X direction and the Y direction of the sample container rack 26. A pair of gripping arms 248, 248 is provided for the dilution nozzle 222 so that it can grip the positioned one. Further, when the sample container 24 is gripped by the pair of gripping arms 248, 248 of the container transfer robot 246, the tip of the dilution nozzle 222 can be inserted into the sample container 24 through the upper end opening of the sample container 24. In addition, a pair of gripping arms 248, 248 are attached. Then, by driving the drive motor 256 in the forward and reverse directions, the elevation drive shaft 242 is rotated clockwise and counterclockwise via the drive pulley 258, the belt 260 and the power transmission roller 252, and the elevation drive shaft 242 is rotated. By the operation, the container transfer robot 246 can be moved up and down along the guide rail 228.

The horizontal movement holding plate 214 to which the dilution nozzle device 210 and the container gripping device 212 are attached is arranged so as to be reciprocally movable in the X direction by being guided by the X direction guide rail 266, and the X direction drive motor 268. A timing belt (not shown) wound around a drive pulley fixed to the rotary shaft of the drive motor and a driven pulley arranged at a distance from the drive pulley. ) Is moved, the horizontal movement holding plate 214 connected to a part of the timing belt via the connecting plate 270 is moved in the X direction. Further, a pair of slide bearings 27 are attached to a holding substrate 272 that holds the horizontally moving holding plate 214 to which the X-direction drive motor 268, the guide rail 266, etc. are fixed.
4, 274 are fixed, and a pair of Y-direction guide rods 276, 276 are slidably inserted into the pair of sliding bearings 274, 274. The pair of Y-direction guide rods 276, 276 are fixed, and although not shown in the figure, they are connected to a part of the timing belt by a Y-direction drive device including a Y-direction drive motor, a drive pulley, a driven pulley and a timing belt. Holding substrate 272 along the pair of Y-direction guide rods 276, 276
It can be reciprocated in any direction.

As shown in FIG. 8, the diluting liquid feeding device comprises a sample liquid measuring syringe 278 and a pure water measuring syringe 280 which are connected to the diluting nozzle 222 via a liquid feeding tube 284.
And a flow path switching valve 282. The pure water measuring syringe 280 is a liquid transfer tube 28 in which a flow path switching valve 282 is inserted.
A container 288 containing pure water (sterile distilled water) 290 via 6.
Is connected to the flow path. The sample liquid measuring syringe 278 and the pure water measuring syringe 280 are the flow path switching valves.
A flow path is connected through a liquid sending tube 292 with 282 interposed. By switching the flow path switching valve 282, the pure water measuring syringe 280 can be selectively connected to the container 288 and the sample liquid measuring syringe 278 (and therefore the dilution nozzle 222) by a flow path. The flow path is configured as follows.

The stirring device 18 may be a conventionally used one, and the stirring device 18 causes the sample container 24 fitted in the holding hole 218 to rock at high speed in a horizontal plane. The liquid contained in the sample container 24 is agitated.

When performing the diluting / stirring operation by the diluting / container transferring device section 16 and the agitating device 18 having the above-described structure, first, the diluting nozzle 222 and the container transferring robot 246 are held at the uppermost positions, respectively, and horizontally. The horizontal movement holding plate 214 is moved in the X direction and the Y direction by the moving mechanism 216, and the plurality of sample containers 20 stored in the sample container rack 22 are moved.
It is positioned so that the dilution nozzle 222 is located directly above the filtered sample liquid 100 to be diluted. Next, the diluting nozzle is driven by the nozzle lifting drive.
222 is lowered so that its lower end is immersed in the sample liquid 100 in the sample container 20. At this time, the diluting liquid sending device is driven so that the tip of the diluting nozzle 222 is filled with pure water. Then, the flow path switching valve 282
8 to switch it to the solid line position as shown in FIG. 8, and drive the piston of the sample liquid measuring syringe 278 in the direction of the solid line arrow while the tip of the dilution nozzle 222 is filled with pure water. A predetermined amount of the sample liquid contained in the container 20 is sucked into the dilution nozzle 222, and the piston of the pure water measuring syringe 280 is driven in the direction of the solid line arrow, so that a predetermined amount of pure water 290 is introduced into the syringe 280. Suction.

When the suction operation of the sample solution is completed, the nozzle elevating / lowering device raises the dilution nozzle 222 to the uppermost position, and while holding the dilution nozzle 222 and the container transfer robot 246 at the uppermost position, the horizontal movement mechanism 216 is used. The horizontal movement holding plate 214 is moved in the X direction and the Y direction by the above, and the dilution nozzle 222 is located directly above the empty container into which the sample liquid is to be injected among the plurality of sample containers 24 stored in the sample container rack 26. To position. Next, the diluting nozzle 222 is lowered by the nozzle lifting drive device so that the lower end portion thereof is inserted into the sample container 24. In parallel with this operation, the container transfer robot 24 is opened with the pair of gripping arms 248, 248 expanded by the robot lifting drive device.
6 is lowered to the position of the sample container 24, and then the pair of gripping arms 248, 248 are driven to narrow the distance between them, and the sample container 24 is gripped by the four contact rods 250. Then, the robot elevating and lowering device raises the container transfer robot 246 in a state of gripping the sample container 24 to take out the sample container 24 from the sample container rack 26, and then the horizontal moving mechanism 216 moves the horizontal moving holding plate 214 in the X direction. And move in the Y direction,
The sample container 24 is transferred to the position of the stirring device 18, and the robot elevating drive device and the container transfer robot 246 are drive-controlled to fit and hold the sample container 24 in the holding hole 218 of the stirring device 18. During the transfer of the sample container 24, the flow path switching valve 282 of the diluting liquid sending device is operated to switch it to the chain line position, and then the pistons of the sample solution measuring syringe 278 and the pure water measuring syringe 280 are set. By simultaneously driving in the direction of the chain line arrow, a predetermined amount of sample liquid and a predetermined amount of pure water are discharged into the empty sample container 24 through the dilution nozzle 222. Thus, the dilution operation is performed while transferring the sample container 24 to the position of the stirring device 18, so that the working time is shortened.

The container transfer robot 246, which has set the sample container 24 in the stirring device 18, releases the grip of the sample container 24 and waits at that position. On the other hand, the sample container 24 held by the stirring device 18 is swung at high speed in the horizontal plane by the stirring device 18, and the liquid contained therein is stirred. When the stirring operation is completed, the container transfer robot 246
Hold the sample container 24 again by
While transferring the sample liquid from 18 to the original sample container rack 26 or another container rack, the sample liquid that has been stirred in the sample container 24 is diluted by the diluting nozzle by another flow channel configuration not shown in FIG.
It should be inhaled into 222 and sent to a liquid chromatograph analyzer or spectrophotometer for injection. Alternatively, the stirring device 18
After setting the sample container 24 in the container, the container transfer robot 24
When the grasping of the sample container 24 by 6 is released, the container transfer robot 246 is raised to the uppermost position by the robot elevating and lowering drive device, and the sample container 24 containing the sample liquid agitated by the agitation device 18 is moved by a not-shown transport mechanism. Alternatively, it may be carried out from the stirring device 18 manually. After that, the series of operations described above is repeated, and the dilution / stirring operation of the sample liquid is performed by the sample liquid 100 in each sample container 20.
Will be carried out in sequence.

The automatic pretreatment system for chemical analysis of the present invention has the above-mentioned structure, but the scope of the present invention is not limited by the above description and the contents of the drawings, and various modifications can be made without departing from the scope of the invention. Examples may be included. That is, the configuration of the filter unit setting device of the automatic filtering device section is not limited to that shown in the above-described embodiment, and the pair of block bodies of the filter take-out portion and the pair of block bodies of the filtering operation portion approach and separate from each other. The operation of does not necessarily need to be interlocked, and may be driven separately, or the filter unit is accommodated in the filter stocker in the upside-down direction, the nozzle is formed in the lower flow path connector, On the other hand, the upper channel connector has the same structure as the liquid feeding member in the above-mentioned embodiment, and the sample liquid is caused to flow from the lower channel connector to the upper channel connector through the filter unit, and the used filter unit is moved downward. The flow path connector may be detached from the flow path connector, or the used filter unit may be removed from the flow path connector. The structure of the withdrawal means for separating is not limited to that of the above-mentioned embodiment, and various mechanisms can be adopted, and further, in the above-mentioned device of the embodiment, the lower flow path connector is horizontally and vertically arranged. Although it is movably supported, the lower flow path connector may be fixed, while the filter stocker and the upper flow path connector may be movably supported. In addition to the mechanism of the above-described embodiment, various structures can be adopted as the configuration of the container transfer robot, its lifting drive device, nozzle lifting drive device, horizontal movement mechanism, and the like.

[0036]

Since the present invention is constructed and operates as described above, chemical analysis such as filtration of sample liquid, dilution of filtered sample liquid, transfer of containers and agitation using the apparatus according to the present invention. When performing a series of pretreatment operations, the time required for the pretreatment operations can be shortened to improve the work efficiency, and no manpower is required at all. Further, according to the present invention, simplification of the device configuration and drive / control mechanism and space saving of the entire device can be achieved.

[Brief description of drawings]

FIG. 1 is a side view showing an overall configuration of an automatic pretreatment system for chemical analysis according to an embodiment of the present invention, with a side cover removed.

FIG. 2 is likewise a front view with the front cover removed.

FIG. 3 is likewise an external perspective view.

FIG. 4 is a perspective view showing a partially broken configuration of a main part of an automatic filtering device portion that constitutes a part of the automatic pretreatment device.

FIG. 5 is a partial perspective view showing an example of a drive mechanism in the automatic filtration device section.

FIG. 6 is a diagram schematically showing a configuration of a main part of an automatic filtration device unit and a flow channel configuration thereof.

FIG. 7 is a perspective view showing a partially broken state of a main part of an automatic diluting / container transferring device that constitutes a part of the automatic pretreatment device.

FIG. 8 is a sectional view schematically showing a schematic configuration of a flow path of an automatic dilution / container transfer device section.

FIG. 9 is a perspective view showing an example of a filter unit used when a sample liquid is filtered by an automatic filtering device section.

[Explanation of symbols]

 2 Filter unit 6, 8 Connection port 10 Automatic filtration device part 12 Dispensing part 14 Container storage part 16 Automatic dilution / container transfer device part 18 Stirrer device 20 Sample container 22 Sample container rack 24 Sample container 26 Sample container rack 100 Filtered sample Liquid 110 Filter storage section 112 Filter removal section 114 Filtration operation section 116 Filter stocker 118, 120, 134, 136 Block body 122 Bearing / removing claws 124, 140 Recesses 126, 130 Bearing surfaces 128, 132, 142, 144 Cam surface 138 Detaching Claw 146 Upper flow path connector 166 Liquid supply tube 174 Lower flow path connector 178 Lifting member 180 Liquid feeding member 190 Lifting drive mechanism 196 Drainage tube 202 Discharge nozzle 210 Dilution nozzle device 212 Container gripping device 214 Horizontal movement holding plate 216 Horizontal Moving mechanism 222 Diluting nozzle 224 Nozzle holding part 228 Guide rail 232 Nozzle drive shaft 236 Nozzle lifting drive motor 242 Lifting drive shaft 246 Container transfer robot 248 Grasping arm 256 Robot lifting drive motor 278 Syringe for measuring sample liquid 280 Syringe for measuring pure water 282 Flow path switching valve 290 Pure water

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Noboru Nakatani No.8 Kamigatanaji, Nagaokakyo, Kyoto Prefecture Daini Seiki Co., Ltd. (72) Kunio Ikejo, No.8 Shinjitanashi, Nagaokakyo, Kyoto Dainihon Co., Ltd. Inside the Seiki (72) Inventor Hiroshi Yanagi 8th Kamiashidana, Nagaokakyo, Kyoto Prefecture Dainippon Seiki Co., Ltd.

Claims (2)

[Claims] 1. A plurality of filter units each having a filter material housed in a package having connection ports formed on the upper side and the lower side, respectively, are housed in a vertically stacked state, and a lower end opening surface is taken out. A cylindrical filter stocker having a mouth, and one of the connection ports of the filter unit, which is sequentially supplied one by one from the outlet of the filter stocker, is connected to a liquid supply tube connected to a sample liquid supply source. , A filter unit setting device for connecting the other to the drainage tube so that they can be inserted and removed freely, and the drainage tube is connected for communication, and flows into the filter unit from the sample liquid supply source through the liquid feed tube and the filter The sample volume that has been filtered while flowing through the unit and flows out into the drain tube is added to the sample volume. An automatic filtering device section consisting of a sample liquid dispensing device having a discharge nozzle for discharging into a container, a sample container rack for storing a plurality of the sample containers in parallel, and a sample container rack for storing a plurality of sample containers in parallel And a flow path connection to a diluent supply source, while sucking the filtered sample liquid contained in the sample container housed in the sample container rack from the lower end port, and the sucked sample liquid together with the diluent from the lower end port. A dilution nozzle that discharges into the sample container stored in the sample container rack, suction of the sample liquid into the dilution nozzle, feeding of the dilution liquid from the diluent supply source to the dilution nozzle, and inside the sample container from the dilution nozzle. Syringe and flow path switching valve for driving and controlling each operation of discharging sample liquid and diluting liquid to and holding the diluting nozzle reciprocally in the vertical direction The movable holding body,
It is held on this movable holder so that it can move back and forth in the vertical direction.
Of the sample containers stored in the sample container rack, a container gripping device having a gripping arm that detachably grips the sample container located immediately below the dilution nozzle, and the container gripping device and the dilution nozzle reciprocate vertically. An automatic diluting / container transfer device section including a gripping arm elevating mechanism and a nozzle elevating mechanism to be moved, and an X / Y direction moving mechanism to move the movable holder in the X and Y directions, respectively, and movement of the container grasping device. An automatic pretreatment device for chemical analysis, which is provided within a possible range and comprises a stirrer for rocking the sample container to stir and mix the sample liquid and the diluent contained therein. 2. A filter unit setting device is disposed below the filter stocker, moves horizontally to and from the outlet, and is located at the lowest position in the filter stocker when it advances to the outlet. A support member for supporting the unit, a drive device for driving the support member, and a filter stocker, which is disposed adjacent to the liquid supply tube or the drain tube and is connected to the lower end of the filter unit above the connection port. And an upper flow path connector having an insertion port connected to and communicated with the upper flow path connector and the filter stocker, which are arranged below the upper flow path connector and the filter stocker in the vertical and horizontal directions. Each of them is supported so as to be reciprocally movable relative to each other, and a drainage tube or a liquid supply tube is connected to The filter unit has an insertion port that is connected to the lower connection port of the filter unit, and one filter unit is sequentially taken out from the ejection port of the filter stocker, and the insertion port is communicated with the lower connection port of the filter unit. A lower flow path connector that is supported in a connected state, each driving means that relatively moves the lower flow path connector, the upper flow path connector, and the filter stocker in the vertical direction and the horizontal direction, respectively. A removal means for detaching the filter unit in a state in which the upper side or the lower side connection port is engaged with the insertion port and is supported from the upper flow path connector or the lower flow path connector. Item 1. An automatic pretreatment device for chemical analysis according to item 1.