JP2996174B2 - Automatic pretreatment method and apparatus - 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 method and apparatus for an automatic sample introduction (injection) device of an analyzer (gas chromatograph, mass spectrometer, etc.). The present invention relates to an automatic pretreatment method and apparatus used in a thermal desorption tube sampler (sample supply device) and the like.

[0002]

2. Description of the Related Art As shown in FIG. 3A, a thermal desorption method, which is a kind of pretreatment method for a sample, is used as a tube.
The container 4 is filled with an adsorbent M, for example, a small amount of sample present in the atmosphere is adsorbed by the adsorbent M, and caps 4a, 4a are stored on both sides for storage.
(See FIG. 1), and the resulting mixture is introduced into an analyzer such as a gas chromatograph (GC) or a mass spectrometer (GC-MS) for analysis. Conventionally, when a sample is taken out from a large number of tube-shaped containers 4 filled with the sample, as shown in FIG. 3B, a large number of tube-shaped containers 4, 4,. In addition, the method of changing while rotating was adopted. In addition, such a service
At present, in the maldesorption method, a method of exchanging a tube containing a sample using a robot hand such as a manipulator is not known.

[0003]

When a large number of tube-shaped containers filled with samples are introduced into an analyzer using a manipulator, the tubes can be set on a tray and transported. And the area is large
Therefore, there is a problem that the entire device becomes large because the operating range of the data becomes large. The area of the tray can be reduced by stacking the tube-shaped containers 4 in multiple stages. However, in the operation of returning the sample container 4 after the analysis and introduction to the original position, the tube with the sample set in the lower position is set. There is a problem that the container cannot be removed.

The present invention has been made in view of the above-mentioned problems, and when pretreating a sample, the area of the tray is reduced and the number of tubes is reduced even if tube-like containers are stacked in multiple stages. It is an object of the present invention to provide an automatic pretreatment method and apparatus capable of treating a container in the form of a container.

That is, in order to solve the above-mentioned problems, the present invention provides an automatic pretreatment method in which a plurality of racks capable of setting tube-shaped sample containers in multiple stages around a column are arranged and a part thereof is provided. Is an empty rack, and is equipped with a gripper having a gripper having a function of holding and releasing the tube-shaped sample container. The arm can be moved up and down, and can be rotated in any direction. Thus, the tube-shaped sample containers set in the multi-stage are picked up and set in the sample processing unit, and all or a part of the processed tube-shaped sample containers are temporarily stored in the empty rack of the part. And then returning the treated tube-shaped sample container to the original rack via the empty rack or directly.

[0006] Alternatively, an automatic pretreatment device is arranged around a column, a plurality of racks capable of setting a plurality of tube-shaped sample containers and a partially empty rack, and the tube-shaped sample container. A gripper having a gripper having a gripping / opening function at an end thereof, an arm capable of moving up and down, and being rotatable in any direction; A sample processing unit provided with a cap-shaped sample container cap attaching / detaching device, a sample feeding means in the tube-shaped sample container, a rotating operation of the manipulator, an up-and-down moving operation of the arm, and a gripper for gripper. And an arithmetic processing unit for controlling the opening operation.

[0007]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1A shows an automatic pretreatment device 1, a sample concentrating device 2, and an analysis device (a sample pretreatment device) for carrying out a method for treating a tube for thermal desorption, which is a kind of an automatic sample pretreatment method of the present invention. FIG. 1 is a front view showing a configuration of a gas chromatograph, a mass spectrometer 3), and FIG.
(B) is a plan view of the automatic pretreatment device 1. That is, in the automatic pretreatment device 1, a large number of tube-shaped sample containers 4 each of which has taken a sample and sealed with caps 4a and 4a for maintaining airtightness are arranged. The sample is further concentrated in the sample concentrator 2, from which it is introduced into the analyzer 3 by a carrier gas.

FIG. 2A is a front view of the automatic pretreatment device 1 and FIG. 2B is a plan view thereof. A plurality of racks 6 (6A, 6B,...) Surround a cylindrical portion (which may be a prism instead of a cylinder) 5 constituting the automatic pretreatment device 1.
・) Is arranged. In the embodiment, the racks 6 (6A, 6B,...) Are formed at a central angle of 60 degrees. However, the number of racks 6 can be increased or decreased. On these racks 6, tube-like containers 4 filled with samples radially are set in two stages. Each of the racks 6A, 6B,... Has fixed plates 7, 7,. , And the gaps 9, 9,... Between the fixed plates 7 and the fixed plates 7 (the fixed plates 8 and 8) are provided in the main body 4 of the tube-shaped sample container 4.
It is set so as to sandwich part b. In the embodiment shown in the figure, five sets of tube-like containers 4 set in two stages on one rack 6A are arranged. Of course, the number and the number of stages can be increased and decreased, and the rack 6A and the like need not have a central angle of 60 degrees.

A manipulator 10, which is rotatably supported in both left and right directions, is installed on a central column portion 5 in which the racks 6 (6A, 6B,...) Are arranged. I have. A gripper 12 capable of holding and releasing the tube-shaped sample container 4 is attached to the tip of the manipulator 10. The manipulator 1
The arm 11 to which the zero gripper 12 is attached can be moved back and forth and up and down by a driving device. The operation of rotating the manipulator 10, moving the arm 11 back and forth, moving up and down, and gripping and opening the tube-shaped container 4 by the gripper 12 are performed by an arithmetic processing unit (CPU) (not shown).

A sample processing unit 13 provided with a sample sending means in the tube-shaped sample container 4 is disposed on a part of the column 5. That is, the tube-shaped sample containers 4 picked up one by one by the manipulator 10 are first fixed to the fixing tables 14, 14 provided in the processing unit 13, and the cap 4a is removed by the cap removing device 15, Next, the main body 4b is moved to another fixed base 16, 16 on the same unit 13, and both sides of the main body 4b of the tube-shaped container 4 are set and inserted into the tube joint connecting devices 17, 18 to suction the inside. The sample adsorbed on the agent M (see FIG. 3 (A)) is subjected to a carrier concentration by the sample concentrating device
To be sent out. The processing unit 13 is provided with a heating block 21 for heating the tube-shaped sample container 4 when removing a sample.

The processing unit 13 has fixed bases 14, 1 on which a main body 4b is set to remove the cap 4a.
4 and fixed bases 16, 16 on which the main body 4b is set in order to send out a sample are separately installed. Therefore, the heating block 21 is placed on the opposite side (end side) because of the double labor.
If the fixed bases 14 and 14 are configured to be movable to the positions of the tube joint connecting devices 17 and 18, the fixed bases 16 and 16 become unnecessary.

Next, the rack 6 (6A, 6B,...) Has an empty rack 6 (for example, one rack 6E may be used) in which the tube-shaped sample container 4 is not set in one of the racks. Are located. When all of the upper stage of the tube-shaped sample container 4 set in the rack 6A is processed, the tube-shaped sample container 4 is temporarily set in the rack 6E. When the lower stage of the tube-shaped sample container 4 of the rack 6A is processed, the rack 6A is processed. The operation of returning to the lower stage, and then returning the processed tube-shaped sample container 4 placed in the empty rack 6E to the original upper position is repeated for each rack. I do.

The automatic preprocessing apparatus of the present invention has the above-described configuration. Next, the specific operation will be described. (1) First, of the tube-shaped sample containers 4 set in two stages on the rack 6A, the upper container 4 is gripped by the gripper 12 of the manipulator 10 and picked up, and the fixing table of the sample processing unit 13 is fixed. 14, and the cap attaching / detaching devices 15, 15 are used to set the caps 4 a,
Remove 4a. (2) Next, the main body 4 of the tube-shaped sample container 4 with the caps 4a, 4a removed by the gripper 12 of the manipulator 10.
b to the fixed bases 16, 16 of the sample processing unit 13,
The two sides of the main body 4b are connected to a tube joint connecting device 17,
The sample in the tube-shaped sample container 4 is sent out to the concentrating device 2 while being set at 18 and heated by the heating block 21. (3) The tube-shaped sample container 4 after sending out the sample is
The main body 4b is returned to the fixed bases 14, 14, and the caps 4a, 4a are again put on by the cap attaching / detaching device 15, then gripped by the gripper 12 of the manipulator 10, and temporarily moved to the empty rack 6E. (4) When the processing of the upper tube-shaped sample container 4 set in the rack 6A is completed, the operations (1) and (2) are performed on the lower tube-shaped sample container 4 of the rack 6A. .
When the processing of the lower tube-shaped sample containers 4 is completed, these tube-shaped sample containers 4 are re-capped on the main body 4b thereof by the cap attaching / detaching device 15, and then directly into the rack 6A. Return to the bottom. (5) Next, the upper tube-shaped sample container 4 temporarily moved to the rack 6E is returned to the upper stage of the rack 6A. (6) The above operations (1) to (5) are performed by the following racks 6A,
6B,... Is performed on the tube-shaped sample container 4 set in.

In the above embodiment, the empty rack 6
In E, the tube-shaped sample containers 4 can be installed in multiple stages, and when the processing of all the upper tube-shaped sample containers 4 of the other racks 6A, 6B,. It is temporarily set on the rack 6E, and the racks 6A, 6
B,... After the processing of the lower tube-shaped sample container 4 is completed, the racks 6A, 6B,.
Thereafter, the processed tube-shaped sample container 4 temporarily placed in the rack 6E may be returned to the racks 6A, 6B,.

Alternatively, the tube-shaped sample containers 4 set in the rack 6A are stacked on the empty rack 6E until the processing is completed, and when the processing of all the tube-shaped containers 4 in the rack 6A is completed, Next, the rack 6E on which the tube-shaped container 4 processed by the manipulator 10 is placed.
May be returned to the original rack 6A in turn. That is, the tube-shaped sample container 4 is connected to the manipulator 1.
0, the processing is started from one rack 6A, and when this is completed, the processing is sequentially performed on the next rack 6B and the tube-shaped container 4 is returned. The tube-shaped container 4 can be processed.

As a modified embodiment of the present invention,
A rack 6 for setting tube-shaped sample containers 4 separately around the racks 6 (6A, 6B,...) And within a position where the arm 11 of the manipulator 10 can reach.
W may be arranged. That is, the upper tube-shaped sample containers 4 stacked and processed in two stages on the rack 6A or the like are sequentially placed on the rack 6W, and when the processing of the upper tube-shaped containers 4 is completed, the lower tube-shaped sample containers 4 are processed. The tube-shaped container 4 is processed, and the lower tube-shaped container 4 after the processing is processed by the rack 6A.
When the processing of the lower tube-shaped container 4 is completed, the upper processed tube-shaped container 4 placed in the separately installed rack 6W is returned to the original rack 6.
A method of returning to the upper stage of A may be used. In the above embodiment, the tube-shaped container 4 is placed in the rack 6 (6A, 6A).
B,...), The number of stages may be further increased.

[0017]

As described above in detail, according to the automatic pretreatment method and apparatus of the present invention, a rack or a place in which a tube-shaped sample container is not set is provided, and the seal shown in the embodiment is provided.
By performing the cans control, it is possible to process containers set in multiple stages in one rack. In addition, since the processing can be performed efficiently by reducing the area of the tray or the installation place, the entire apparatus can be downsized.

[Brief description of the drawings]

FIG. 1A is a front view showing a configuration of an automatic pretreatment device, a sample concentration device, and an analyzer for carrying out the automatic pretreatment method of the present invention, and FIG. It is a top view of a processing apparatus.

FIG. 2A is a front view of an automatic pretreatment device,
FIG. 2B is a plan view thereof.

FIG. 3A is an external view of a tube-shaped sample container, and FIG. 3B is an example of a drum-shaped rack for setting a conventional tube-shaped sample container.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Automatic pre-processing apparatus 2 Sample concentrating apparatus 3 Analyzer 4 Tube-shaped sample container 5 Column 6 (6A, 6B, ...) Rack 6E Rack (empty rack) 6W Rack (outside empty rack) 7, 8 Fixing plate 10 Manipulator 11 Arm 12 Gripper 13 Processing unit 21 Heating block

Claims (2)

(57) [Claims] 1. A plurality of racks capable of setting tube-shaped sample containers in multiple stages around a column and a part of the racks being empty racks, and a function of holding and opening the tube-shaped sample containers. The multi-stage set of tube-shaped sample containers is picked up by a manipulator equipped with a gripper having a gripper having a fore-and-aft vertical movement and rotatable in any direction. Set in a processing unit, temporarily or temporarily place all or a part of the processed tube-shaped sample container in the empty rack of the part, and then place the processed tube-shaped sample container in the empty space. An automatic pretreatment method characterized by returning to an original rack via a rack or directly. 2. A plurality of racks which are arranged around a column, on which tube-shaped sample containers can be set in multiple stages, and a partially empty rack, and a gripping / opening function of said tube-shaped sample containers. A manipulator mounted on the column, equipped with an arm having a gripper at its end and capable of moving up and down and up and down, and being rotatable in any direction; An automatic preprocessing device comprising: a sample processing unit having a sample sending means; and an arithmetic processing device for controlling the rotating operation of the manipulator, the forward / backward vertical moving operation of the arm, and the gripper gripping / opening operation. .