Chemical apparatus and process disinfecting – deodorizing – preser – Analyzer – structured indicator – or manipulative laboratory... – Sample mechanical transport means in or for automated...
Reexamination Certificate
1998-06-26
2004-01-06
Warden, Jill (Department: 1743)
Chemical apparatus and process disinfecting, deodorizing, preser
Analyzer, structured indicator, or manipulative laboratory...
Sample mechanical transport means in or for automated...
C422S065000, C422S105000, C422S130000
Reexamination Certificate
active
06673316
ABSTRACT:
TECHNICAL FIELD
The present invention relates to a synthesis experiment automation system for automating chemical synthesis experiments, and to a liquid level/interface position detecting device, a separation processing device, and a reaction container, which are suitable for use in the synthesis experiment automation system.
BACKGROUND ART
In the past, various automated experiment devices have been developed in order to increase the efficiency of chemical experiments and reduce the effort involved therein.
Automated experiment devices of this kind can be broadly divided into, for example, (1) devices which control reaction conditions by, for example, controlling temperature, pressure, flow, etc., precision measuring of heat balance, and analyzing reaction parameters; (2) sequential devices for synthesizing samples of small quantity by performing synthesis, post-processing, refinement, etc.; and (3) devices which use a robot to perform synthesis, post-processing, and analysis.
Specific examples of these kinds of automated experiment devices are (I) synthesis reaction devices such as those disclosed in Japanese Unexamined Patent Publication Nos. 1-249135/1989 (Tokukaihei 1-249135), 2-2870/1990 (Tokukaihei 2-2870), 6-63389/1994 (Tokukaihei 6-63389), and 6-79166/1994 (Tokukaihei 6-79166); (II) automated synthesis devices such as the Contalab (manufactured by Mettler Co.) and the ARS (manufactured by Sogo Chemical Industries Co., Ltd.); and (III) the synthesis experiment device CombiTec (manufactured by Tecan Co.), which uses a robot.
However, the synthesis reaction devices in (I) above are integral sequence control devices, which conduct a reaction in a single location by introducing reagents, solvents, etc. into a pre-set reaction container. For this reason, with these devices, the system has little flexibility or extendibility, and since the location of the reaction is limited, it is difficult to conduct several reactions simultaneously or freely rearrange the reaction process.
Again, the automated synthesis devices in, (II) above can only perform a single reaction in a single reaction device, and thus have the drawback that only one reaction can be conducted at a time.
Since the synthesis experiment device in (III) above uses a robot, it has more extendibility than the devices in (I) or (II), but since the number of possible experiment unit operations is small, it is unable to perform complex synthesis experiments which combine a plurality of unit operations.
In each of the foregoing conventional automated devices, a machine performs operations formerly performed by humans. However, these conventional automated devices have several problems, such as inability to perform several experiments simultaneously, a limited number of reagents which can be supplied automatically, a narrow reaction temperature range, a limited number of possible experiment unit operations, difficulty of improvement or extension of the device, etc. Accordingly, these conventional automated devices cannot be said to have dramatically reduced the effort or improved the efficiency of chemical experiments.
Further, with organic synthesis reactions, there are many cases in which the reaction produces a solution phase made up of at least two incompatible solutions. In such a case, the desired compound must be separated out from the reaction container.
With this kind of solution phase made up of two incompatible solutions which have separated into layers, separation processing to separate out each solution is often carried out in extraction processing, in which a desired compound is separated out from a reaction liquid obtained by, for example, an organic synthesis reaction. A separation funnel is often used for this separation processing.
In separation processing using a separation funnel, the operator separates the two solutions by, first, visually checking the liquid level of the solution phase which has separated into layers and the interface between the two solution layers, and then, in accordance with the liquid level and interface, extracting from the separation funnel one of the solutions of the solution phase, after which, as necessary, the other solution remaining in the separation funnel may be extracted into another container.
However, in using a separation funnel to separate out each solution from this kind of solution phase made up of two incompatible solutions which have separated into layers, the operator must check the positions of the liquid level of the solution phase and the interface between the two solutions, as well as perform the operations for separating out each solution.
Accordingly, in conventional separation processing using a separation funnel, since the separation processing itself is carried out by the operator, the operator must be used to operating with a separation funnel in order to perform the separation processing correctly. In other words, if the operator is not used to operating with a separation funnel, when the difference in color of the two solutions in the solution phase is subtle, it is difficult to correctly distinguish the interface, and the operator may not be able to correctly separate out the solutions of the solution phase.
Since the operations of the above-mentioned separation funnel are manual, it has been difficult to use in conventional devices which perform organic synthesis reactions automatically, and this has made automation of organic synthesis reactions difficult.
In conventional chemical experiments, when allowing two or more reagents to react in a reflux, reaction containers like that shown in
FIG. 39
have been used (see Experimental Chemistry Lectures 2: Basic Operations II, 4th Ed., Maruzen Co., Ltd.).
The reaction container shown in
FIG. 39
is made up of a flask
511
which contains a reagent C, a drip funnel
512
which contains a reagent D, a condenser
513
, and a stirrer
514
.
A reaction between the reagents C and D is conducted by dripping the reagent D from the drip funnel
512
into the flask
511
which contains the reagent C. This kind of reaction is often conducted with the application of heat, and reaction raw materials, reaction products, and reaction solvent vaporized by heating are cooled by the condenser
513
, and are thus liquefied and returned to the flask
511
. Further, in order to stabilize the reaction, stirring is usually performed using the stirrer
514
.
In addition, this kind of reaction is usually performed with the reaction system sealed under open pressure by means of a filling tube filled with drying agent, etc. and attached to the top of the condenser
513
.
In this way, in conventional reaction containers, the drip funnel
512
, which is a reagent introducing member, the condenser
513
, which is a cooling member, and the sealing member (not shown) were provided separately from the flask
511
.
However, since the reagent introducing member, cooling member, and sealing member are provided separately, disadvantages of this kind of conventional reaction container are that the size of the container as a whole in increased, and that assembly of the container is troublesome.
Because of these problems, it has been difficult to use the above-mentioned conventional reaction container in conventional devices which perform organic synthesis reactions automatically, and this has made automation of organic synthesis reactions difficult.
DISCLOSURE OF THE INVENTION
The object of the present invention is to provide a synthesis experiment automation system which is capable of simultaneously performing a plurality of different experiments as complex as those usually performed by researchers, which has a large number of possible experiment operations, and which can be easily improved and/or extended.
Another object of the present invention is to provide a separation processing device which automatically detects a liquid level position and an interface position in a solution phase made up of two incompatible solutions which have separated into layers, and which automatically performs solution extraction operations based on the d
Deuchi Kouji
Hirata Norihiko
Kawata Yasuharu
Koike Toshio
Murata Hirokazu
Fitch Even Tabin & Flannery
Sumitomo Chemical Co,. Ltd.
Warden Jill
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