JP2000189706A - Automatic concentration device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an automatic concentration device enabling to automatically feed a sample liquid to be concentrated, and automatically discharge a solvent taken out with a concentration operation from the storage tank. SOLUTION: In this automatic concentration device, the weight of the sample liquid in a flask 14 is monitored, and the weight of a storage tank 4 of the sample liquid for storing the sample liquid to be condensed, is monitored, and also respective weights of a plurality of solvent storage tanks 9A, (9B) for storing the solvent taken out with the concentration operation are monitored, and the sample liquid is automatically fed from the storage tank 4 of the sample liquid into the flask 14 when the condensing sample liquid is shortened, and a flow path can be automatically switched so as to allow the solvent to flow into another solvent storage tank 9B when the storage tank 9A of the solvent is fulfilled.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic concentrator, and more particularly, to an automatic concentrator in which a rotary evaporator automates the charging of a sample solution into a flask and the removal of a solvent.

[0002]

2. Description of the Related Art Conventionally, as an industrial-scale concentrator, 1
There is a rotary evaporator provided with a flask having an inner volume of 0 liter or more. The rotary evaporator includes a flask, a rotation driving device for rotating the flask, a heating device for heating a sample solution in the flask, a sample solution storage tank for supplying a sample solution in the flask, A cooling device that cools and condenses the solvent evaporated from the sample liquid, a decompression device that decompresses the inside of the flask, and a solvent storage tank that stores the solvent condensed by the cooling device.

In this rotary evaporator,
During the process of concentrating the sample liquid in the flask, the sample liquid is added to the flask.If the amount of the remaining sample liquid in the sample liquid storage tank for adding the sample liquid decreases, the concentration of the sample liquid in the flask will increase. Even if not completely achieved, the operation of the rotary evaporator was once stopped, the sample liquid was added to the sample liquid storage tank, and the operation of the rotary evaporator was restarted. When the storage tank is full, the operation of the rotary evaporator is temporarily stopped even at this time,
Replace the full solvent storage tank with an empty solvent storage tank,
Thereafter, the operation of the rotary evaporator was restarted.
As described above, in the conventional rotary evaporator, the operation of the rotary evaporator often needs to be temporarily stopped in order to replenish the sample liquid in the sample liquid storage tank and to extract the solvent in the solvent storage tank. There is a problem that efficient concentration cannot be performed.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to solve the above problems. An object of the present invention is to automatically inject a sample solution into a flask in a rotary evaporator, and furthermore, when the sample solution to be added does not run out, and when the solvent reservoir is full, the solvent reservoir is automatically emptied. Accordingly, it is an object of the present invention to provide an automatic concentrator that can be automatically operated almost unattended.

[0005]

According to the present invention, there is provided a rotary evaporator having a rotatable flask capable of storing a sample liquid, and a method for measuring the weight of the rotary evaporator. 1, a sample liquid storage tank for storing a sample liquid to be supplied into the flask, and the sample liquid storage tank when the weight of the rotary evaporator measured by the first weight measuring apparatus reaches a predetermined value. First sample liquid transfer means for transferring a sample liquid from the tank into the flask, a second weight measuring device for measuring the weight of the sample liquid storage tank, and a preliminary sample liquid storage tank for storing the sample liquid; When the weight of the sample liquid storage tank measured by the second weight measuring device reaches a predetermined value, a second sample liquid transfer means for transferring the sample liquid in the preliminary sample liquid storage tank to the sample liquid storage tank. A plurality of solvent storage tanks for storing the solvent evaporated and recovered from the sample liquid in the flask, a third weight measuring device for measuring the weight of each of the plurality of solvent storage tanks, and a sample in the flask. Third solvent transfer means disposed so as to transfer the solvent evaporated from the liquid, cooled and liquefied to the plurality of solvent storage tanks, and the third solvent transfer means in a specific solvent storage tank in the plurality of solvent storage tanks. When the solvent evaporated / recovered from the sample liquid in the flask is transferred through the solvent transfer means, the weight of the specific solvent storage tank measured by the third weighing device is a predetermined value. Flow rate switching means for switching the flow path so that the solvent evaporated / recovered from the sample liquid in the flask flows from the specific solvent storage tank to another solvent storage tank when the value reaches the value. Is characterized by That is an automatic concentrator.

[0006]

DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 is an explanatory view showing one specific example of an automatic concentration device according to the present invention.

[0007] As shown in FIG.
Are a rotary evaporator main body 2, a first weighing device 3, a sample liquid storage tank 4, and a first sample liquid transfer means 5.
A second weight measuring device 6, a preliminary sample liquid storage tank 7,
A second sample liquid transfer means 8, two solvent storage tanks 9, a third weighing device 10, a third solvent transfer means 11,
It comprises a flow path switching means 12, a control means 13, an input means such as a keyboard (not shown), and a display device such as a liquid crystal display screen (not shown).

The rotary evaporator main body 2 evaporates the solvent present in the sample liquid supplied to the inside of the rotating flask 14, cools the evaporated solvent to condense it, and discharges the liquefied solvent out of the system. It has a function to do. Evaporation of the solvent is carried out at normal pressure or reduced pressure, at heating or at normal temperature.

As a specific example, the rotary evaporator main body 2 includes a rotatable flask 14, a rotary drive unit for rotating the flask 14, such as a motor M and a speed reducer, and the contents of the flask 14. Heating means, for example, a water bath 15, an introduction pipe 16 for introducing a sample solution into the flask 14, and a cooling means 17, for cooling a solvent evaporated from the sample solution in the flask 14, for example, the inside of a cylindrical tube. A cooling device provided with a cooling snake tube through which cooling water passes, a discharge port 18 for discharging the solvent cooled by the cooling means 17 to the outside of the system, and the pressure in the system including the flask 14 and the cooling means 17 are reduced. An exhaust means, for example, an exhaust pump P 1 is provided, and these are attached to a support 20 erected on a base 19.

The first weight measuring device 3 has a function of measuring the weight of the rotary evaporator main body 2 and outputting an electric signal indicating the weight value.

In this example, a base 19 of the rotary evaporator main body 2 is mounted on the first weight measuring device 3. From the first weight measuring device 3, an electric signal indicating the weight of the rotary evaporator body 2 is continuously output to the control means 13 described later. As the first weight measuring device 3, for example, a weight measuring device using a load cell can be cited.

The sample liquid storage tank 4 is provided with the flask 14.
This is a tank for storing the sample liquid supplied to the tank. The sample liquid storage tank 4 can be composed of, for example, a metal tank, a glass container, or the like.

The first sample liquid transfer means 5 includes the first sample liquid transfer means 5.
When the weight of the rotary evaporator body 2 measured by the weight measuring device 3 reaches a predetermined value, the sample liquid storage tank 4
And a means for transferring the sample liquid into the flask 14. In the example shown in FIG. 1, the first sample liquid transfer means 5 includes a pipe connecting the sample liquid storage tank 4 to the end of the introduction pipe 16 in the rotary evaporator main body 2, and an interposition between the pipe. And a first opening / closing valve 21 provided. Since the inside of the flask 14 in the rotary evaporator main body 2 is usually depressurized, when the first opening / closing valve 21 is opened, the sample liquid in the sample liquid storage tank 4 is immediately passed through the pipe due to a pressure difference, and the flask is heated. 14 can be provided. The first opening / closing valve 21 performs an opening / closing operation in accordance with an operation command signal b output from the control means 13.

When the sample liquid in the flask 14 is concentrated while the inside of the flask 14 is at normal pressure, that is, in the case of a rotary evaporator of the normal pressure concentration type, the first opening / closing valve 21 is opened. Only sample storage tank 4
In such a case, it is preferable to interpose a liquid sending pump in the pipe because the sample liquid cannot move from the sample into the flask 14.

The second weight measuring device 6 is configured to measure the weight of the entire sample liquid storage tank 4 and to output an electric signal corresponding to the measurement result to the control means 13 with time. Therefore, the sample liquid storage tank 4 is placed on the second weight measuring device 6. In the example shown in FIG.
The second weight measuring device 6 can be configured using, for example, a load cell.

The reserve sample liquid storage tank 7 is a tank for storing a sample liquid to be concentrated, which is collected at various sites. Examples of the reserve sample liquid storage tank 7 include a metal or glass tank. This preliminary sample liquid storage tank 7 is appropriately replenished with the sample liquid conveyed from the site.

It is preferable to provide a liquid level checking means capable of indicating the liquid level so as to check how much the sample liquid is loaded in the preliminary sample liquid storage tank 7. As a liquid level checking means, a liquid level gauge may be installed in this preliminary sample liquid storage tank 7 or this preliminary sample liquid storage tank 7
On the wall of the, there is a vertically long observation window fitted with glass,
The inside may be visually observed. If the liquid level checking means is provided, the preliminary sample liquid storage tank 7 is provided.
It is possible to check the amount of the sample solution in the sample solution, and when it is determined that the amount of the sample solution is low, the sample solution can be replenished to the spare sample solution storage tank 7 at an appropriate time.
It is possible to prevent the sample solution from running out.

When the weight of the sample liquid storage tank 4 measured by the second weight measuring device 6 reaches a predetermined value, the second sample liquid transfer means 8 stores the sample liquid in the preliminary sample liquid storage tank 7. Is a means having a function of transferring the sample into the sample liquid storage tank 4. When the weight of the sample liquid storage tank 4 measured by the second weight measuring device 6 is a predetermined minimum value, the preferable second sample liquid transfer means 8 transfers the sample liquid in the preliminary sample liquid storage tank 7. When the weight of the sample liquid storage tank 4 measured by the second weighing device 6 reaches a predetermined maximum value, the sample liquid is stored in the preliminary sample liquid storage tank 7. This is a means having a function of stopping the transfer of the sample into the tank 4.

As the second sample liquid transfer means 8, when the position of the preliminary sample liquid storage tank 7 is higher than the position of the sample liquid storage tank 4, for example, the preliminary sample liquid storage tank 7 and the sample liquid storage tank A pipe connecting the tank 4 and a second opening / closing valve 22 provided in the middle of the pipe,
When there is almost no height difference between the preliminary sample liquid storage tank 7 and the sample liquid storage tank 4, for example, a pipe connecting the preliminary sample liquid storage tank 7 and the sample liquid storage tank 4 and a second pipe provided in the middle of the pipe are provided. 2 and an on-off valve 22 and a liquid feed pump (not shown) provided in the middle of the pipe.
In the example shown in FIG. 1, a liquid feed pump (not shown) is interposed in the middle of the pipe. The second opening / closing valve 22 is provided with an operation command signal c output from the control unit 13.
Controls its operation.

Each of the two solvent storage tanks 9 is a tank for receiving and storing the solvent cooled and condensed by the cooling means 17 in the rotary evaporator body 2, and is made of metal or glass. The two solvent storage tanks 9 are respectively divided into a first solvent storage tank 9A and a second solvent storage tank 9A.
B.

In this automatic concentration apparatus, there is provided a solvent discharging means for discharging the solvent from the filled solvent storage tank in the two solvent storage tanks.

The solvent discharging means basically includes a discharge pipe attached to the solvent storage tank, a valve for opening and closing the discharge pipe, and a waste liquid pump for sucking and discharging the solvent in the solvent storage tank.

In the example shown in FIG. 1, the solvent discharging means is formed as follows. That is, the first discharge pipe 24 is attached to the first solvent storage tank 9A,
A second discharge pipe 25 is attached to the second solvent storage tank 9B. A first switching valve 23A is interposed in the middle of the first discharge pipe 24. In the middle of the second discharge pipe 25,
The second switching valve 23B is interposed. First discharge pipe 2
The fourth and second discharge pipes 25 are connected to a discharge main pipe 26. A discharge pump (not shown) for sucking and discharging the waste liquid is attached to the discharge main pipe 26. The first switching valve 1
The operation of the 2A and second switching valves 12B is controlled by inputting operation command signals da and db, which are control signals output from the control means 13.

In this embodiment, two solvent storage tanks 9 are provided. However, in the present invention, any number more than two may be used. The number of the solvent storage tanks 9 is determined according to the internal volume of the storage tank 9 and the like. In many cases, the number of solvent storage tanks 9 is two.

The automatic concentrator according to the present invention is not limited to the structure shown in Example 1, but includes a discharge pipe in which the solvent discharge means is connected to each solvent storage tank, and a discharge pipe for discharging the solvent in each solvent storage tank. It can also be formed by a pipe, and a switching valve that can be switched so as to be able to communicate with one of the pipes and the main pipe.

Two third weight measuring devices 10 are provided. Each of the two third weighing devices 10 will be referred to as a third first weighing device 10A and a third second weighing device 10B. Each of the third weight measuring devices 10 has a function of measuring the weight of each solvent storage tank 9 and outputting the measured value as an electric signal. Therefore,
For example, the first solvent storage tank 9A is placed on the third first weighing device 10A, and the third second weighing device 10B
The second solvent storage tank 9B is placed on the storage.

The third solvent transfer means 11 transfers the solvent cooled and condensed by the cooling means 17 in the rotary evaporator main body 2 from its outlet 18 to the first solvent storage tank 9A and the second solvent storage tank 9A. This is a transfer path for transferring to any of the tanks 9B, and is usually formed by piping.

When the automatic concentrator is of a reduced pressure evaporation type in which the pressure inside the flask 14 is reduced to evaporate the solvent,
The inside diameter of the pipe forming the transfer path is set to be sufficiently large so that a space in which the solvent flows and a space in which the gas in the solvent storage tank flows can be secured, or the transfer path is formed. When the pipe has an inner diameter enough to be closed by the solvent, a bypass may be provided between the solvent storage tank and the rotary evaporator main body so that the pressure in the solvent storage tank becomes approximately the same as the pressure in the flask.

The flow path switching means is one of a transfer path for sending the cooled and condensed solvent to the first solvent storage tank 9A and a transfer path for sending the solvent to the second solvent storage tank 9B. It has a function of switching to a flow path, and in this example, a flow path switching valve 12 is employed.

The flow path switching valve 12 includes (1) a flow path from the discharge port 18 in the rotary evaporator body 2 to the flow path switching valve 12 and a flow path from the flow path switching valve 12 to the first solvent storage tank 9A. Open the flow path,
A switching position X in which the flow path from the discharge port 18 to the flow path switching valve 12 and the flow path from the flow path switching valve 12 to the second solvent storage tank 9B are closed, (2) the discharge port 1
8 to the flow path switching valve 12 and the flow path from the flow path to the flow path switching valve 12 to the first solvent storage tank 9A are closed. A switching position Y for opening the flow path to the path switching valve 12 and the flow path from the flow path switching valve 12 to the second solvent storage tank 9B; and (3) switching this flow path from the discharge port 18. The flow path to the valve 12 and the flow path from the flow path switching valve 12 to the first solvent storage tank 9A are closed, and the flow path from the outlet 18 to the flow path switching valve 12 and the flow path The switching position Z can be set such that the flow path from the path switching valve 12 to the second solvent storage tank 9B is closed. In short, the flow path switching valve 12 allows the solvent to flow into the first solvent storage tank 9A at the switching position X, the solvent to flow into the second solvent storage tank 9B at the switching position Y, and the first solvent at the switching position X. The solvent is prevented from flowing into the storage tank 9A and the second solvent storage tank 9B. The flow path switching valve 12 is automatically controlled by an operation command signal a, which is a control signal output from the control means 13, so as to be in one of the switching positions.

Each of the first solvent storage tank 9A and the second solvent storage tank 9B is provided with a normal pressure return means and a pressure reducing means.

The means for returning to normal pressure is provided in the first solvent storage tank 9.
A means for recovering the reduced pressure state in the first storage tank 9A or the second solvent storage tank 9B to the normal pressure state when discharging the solvent stored in the first storage tank 9A or the second solvent storage tank 9B. .

Each of the first solvent storage tank 9A and the second solvent storage tank 9B includes an air introduction pipe provided in each solvent storage tank and an open / close valve interposed between the air introduction pipes.

In the automatic concentration apparatus as a whole, the normal pressure return means is, in this example, a first air introduction pipe 27 attached to the first solvent storage tank 9A, and a first air introduction pipe. 27, a second on-off valve 28 mounted on the second solvent storage tank 9B, and a second on-off valve 29 mounted on the middle of the second air introduction pipe 29. 2 opening / closing valve 30, and the first air introduction pipe 27 and the second air introduction pipe 29 are connected, and have, for example, a gas introduction main pipe 31 opened to the atmosphere or connected to a nitrogen cylinder. It is formed.

The first on-off valve 28 and the second on-off valve 3
0 is the operation command signal e output by the control means 13
The switching operation is controlled by a and eb.

The pressure reducing means comprises a first solvent storage tank 9A,
And means for setting the inside of the second solvent storage tank 9B to a predetermined degree of reduced pressure, for example, the same degree of reduced pressure as the inside of the flask 14.

As shown in FIG. 1, the pressure reducing means includes a first
First exhaust pipe 32 attached to the solvent storage tank 9A
A first opening / closing cock 33 interposed in the first exhaust pipe 32, a second exhaust pipe 34 attached to the second solvent storage tank 9B, and a second exhaust pipe 34. A second opening / closing cock 35 interposed in the middle of the first exhaust pipe 32 and an exhaust main pipe 36 connected to the first exhaust pipe 32 and the second exhaust pipe 34 and having an exhaust pump P2 interposed in the middle. Be prepared. The first open / close cock 33 and the second open / close cock 35
Operation command signal f output from control means 13
The operation is controlled by a and fb.

The control means 13 has a function of controlling the operation of the entire automatic concentration apparatus 1. In particular, the control means 13 judges the concentration state in the flask 14 and automatically stores the sample liquid in the flask 14 at a predetermined time. The opening / closing operation of the first opening / closing valve 21 is controlled so that the sample liquid can be charged, and when the sample liquid in the sample liquid storage tank 4 reaches a predetermined remaining amount, the sample liquid in the preliminary sample liquid storage tank 7 is changed to the sample liquid storage tank. 4 to control the operation of the liquid feed pump and the opening / closing operation of the second opening / closing valve 22,
The switching operation of the flow path switching valve 12 is controlled so that the solvent can be circulated to the solvent storage tank 9A or the solvent can be circulated to the second solvent storage tank 9B, and the first solvent storage tank 9A and When any one of the second solvent storage tanks 9B reaches a predetermined storage amount, the first solvent storage tank 9A and the second solvent storage tank 9B
And the first and second switching valves 23A, 23A so that the solvent can be discharged from one of the solvent storage tanks 9B.
B, a function of controlling the switching operation of the first and second on-off valves 28 and 30 and the first and second on-off cocks 33 and 35.

The control means 13 includes control operation means, storage means and the like. The control calculation means continuously receives, for example, an electric signal indicating the weight value of the rotary evaporator main body 2 output from the first weight measuring device 3 and reduces the weight of the rotary evaporator main body 2 at regular intervals. The rate is calculated, and it is determined whether or not the weight reduction rate has reached a predetermined threshold value, and it is determined whether or not the reduction rate calculated at regular time intervals has been repeated a predetermined number of times. The control means 13 further sends an operation command signal b as a control signal to the first opening / closing valve 21 when it is confirmed by the arithmetic means that the reduction rate reaching the predetermined threshold value has been repeated a predetermined number of times. Then, the first opening / closing valve 21 that has been normally closed is switched to the open state.

The control calculation means continues to measure the weight of the rotary evaporator body 2 output from the first weight measuring device 3 and determines whether the weight of the rotary evaporator body 2 reaches a preset maximum weight value. or it determines, when a set maximum weight value RW _{ma x} and the measured weight value RW is determined that match to within a predetermined threshold value, the operation command signal to the first on-off valve 21 was opened until it b, and has a control function of closing the first opening / closing valve 21.

When the weight of the sample liquid storage tank 4 output from the second weight measuring device 6 reaches a predetermined value, the control arithmetic means reads the sample from the preliminary sample liquid storage tank 7 into the sample liquid storage tank 4. When the sample liquid in the sample liquid storage tank 4 reaches a predetermined amount, the transfer of the sample liquid from the preliminary sample liquid storage tank 7 to the sample liquid storage tank 4 is stopped. It has a function to manage and control the amount of sample liquid.

More specifically, the control operation means sets the weight of the sample liquid storage tank 4 in a state where the minimum allowable amount of the sample liquid is contained therein as an allowable minimum weight value, Storage means for storing the weight of the sample liquid storage tank 4 in a state where a large amount of sample liquid is contained as an allowable maximum weight value;
The measured weight value indicated by the electric signal output from the second weight measuring device 6 is compared with the allowable minimum weight value (this comparison is usually a subtraction process) and measured as a calculation result. When it is determined that the weight value and the allowable minimum weight value are within a predetermined threshold value, an operation command signal c is output to the second opening / closing valve 22 to open the second opening / closing valve 22, and When the supply of the sample liquid from the reserve sample liquid storage tank 7 to the sample liquid storage tank 4 is started, the measured weight value output from the second weight measuring device 6 is compared with the allowable maximum weight value, and the calculation result is obtained. When it is determined that the measured weight value and the allowable maximum weight value are within a predetermined threshold value, an operation command signal c is output to the second opening / closing valve 22, and the second opening / closing valve 22 is closed. , The preliminary sample liquid storage tank 7
Has a function of stopping the supply of the sample liquid from the sample liquid into the sample liquid storage tank 4.

The control operation means evaporates the sample liquid in the flask 14 by the rotary evaporator body 2.
The collected solvent is distributed and stored in one solvent storage tank 9 of the two solvent storage tanks 9, and
First and second switching valves 23A and 23B, first and second opening / closing valves so that the solvent is discharged from the solvent storage tank 9 when the two solvent storage tanks 9 are filled with a predetermined amount of solvent. Valves 28, 30, first and second opening / closing cocks 33, 35,
In addition, it has a function of controlling the operation of each of the flow path switching valves 12.

More specifically, the control operation means includes, for example, an electric signal as a measured weight value output from the third first weight measuring device 3 for measuring the weight of the first solvent storage tank 9, An electric signal as a measured weight value output from the third second weight measuring device 6 that measures the weight of the solvent storage tank 9, and a first solvent storage tank 9A and a second solvent storage tank 9B. When comparing the measured weight value and the allowable maximum weight value read from the storage means for storing the allowable minimum weight value and the allowable maximum weight value and determining that the calculation result is within a predetermined threshold value The flow of the solvent into the solvent storage tank 9 relating to the measured weight value is stopped, and the solvent is discharged so as to flow into the other solvent storage tanks 9 and to discharge the solvent from the filled solvent storage tanks. 1
And second switching valves 23A and 23B, first and second on-off valves 28 and 30, first and second on-off cocks 33 and 3,
5, and a function of controlling the operation of each of the flow path switching valves 12.

The automatic concentrator 1 having the above configuration operates as follows. (1) Initial state As the initial state of the automatic concentrator 1, the flask 14, the third first solvent storage tank 9, the third second solvent storage tank 9, and the sample liquid storage tank incorporated in the rotary evaporator body 2 are used. 4 is empty, the preliminary sample liquid storage tank 7 is filled with the sample liquid, the first open / close valve 21 and the second open / close valve 22 are closed, and the first and second open / close valves 28, 3
0, first and second opening / closing cocks 28, 30, first and second cocks
Switching valves 23A and 23B and flow path switching valve 1
Assume that both of the two are in a closed state.

In this example, when the automatic concentration device 1 is activated by, for example, turning on a start switch, the control means 13 controls the first weight measurement device 3, the second weight measurement device 6, By inputting the weight measurement values output from the first and third weighing devices 10A and 10B, it is confirmed that the weighing device is in the initial state.
In the initial state, a lock signal is output to necessary parts so that the automatic concentrator 1 does not perform a runaway operation.
This is preferable because safe driving of the device can be realized.

To start the enrichment operation, for example, the operation start switch is turned ON to bring the operation state.

(2) State Confirmation Operation In the automatic concentrator 1 according to this specific example, when the operation state is set, first, the operation of confirming the state of each part is performed.

That is, the control calculation means determines whether or not the measured weight value output from the first weight measuring device 3 matches the set weight value of the rotary evaporator body 2 with the empty flask 14 loaded. Then, for example, when the measured weight value and the set weight value coincide with each other, a warning display is not particularly displayed on a display portion displaying, for example, "flask" on the liquid crystal display screen, while the measured weight value is larger than the set weight value. When it is determined that the size is large, a warning display, for example, "The flask in the previous concentration operation remains." Appears on the display portion displaying, for example, "flask" on the liquid crystal display screen. The operator can surely attach the empty flask 14 to the rotary evaporator main body 2 by seeing such a warning display, and eliminates the inconvenience of mistakenly using the flask which was used in the previous concentration operation and was forgotten to be removed. Is done.

Further, the control calculation means for inputting the measured weight value output from the third first weight measuring device 10A confirms that the first solvent storage tank 9A has the maximum allowable weight value, and at the same time, determines whether the first solvent storage tank 9A has the maximum allowable weight value. When the path switching valve 12 is switched to the switching position X
If it is confirmed that the solvent is left in the first solvent storage tank 9A in the previous concentration operation, the liquid crystal display screen displays, for example, "The first solvent storage tank 9A is full." Is displayed, the switching position of the flow path switching valve 12 is set to Z, the first opening / closing valve 28 is automatically opened, and the inside of the first solvent storage tank 9A is set to atmospheric pressure, Open the first switching valve 23A,
The solvent accumulated in the first solvent storage tank 9A is discharged to empty the first solvent storage tank 9A. When the inside of the first solvent storage tank 9A becomes empty, the first switching valve 12A and the first opening / closing valve 28 are switched to a closed state, and then the first opening / closing cock 33 is opened to be in an always operating state. The inside of the first solvent storage tank 9A is reduced to a predetermined pressure by the exhaust pump P2. Thus, this control means 13
It has a warning function.

Even if the sample liquid storage tank 4 is full of sample liquid, it is possible to immediately proceed to the concentration operation. In this specific example, it is assumed that the initial state is empty.

(3) Supply of Sample Liquid to Sample Reservoir When in the operating state, first, an operation of filling the sample liquid reservoir 4 with the sample liquid is performed. As shown in FIG. 2, the measured weight value SV of the sample liquid storage tank 4 is output from the second weight measuring device 6 to the control calculation means as an electric signal.

As shown in FIG. 2, the control calculating means compares the input measured weight value SV with a previously stored allowable minimum weight value SV _min, and in this case, the measured weight value is changed to the allowable minimum weight value. It is determined that the value is smaller than or equal to the value, and an operation command signal is output to the second opening / closing valve 22 and the liquid sending pump to open the second opening / closing valve 22 and drive the liquid sending pump. Let it. Second open / close valve 2
The sample liquid is transferred from the preliminary sample liquid storage tank 7 to the sample liquid storage tank 4 through the second sample liquid transfer means 8 when the liquid supply pump 2 is opened and the liquid feed pump is driven. The second opening / closing valve 22 is kept open.

When the sample liquid is transferred to the sample liquid storage tank 4, the weight of the sample liquid storage tank 4 increases. The increasing weight of the sample liquid storage tank 4 is measured by the second weight measuring device 6, and the measured weight value is output to the control calculation means.

The control operation means compares the input measured weight value SV with the allowable maximum weight value SV _max of the sample liquid storage tank 4 and calculates whether the calculation result falls within a predetermined threshold value or the measured value and the allowable maximum weight value. If the values match, the second on-off valve 22
Then, an operation command signal is output to the liquid feed pump, the second opening / closing valve 22 is closed, and the driving of the liquid feed pump is stopped. As a result, the sample liquid storage tank 4 is filled with a required amount of the sample liquid, and a “full state” is set. The second on-off valve 22 is thereafter kept closed.

When the automatic concentrator 1 is in the operating state, the control calculation means constantly monitors the measured weight value of the sample liquid storage tank 4 output from the second weight measuring device 6,
As a result of the sample liquid being supplied from the sample liquid storage tank 4 to the flask 14 many times, the result of the comparison between the measured weight value of the sample liquid storage tank 4 and the allowable minimum weight value falls within a predetermined threshold value or is measured. When the weight value matches the allowable minimum weight value, it is determined that the amount of the sample liquid in the sample liquid storage tank 4 is insufficient, and an operation command signal is output to the second opening / closing valve 22 and the liquid sending pump, and The second opening / closing valve 22 is opened and the liquid feed pump is driven.

In this way, the sample liquid in the sample liquid storage tank 4 is not hindered from being supplied to the flask 14.
The sample liquid is automatically supplied to the sample liquid storage tank 4, and the sample liquid in the sample liquid storage tank 4 does not run out.

In this example, the sample liquid is supplied to the preliminary sample liquid storage tank 7 manually. However, in this preliminary sample liquid storage tank 7, a liquid level meter that detects the liquid level and outputs the detection result to the control calculation means, or measures the weight of the preliminary sample liquid storage tank 7 and calculates the measured weight value A fourth weight measuring device for outputting to the control arithmetic means is provided, and when the detection result of the liquid level is input and reaches a predetermined threshold value, or when the measured weight value output from the fourth weight measuring device is a predetermined value, When the threshold value is reached, a warning signal may be output from the control calculation means, for example, a warning display may be performed on a display means (not shown), or a warning buzzer may be sounded based on the warning signal.

(4) Supply of Sample Liquid to Flask As shown in FIG. 3, the control arithmetic means includes a measured weight value SV output from the second weight measuring means and a maximum allowable weight value SV of the sample liquid storage tank 4. It is confirmed that the calculation result with _min is within a predetermined threshold value or does not match as a calculation result, that is, that the sample liquid storage tank 4 has an amount of sample liquid that can be added, and that the first weight or measurement weight value RW rotary evaporator body 2 output from the measuring device 3 is equal to a predetermined permissible minimum weight value RW _min, to verify that it is smaller than the operation command signal to the first on-off valve 21 And the first open / close valve 21 is opened.

At this time, the control operation means has already output the operation command signal to the heating means and the exhaust means, and the heating means heats the inside of the flask 14 to a predetermined temperature. The inside is set to a predetermined reduced pressure.

[0061] Control operation means calculates a matching the measured weight value SV and the allowable maximum weight value SV _min, when determining, stop the operation of supplying the sample solution in the flask 14, the sample liquid reservoir 4 The operation of replenishing the sample liquid is performed.
This operation is as described in the section “(3) Supply of sample liquid to sample storage tank”.

The control calculation means also outputs an operation command signal to the flow path switching valve 12, and the flow path from the discharge port 18 to the flow path switching valve 12 and the flow path switching valve 12 are controlled by the flow path switching valve 12. To the third first solvent storage tank 9A.

When the first opening / closing valve 21 is opened, the pressure in the flask 14 is reduced, and the pressure difference between the flask 14 and the sample liquid storage tank 4 causes the pressure in the sample liquid storage tank 4 to increase.
The sample liquid is transferred from the inside into the flask 14 through the second sample liquid transfer means 8. By being transferred, the weight of the rotary evaporator main body 2 increases.

The first weight measuring device 3 measures the weight of the rotary evaporator body 2 and outputs an electric signal indicating the measured weight value to the control calculation means. The control calculation means calculates the input measured weight value RW and the maximum allowable weight value RW _{max of the} rotary evaporator body 2 stored in advance.
Is calculated, and the measured weight value RW and the allowable maximum weight value RW are calculated.
_max reaches a predetermined threshold value or the measured weight value RW
If the permissible maximum weight value RW _{m ax} matches, flasks 1
It is determined that a predetermined amount of the sample liquid has been supplied into 4, and an operation command signal is output to the first opening / closing valve 21. The first opening / closing valve 21 shuts off the first sample liquid transfer means 5.

(5) Concentration and Addition of Sample Solution The control calculation means keeps inputting the weight value RW of the rotary evaporator body 2 output from the first weight measuring device 3.

In the rotary evaporator main body 2, the flask 14 is heated to heat the flask 14.
The solvent in the sample liquid in the inside evaporates, the evaporated solvent is cooled by the cooling means 17 and condensed, and the liquefied solvent is discharged into the outlet 1
8 and accumulates in the first solvent storage tank 9A. As the solvent evaporates from the sample liquid in the flask 14, the weight of the rotary evaporator body 2 decreases as shown in FIG.

The measured weight value RW decreases linearly from the initial time t ₀ to a certain time,
As the concentration of the sample liquid in the inside increases, the rate of decrease ΔRW / Δt of the weight value RW slows down, and a state in which the rate of decrease does not change much over time. In this example, when the reduction rate reaches a certain value, it is determined that it is not efficient to further concentrate, and a fresh sample solution is injected into the flask 14.

That is, the measured weight value RW of the rotary evaporator body 2 output from the first weight measuring device 3
Is input to the control calculation means, and the measured weight value R at a certain point in time is
W and a measured weight value RW at a time point when a predetermined time Δt has elapsed from the time point are selected, and a weight value reduction rate ΔRW / Δt at the time interval is calculated, and the calculated weight value reduction rate is determined in advance. It is determined whether or not the weight value that gives the reduction rate that matches the threshold value is output within a predetermined time after the sample liquid injection, and the calculated weight value reduction rate is determined. When it is confirmed that the predetermined number (m) of the sample liquids continuously match the threshold value and that the weight value giving the decrease rate that matches the threshold value is not output within a predetermined time after the injection of the sample liquid, the sample liquid in the flask 14 is checked. Is determined to have been concentrated to a predetermined concentration,
An operation command signal is output to the first opening / closing valve 21. At this time, the threshold is updated.

The timing at which the operation command signal is output to the first opening / closing valve 21 is determined by the fact that the decreasing rate at which the threshold value is reached is continuously repeated a predetermined number of times as described above. This is because attention has been paid to a phenomenon in which the evaporation rate of the solvent decreases as the liquid is concentrated. Of course, the timing at which the operation command signal is output to the first opening / closing valve 21 can be determined based on the amount of the remaining liquid in the flask 14, but the remaining amount of the sample liquid at the time of the first replenishment of the sample liquid and the second time The remaining amount of the sample solution at the time of replenishing the sample solution and the remaining amount of the sample solution at the time of the n-th (where n is an integer of 3 or more) sample solution must be determined in advance.

The first opening / closing valve 21 for inputting the operation command signal brings the first sample liquid transfer means 5 into the open state. As a result, the sample liquid is supplied from the sample liquid storage tank 4 into the flask 14 through the first sample liquid transfer means 5.

[0071] When in the sample liquid is supplied into the flask 14 reaches a predetermined maximum allowable volume RW _max, control calculation means first by the first on-off valve 21 by outputting an operation command signal to the first on-off valve 21 The sample liquid transfer means 5 is turned off. The operation of the control calculation means at this time can be well understood in the description of "(4) Supply of sample liquid to flask".

When the sample liquid is newly poured into the flask 14, the solvent in the sample liquid in the flask 14 evaporates and is cooled and condensed by the cooling means 17, and the liquefied solvent is removed from the first solvent storage tank. Stored in 9A.

As the solvent in the flask 14 evaporates, the weight of the rotary evaporator body 2 decreases. The control calculation means that constantly monitors the reduction rate of the measured weight value of the rotary evaporator main body 2 determines that the calculation result that the reduction rate has reached a predetermined threshold and the reduction rate has reached a predetermined threshold has been repeated a predetermined number of times. Then, the sample liquid is supplied from the sample liquid storage tank 4 into the flask 14 as described in the section of “(3) Sample liquid supply to flask”.

When the concentration by evaporating the solvent from the sample liquid in the flask 14 and the replenishment of the sample liquid into the flask 14 after the concentration are repeated, the amount of the residual liquid after the concentration increases. Then, as a result of repeating the evaporation of the solvent from the sample solution in the flask 14 and the replenishment of the sample solution into the flask 14, an increased amount of the concentrated solution remains in the flask 14, and even if the sample solution is further replenished, The state in which the evaporation rate of the solvent evaporating from the high-concentration sample solution in the flask 14 becomes extremely low. Under this state, the reduction rate of measured weight values of the rotary evaporator body 2, since decreasing value from the beginning, as shown in FIG. 4, the control operation means a predetermined time from the supply when t _n of the sample liquid Within this time, it is confirmed that the reduction rate of the measured weight value has reached a predetermined low reduction rate, and upon confirmation, it is determined that the concentration operation is completed, and the concentration operation is stopped. At the same time, the display means displays "concentration operation completed" or a warning sound is issued by a warning buzzer or the like.

When the concentration operation is completed, the operator removes the flask 14 whose rotation has been stopped from the rotary evaporator body 2 and takes out the concentrated liquid in the flask 14. The empty flask 14 is mounted on the rotary evaporator body 2, and the concentration and the addition of the sample liquid are resumed.

(6) Recovery of Solvent The control operation means includes the concentration in the flask 14 and the
4 while the addition of the sample solution into
The measured weight value of the first solvent storage tank 9A measured by the third first weight measuring device 10A is continuously monitored.

That is, as shown in FIG.
The solvent evaporated from the sample solution in the fourth solvent storage tank 9A
As it is stored in the third weighing device 1
The measured weight value SW1 of the first solvent storage tank 9A output from 0A increases. The control calculation means is configured to store the measured weight value SW1 of the first solvent storage tank 9A and the first stored weight value SW1 in advance.
Maximum weight value SW1 _max for the solvent storage tank 9A
And the measured weight value SW1 and the allowable maximum weight value SW
_It is determined whether or not the result of subtraction from _max reaches a predetermined threshold. This threshold is determined in advance and stored in the storage means of the control calculation means. The control operation means determines that the first solvent storage tank 9
When it is determined that the inside of A is full of the solvent, the flow of the solvent is changed from the first solvent storage tank 9A to the second solvent storage tank 9B. Thereby, the solvent evaporated from the sample liquid in the flask 14 and condensed and liquefied flows from the outlet 18 into the second solvent storage tank 9B, and thereafter, the second solvent storage tank 9B
Solvent starts to accumulate in the.

That is, before the flow path switching valve 12 is switched, the first opening / closing cock is switched to the open state, and the inside of the second solvent storage tank 9B is reduced to a predetermined pressure by the exhaust pump P2. Next, the flow path switching valve 12 is switched so that the solvent flowing out of the outlet is discharged to the second solvent storage tank 9B.
So that it flows into By switching the flow path switching valve 12, the flow path switching valve 12 is closed with respect to the first solvent storage tank 9A. Since the pressure inside the first solvent storage tank 9A is reduced, the first solvent storage tank 9A is opened by opening the first opening / closing valve 28 and keeping the first opening / closing cock 33 closed. Atmospheric pressure inside. After the inside of the first solvent storage tank 9A returns to the atmospheric pressure, the first switching valve 23A is opened. Thereby, the solvent in the first solvent storage tank 9A is discharged through the first discharge pipe 24 and the discharge main pipe 26. As the solvent in the first solvent storage tank 9A is discharged, the weight of the first solvent storage tank 9A decreases.

The measured weight value SW1 output from the third first weight measuring device 10A for measuring the weight of the first solvent storage tank 9A is input to the control calculation means. The control operation means is
The measured weight value SW1 input over time is compared with a previously stored minimum allowable weight value SW1 _{min of} the first solvent storage tank 9A which is stored in advance, and whether or not the calculation result matches a predetermined threshold value is determined.
Alternatively, if the measured weight value matches the allowable minimum weight value, the control calculation means outputs an operation command signal to the first switching valve 23A.

In response to the operation command signal, the first switching valve 2
3A closes the first discharge pipe 24 and the discharge main pipe 26.

Thereafter, the first opening / closing valve 28 is closed, and the first opening / closing cock 33 is opened. The inside of the first solvent storage tank 9A is evacuated to a predetermined pressure reduction degree by the discharge pump P2, and when the predetermined pressure reduction degree is achieved, the first opening / closing cock 33 is closed.

On the other hand, the third second weighing device 10B
As shown in FIG. 7, the weight of the second solvent storage tank 9B is continuously measured, and the measured weight value SW2 is output to the control calculation means. The control calculation means inputs the measured weight value SW2 and monitors and manages the storage state of the solvent in the first solvent storage tank 9A in the same manner as the storage state of the solvent in the second solvent storage tank 9B. Monitor and manage

That is, the third second weight measuring device 10B
Weight value SW of second solvent storage tank 9B output from
2 is compared with a preset allowable maximum weight value SW2 _max for the second solvent storage tank 9B, and the comparison calculation result reaches a predetermined threshold value, or the measured weight value SW2 is obtained as a comparison calculation result. the permissible maximum weight value SW2 _{ma x}
Is determined to match, the flow path switching valve 12, the second
An operation command signal is output to the switching valve 23B, the second opening / closing valve 30, and the second opening / closing cock 35.

The flow path switching valve 12 connects the flow path of the solvent from the discharge port 18 to the second solvent storage tank 9 B with the discharge port 18.
To the solvent flow path to the first solvent storage tank 9A. As a result, the filled second solvent storage tank 9
The solvent no longer flows to B, and the solvent starts to flow to the first solvent storage tank 9A which is already empty and has a predetermined degree of reduced pressure.

Next, the second on-off valve 30 is switched to return the inside of the second solvent storage tank 9B to the normal pressure state. The second switching valve 23B establishes communication between the second discharge pipe 25 and the discharge main pipe 26, thereby discharging the solvent in the second solvent storage tank 9B.

The procedure of discharging the solvent in the second solvent storage tank 9B and setting the inside of the second solvent storage tank 9B to a predetermined degree of reduced pressure after the solvent is completely drained is as follows. The procedure is the same as that in the tank 9A.

When such an operation is automatically performed, when the first solvent storage tank 9A becomes full of the solvent,
The storage destination is changed from the first solvent storage tank 9A, in which the solvent evaporated and recovered from the flask 14 is stored, to the second solvent storage tank 9B, and the solvent from the filled solvent storage tank 9 is removed. Automatically ejected.

[0088]

According to the present invention, the additional injection of the sample liquid into the flask can be automatically performed, and even if the storage tank for storing the solvent evaporated / recovered from the sample liquid becomes full, the automatic injection is performed. The solvent can be discharged from the storage tank,
An automatic concentration device that automates the concentration operation can be provided.

[Brief description of the drawings]

FIG. 1 is an explanatory diagram showing an example of an automatic concentration device according to the present invention.

FIG. 2 is a flowchart showing a control procedure by a control unit when a sample liquid is supplied to a sample liquid storage tank in the automatic concentration device.

FIG. 3 is a flowchart showing a control procedure by a control unit when a sample solution is injected from a sample solution storage tank into a flask in the automatic concentration device.

FIG. 4 is a graph showing the change over time in the weight of the sample solution when the sample solution in the flask is concentrated by the automatic concentration device.

FIG. 5 is a flowchart showing a procedure for additionally injecting a sample solution into the flask when the sample solution in the flask is concentrated by the automatic concentration device.

FIG. 6 is a flowchart showing a procedure for managing and monitoring a solvent in a first solvent storage tank when a sample solution in a flask is concentrated by an automatic concentration device.

FIG. 7 is a flowchart showing a procedure for managing and monitoring the solvent in the first solvent storage tank when the sample solution in the flask is concentrated by the automatic concentration device.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Automatic concentration apparatus, 2 ... Rotary evaporator main body, 3 ... 1st weight measuring apparatus, 4 ... Sample liquid storage tank, 5 ... 1st sample liquid transfer means, 6 ... ..Second
Weight measuring device, 7 ... reserve sample liquid storage tank, 8 ...
Second sample liquid transfer means, 9 ... Solvent storage tank, 9A ...
1st solvent storage tank, 9B ... second solvent storage tank, 1
0 ... third weight measuring device, 11 ... third solvent transfer means, 12 ... flow path switching means, 13 ... control means, 14 ... flask, 15 ... water bath ,
16 ... Introduction pipe, 17 ... Cooling means, 18 ... Outlet, 19 ... Base, 20 ... Post, 21 ... First open / close valve, 2 ... Second Open / close valve, 23A
..First switching valve, 23B... Second switching valve, 24... First discharge pipe, 25... Second discharge pipe, 26. 1st air introduction pipe, 28 ... 1st on-off valve, 29 ... 2nd air introduction pipe, 30 ... 2nd on-off valve, 31 ... air introduction main pipe, 32 ... 1 exhaust pipe, 33 ... first open / close cock, 34 ... second exhaust pipe, 35 ... second open / close cock, 36 ... exhaust main pipe.

Claims (1)

[Claims] 1. A rotary evaporator main body having a rotatable flask capable of storing a sample liquid, and a first evaporator for measuring the weight of the rotary evaporator main body.
A weight measuring device, a sample liquid storage tank for storing a sample liquid to be supplied into the flask, and the sample liquid storage when the weight of the rotary evaporator body measured by the first weight measuring device reaches a predetermined value. First sample liquid transfer means for transferring the sample liquid from the tank into the flask, a second weight measuring device for measuring the weight of the sample liquid storage tank, and a preliminary sample liquid storage tank for storing the sample liquid; A second sample liquid transferring means for transferring the sample liquid in the preliminary sample liquid storage tank into the sample liquid storage tank when the weight of the sample liquid storage tank measured by the second weight measuring device reaches a predetermined value; A plurality of solvent storage tanks for storing the solvent evaporated and recovered from the sample liquid in the flask; a third weight measuring device for measuring the weight of each of the plurality of solvent storage tanks; and a sample in the flask. Evaporated from liquid and cooled A third solvent transfer means disposed so as to transfer the liquefied solvent to the plurality of solvent storage tanks; and a specific solvent storage tank in the plurality of solvent storage tanks via the third solvent transfer means. When transferring the solvent evaporated and recovered from the sample solution in the flask, when the weight of the specific solvent storage tank measured by the third weighing device reaches a predetermined value, the flask A flow path switching means for switching a flow path so that the solvent evaporated / recovered from the sample liquid in the inside flows from the specific solvent storage tank to another solvent storage tank. Automatic concentrator.