JPH0675644B2 - Control method for rotary evaporator - Google Patents

Description

The present invention relates to a method for controlling a rotary evaporator.

[Conventional technology]

When the sample is concentrated, the conventional rotary evaporator manually stops the flask rotation motor, moves the flask upwards to bring the flask into a non-heated state, returns the vacuum state in the flask to atmospheric pressure, and Had taken a sample from. However, in this method, the end time of the concentration was not clear, and the end point was constantly checked while visually observing, so that it was largely dependent on the judgment of the researchers.

Therefore, as disclosed in Japanese Patent Laid-Open No. 59-73001, a method has been developed in which the concentration time of the sample solution is set and when the set time elapses, the work of the upper air is automatically performed.

[Problems to be solved by the invention]

However, this method raises and lowers the glass flask containing the sample solution, the condenser, and the motor for rotating the flask, so that the flask and the condenser may be damaged unless handled carefully. , The tube connected to the condenser may fall out, and
Since the time for concentrating the sample is set, it is good for concentrating a known sample, but any other sample cannot be used.

Therefore, the present invention has been invented in view of these points,
The present inventor continued to evaporate while concentrating the sample solution in a constant vacuum state while maintaining a constant vapor temperature, and when the water content began to disappear, the temperature started to rise and the relative evaporation temperature difference between two or more liquids was high. In the case of concentrating and separating a large mixed solution of, the evaporation temperature rises when the first low boiling point component begins to distill and then the second low boiling point component begins to distill. Another object of the present invention is to provide a control method in which the safety of a rotary evaporator is improved by lowering a constant temperature water tank, which is stronger than a flask or the like, with respect to the flask to automatically control the work after the concentration.

[Means for solving problems]

In order to solve such a problem, the present invention, by rotating the flask containing the sample solution by a motor drive and heating the sample solution in the flask in a constant temperature water tank under constant decompression, Concentration, in the method of controlling the rotary evaporator that separates the flask and the constant temperature water tank after the completion of concentration, when the vapor temperature of the sample solution in the flask that is constant temperature heated in the constant temperature water tank rises with respect to the set temperature, this rise The temperature is detected by the vapor temperature detection sensor provided in the flask, and based on this detection, the alarm device is activated in the following order, the heater for heating the constant temperature water tank is stopped, and the drive motor is stopped to stop the flask. To stop the rotation of the machine and drive the lift motor to lower the constant temperature water bath to separate the flask from the flask to keep the flask in a non-heated state and to maintain a vacuum inside the flask. Back in the flask by opening the solenoid valve to the atmospheric pressure, it is characterized in that for automatically controlling the working time of concentration termination.

[Work]

Therefore, when the temperature in the flask rises above the set temperature, it is possible to detect this and operate the control device to automatically carry out the work for completing the concentration.

〔Example〕

Hereinafter, the method of the present invention will be described based on an embodiment shown in the drawings.

FIGS. 1 and 2 show an evaporator used in the method of the present invention. On a support leg 1, a support column 3 is erected which extends and contracts in the vertical direction by loosening the fixing metal fitting 2. A flask 4 containing a sample solution T is rotatably supported by a rotation driving motor 5 on the column 3. At the front of the flask 4 is a condenser 6 for condensing the evaporated solvent.
Is connected, and the condenser 6 is provided with a recovery flask 7 for recovering the condensed solvent, and the condenser 6 is provided with a cooling pipe 8 through which a cooling liquid flows. In addition, the condenser 6 has a tube 10 connected to the vacuum pump 9.
Are continuously connected via a solenoid valve 11.

A base 12 arranged near the support leg 1 is provided with a constant temperature water tank 13 so as to be vertically movable. A screw rod 14 is rotatably provided at the lower part of the constant temperature water tank 13, and the lower end of the constant temperature water tank 13 is screwed into a female screw piece 15 provided on the base 12. Further, a lift motor 16 for the constant temperature water tank 13 is provided in the base 12, and a bevel gear 17 provided on the output shaft of the motor 16 meshes with a bevel gear 18 provided on the screw rod 14 to provide a lift motor 16 The constant temperature water tank 13 is moved up and down with respect to the flask 4 by the driving. A heater 19 for heating the water W in the constant temperature water tank 13 is arranged in the constant temperature water tank 13.

Further, a vapor temperature detecting sensor 20 in the flask 4 is provided in the flask 4, and a water temperature detecting sensor for the water W is provided in the constant temperature water tank 13.
21 are provided respectively.

A control device 22 for controlling the rotation driving motor 5, the solenoid valve 11, the lift motor 16 and the heater 19 is provided in the base 12. The control device 22 supplies the analog signals of the steam temperature detecting sensor 20 and the water temperature detecting sensor 21 to the steam temperature detector.
It is digitized by the A / D converter 25 and input via the 23 and the water temperature detector 24. Further, the control device 22 has a first motor driver 26 for operating the rotary drive motor 5, an electromagnetic valve driver 27 for turning on / off the solenoid valve 11, a second driver 28 for operating the lift motor 16, and a heater according to the output thereof. 19
The heater controller 29 that supplies electric power to Further, a signal is input to the control device 22 from a setter 30 that sets the known concentration time of the sample solution T, the rotation speed of the rotation driving motor 5, and the like.

Next, the control method of the present invention will be described based on the above apparatus.

FIG. 3 is a flow chart of the apparatus shown in FIG. 2, in which the evaporator is started by powering on the controller 22.

First, when the water temperature of the constant temperature water tank 13 is set via the setting device 30 (step 50), while measuring the water temperature in the constant temperature water tank 13 (step 51), the heater controller 28 is operated to reach the set temperature. Power is supplied to the heater 19 (step 52). As a result, if the water temperature in the constant temperature water tank 13 becomes equal to the set value (step 53), the operator is notified by a visual alarm that the water temperature in the constant temperature water tank 13 has reached the set value (for example, 60 ° C) (the water temperature is digitally displayed. ). Based on this, the operator drives the rotary drive motor 5 via the setting device 30.
When the number of revolutions is set (step 70), electric power according to the set number of revolutions is applied to the motor 5 (step 71), and when the number of revolutions becomes equal to the set value (step 72), the number of revolutions is digitally displayed. Can be confirmed by (step 73). Next, the operator actuates the lift motor 16 to raise the constant temperature water tank 13, sink the flask 4 into the water W in the constant temperature water tank 13, stop the operation of the lift motor 16 and stop the rise of the constant temperature water tank 13. .

On the other hand, the vapor temperature in the flask is separately set (step 80), and the set temperature is digitally displayed. Then, while measuring the vapor temperature of the sample solution T (step 81)
(The steam temperature is digitally displayed), concentration work is performed, and it is determined whether the steam temperature is lower than the set value (step 82) or higher than the set value (step 83).

As the concentration work progresses, the water content of the sample solution T in the flask 4 is running out, and the first sample solution T of two or more liquids is mixed.
When the low boiling point component evaporates and the second low boiling point component begins to evaporate, the temperature in the flask rises. When this temperature rise is detected by the evaporation temperature detecting sensor 20 (for example, when the temperature rises by 1 ° C.) (step 83), the control device 22 sounds a voice alarm (for example, a buzzer) (step 84) and at the same time a first visual alarm is issued. Turn on the container (eg lamp) (step 85),
The operator is notified, the heater controller 28 is controlled to stop the power supply to the heater 19 (step 86), the rotation drive motor 5 is stopped (step 87), and the lift motor 16 is driven to keep the constant temperature water tank 13 The flask 4 is lowered to separate the flask 4 from the water W (step 88), the electromagnetic valve 11 is operated to return the inside of the flask 4 to atmospheric pressure (step 89), and the concentration operation is completed.

Further, the control device 22 causes the water temperature detecting sensor 21 to raise the temperature of the water in the constant temperature water tank by a predetermined temperature (for example, 5 ° C.).
Rise), sound the voice alarm (step 55), turn on the second visual alarm (step 56), notify the operator, and control the heater controller 28 to stop the power supply to the heater 19 (step 57). ), Lift motor 16
Is driven to lower the constant temperature water tank 13 to separate the flask 4 from the water W (step 58), the rotation drive motor 5 is stopped (step 59), and the solenoid valve 11 is operated to bring the flask 4 to atmospheric pressure. Return (step 60) and interrupt the concentration operation.

Further, when the known concentration time of the sample solution T is set by the setter 30 (step 90), the control device 22 starts the timer (step 91) and when the concentration time elapses (step 92). ), Sound an audio alarm (step
93) and turn on the third visual warning device (step 9).
4) Notify the operator, control the heater controller 28 to stop the power supply to the heater 19 (step 86),
The lift motor 16 is driven to lower the constant temperature water tank 13 to separate the flask 4 from the water W (step 87), the rotation drive motor 5 is stopped (step 88), and the solenoid valve 11 is operated to operate the inside of the flask 4. Is returned to atmospheric pressure (step 89), and the concentration work is completed.

Incidentally, step 84,85,86,87,88,89 or step 93,94,86,87,88,89 or step 55,5 in the above embodiment
The order of 6,57,58,59,60 can be changed as appropriate.

Further, if a control device for keeping the water level of the constant temperature water tank 13 constant is added, even if the water level is lowered due to some reason and the water level is lowered, the stop mechanism can be activated to notify the operator by an alarm device. .

〔The invention's effect〕

As described above, the present invention detects the increase in the vapor temperature of the sample solution being distilled by the vapor temperature detecting sensor provided in the flask, and based on this detection, activates the alarm device in the following order. Then, the heater for heating the constant temperature water tank is stopped, the rotation of the flask is stopped by stopping the driving motor, the motor for lifting is driven to lower the constant temperature water tank, and the flask is separated from the flask to put the flask in a non-heating state. Open the electromagnetic valve to keep the inside of the flask vacuum and return the inside of the flask to atmospheric pressure,
Since the work at the end of the concentration is automatically controlled, the sample which is easily decomposed by heat can be surely protected from heat and a highly reliable sample can be obtained. Moreover, since the constant temperature water tank is moved up and down, it is easy to move and work is safe, and since the vapor temperature is measured, unknown samples can be concentrated.

[Brief description of drawings]

The drawings are for explaining the method of the present invention. FIG. 1 is a schematic perspective view of a rotary evaporator, FIG. 2 is a view showing a relationship between a rotary evaporator and a control device, and FIG. 3 is a flowchart of the evaporator. 4 ... Flask, 5 ... Rotation drive motor 6 ... Condenser, 11 ... Solenoid valve, 13 ... Constant temperature water tank 19 ... Heater, 20 ... Steam detection sensor 21 ... Water temperature detection sensor, 22 ...... Control device 30 …… Setting device, T …… Sample solution, W …… Water

Claims (1)

[Claims] 1. A sample solution is concentrated by rotating the flask containing the sample solution by a motor drive and heating the sample solution in the flask in a constant temperature water tank under constant decompression, and after the concentration is completed, In the method of controlling a rotary evaporator that separates the constant temperature water tank from the constant temperature water tank, when the vapor temperature of the sample solution in the flask that is constant temperature heated in the constant temperature water tank rises with respect to the set temperature, this rising temperature is the vapor temperature provided in the flask. Detect with the detection sensor, and based on this detection, activate the alarm in the following order, stop the heater for heating the constant temperature water tank, stop the drive motor to stop the rotation of the flask, and lift the motor. To lower the constant temperature water tank to separate it from the flask to put the flask in a non-heated state, open the solenoid valve to keep the inside of the flask under vacuum, and open the inside of the flask. Back to pressure, the control method of a rotary evaporator, characterized by automatically controlling the working time of concentration termination.