JP2021107051A - Concentrator and control method of the same - Google Patents

Abstract

To provide a concentrator which prevents bumping of a solvent to improve efficiency of concentration, and to provide a control method of the concentrator.SOLUTION: A concentrator includes: a constant-temperature liquid tank 12 which heats a sample vessel 11 into which a sample is introduced; a condenser 15 which condenses a gas evaporated in the sample vessel 11; a coolant circulator 18 which cools the condenser 15; a decompression pump 17 which decompress the sample vessel; and a controller 31 which controls a bath temperature Tb of the constant-temperature liquid tank 12 and a chiller temperature Tc of the coolant circulator 18 and controls driving of the decompression pump 17. The controller 31 sets a temperature, which is decreased from the bath temperature Tb by a predetermined temperature, as a target boiling temperature T and controls the decompression pump 17 to decompress a pressure in the sample vessel 11 to a target pressure so that a boiling temperature of the solvent becomes the target boiling temperature. The pressure in the sample vessel 11 is adjusted to the target pressure and the sample vessel 11 is heated by the constant-temperature liquid tank 12 to evaporate the solvent.SELECTED DRAWING: Figure 1

Description

The present invention relates to a concentrator and a control method for the concentrator, and particularly relates to a technique for preventing bumping and efficiently concentrating a sample.

Conventionally, a concentrator (sometimes called an evaporator) has been used to remove a specific solvent contained in a sample. In the concentrator, the sample to be concentrated is introduced into a sample container such as an eggplant flask, and the inside of the sample container is depressurized and then inserted into a constant temperature liquid tank filled with a liquid such as heated water or oil. , Warm the sample. After a while, the temperature of the sample introduced into the sample container rises, and when the boiling point of the solvent to be removed is reached, this solvent evaporates, so that this solvent can be removed from the sample (for example, patent). Reference 1).

However, in the conventional concentrator, when the boiling point temperature of the solvent is reached while the sample container is being heated, the solvent contained in the sample may suddenly boil. When sudden boiling occurs, the contents of the sample are ejected to the outside at that momentum, causing a problem that the concentration efficiency is lowered.

Japanese Unexamined Patent Publication No. 8-266803

As described above, the conventional concentrator has a problem that when the sample container is heated to remove the solvent contained in the sample, the solvent may suddenly boil and the concentration efficiency is lowered.

The present invention has been made to solve such a conventional problem, and an object of the present invention is a concentrator capable of preventing solvent bumping and improving concentration efficiency, and a concentrator. Is to provide a control method for.

In order to achieve the above object, the concentrator according to the present invention is a concentrator that evaporates the gas to be removed contained in the sample to concentrate the sample, and heats the sample container into which the sample is introduced. A warmer, a condenser that condenses the gas evaporated in the sample container, a cooler that cools the condenser, a decompression pump that depressurizes the inside of the sample container, and a heating temperature by the warmer. , The cooling temperature by the cooler, and a control unit that at least controls the drive of the decompression pump. The control unit sets a temperature obtained by subtracting a predetermined temperature from the heating temperature as a target boiling point, and sets the solvent. The pressure in the sample container is reduced to the target pressure by controlling the decompression pump so that the boiling point of the sample container becomes the target boiling point, the pressure in the sample container is set to the target pressure, and the warmer is used. The sample container is heated to evaporate the solvent.

The control method of the concentrator according to the present invention is a control method of the concentrator that concentrates the sample by evaporating the solvent to be removed contained in the sample, and heats the sample container into which the sample is introduced. The step of acquiring the heating temperature by the warmer and setting the temperature obtained by subtracting a predetermined temperature from the heating temperature as the target boiling point of the solvent and the pressure of the sample container set the boiling point of the solvent as the target boiling point. The step of controlling the decompression pump so as to reach the target pressure, which is the pressure, and the state where the inside of the sample container is the target pressure, the sample container is heated to evaporate the solvent contained in the sample. It is characterized by having steps.

According to the present invention, it is possible to prevent the solvent from suddenly boiling and improve the efficiency of concentration.

FIG. 1 is an explanatory diagram showing a configuration of a concentrator according to the first embodiment of the present invention. FIG. 2 is a flowchart showing a processing procedure of the concentrator according to the first embodiment. FIG. 3 is an explanatory diagram showing a configuration of a concentrator according to the second and third embodiments of the present invention. FIG. 4A is a first fractionated diagram of a flowchart showing a processing procedure of the concentrator according to the second embodiment. FIG. 4B is a second fraction of a flowchart showing a processing procedure of the concentrator according to the second embodiment. FIG. 5A is a first fractionated diagram of a flowchart showing a processing procedure of the concentrator according to the third embodiment. FIG. 5B is a second fraction of a flowchart showing a processing procedure of the concentrator according to the third embodiment.

Hereinafter, embodiments of the present invention will be described with reference to the drawings. FIG. 1 is an explanatory diagram schematically showing a configuration of a concentrator according to the first embodiment of the present invention.
As shown in FIG. 1, the concentrator 101 according to the present embodiment includes a sample container 11, a constant temperature liquid tank 12, a trap ball 13, a rotary drive unit 14, a condenser 15, and a recovery liquid storage unit 16. The elevating device 22, the decompression pump 17, and the cooling water circulator 18 are provided. Further, it includes a controller 31 that controls the drive of the rotary drive unit 14, the decompression pump 17, and the cooling water circulator 18, and controls the temperature of the constant temperature liquid tank 12.

The sample container 11 is, for example, an eggplant flask, a round bottom flask, an Erlenmeyer flask, or the like, and a sample to be concentrated is introduced therein. In addition, the sample contains a solvent to be removed. Examples of the solvent to be removed include ethyl acetate, ethanol, methanol, methyl ethyl ketone, toluene, xylene, dichloromethane, chloroform, hexane and the like. In addition, the inside of the sample may contain a single solvent or a plurality of solvents.

The constant temperature liquid tank 12 (sometimes referred to as "water bath" or "oil bath") is filled with a liquid such as water or oil, and is heated by a heater such as a heating wire to heat the liquid to a desired temperature. Can be adjusted to. With the sample container 11 inserted inside the constant temperature liquid tank 12, the sample container 11 is heated by adjusting the liquid temperature in the constant temperature liquid tank 12, and by extension, the sample in the sample container 11 is heated. Can be done. Therefore, the solvent to be removed contained in the sample can be evaporated (vaporized). The method for heating the liquid (water, oil, etc.) in the constant temperature liquid tank 12 is not limited to the heating wire, and other methods can be adopted. It is also possible to directly heat the sample container 11 using a heater without using a liquid. That is, the constant temperature liquid tank 12 has a function as a warmer for heating the sample container 11 into which the sample is introduced.

The constant temperature liquid tank 12 is provided with a temperature sensor 12a (hereinafter, referred to as “bath temperature sensor 12a”) for measuring the temperature of the liquid. The detection data of the bus temperature sensor 12a is output to the controller 31.

The trap ball 13 accumulates the liquid released by the sudden boiling when the sudden boiling occurs in the sample container 11.

The rotation drive unit 14 includes a reduction motor (not shown) for driving, and rotates the sample container 11 at a constant speed with its central axis as a rotation axis.

The condenser 15 communicates with the tip opening of the sample container 11 and condenses the gas evaporated in the sample container 11.

The elevating device 22 operates the sample container 11 to be taken in and out of the constant temperature liquid tank 12 by raising and lowering the sample container 11.

The cooling water circulator 18 (sometimes referred to as a “chiller”) includes a cooling water tank 19 for accumulating cooling water and a cooling device (not shown) for cooling the cooling water in the cooling water tank 19. The cooling water tank 19 is connected to the spiral pipe 21 spirally installed in the condenser 15 via the cooling water pipe 20. The cooling water tank 19 is provided with a temperature sensor (hereinafter, referred to as “chiller temperature sensor 19a”) for measuring the temperature of the cooling water in the cooling water tank 19. The detection signal of the chiller temperature sensor 19a is output to the controller 31.

Then, the cooling water circulator 18 circulates the cooling water stored in the cooling water tank 19 through the spiral pipe 21 via the cooling water pipe 20 to cool the inside of the condenser 15. That is, the cooling water circulator 18 has a function as a cooler that cools and liquefies the steam in the condenser 15.

The recovery liquid reservoir 16 is provided below the condenser 15 and communicates with the condenser 15 to store the liquid condensed by the condenser 15. That is, since the gas (for example, vaporized solvent) that evaporates in the sample container 11 and is introduced into the condenser 15 is cooled by the cooling water flowing through the spiral pipe 21 and liquefied, this liquefied liquid (for example, for example). Accumulate the solvent to be removed).

The pressure reducing pump 17 is driven under the control of the controller 31 to reduce the pressure in the condenser 15. Since the condenser 15 communicates tightly with the sample container 11 via the rotary drive unit 14 and the trap ball 13, the inside of the sample container 11 is depressurized by depressurizing the inside of the condenser 15. Can be done. Therefore, the boiling point of the solvent introduced into the sample container 11 can be arbitrarily set within a predetermined range.

The controller 31 (control unit) controls the drive of the rotary drive unit 14, the decompression pump 17, and the cooling water circulator 18. Specifically, when the concentrator 101 is in operation, the controller 31 controls the decompression pump 17 so that the pressure in the condenser 15 becomes a desired pressure (pressure lower than atmospheric pressure). The controller 31 also controls the temperature of the cooling water circulated by the cooling water circulator 18 and the amount of circulating water. The controller 31 also controls the temperature of the liquid filled in the constant temperature liquid tank 12 to be a desired temperature. The controller 31 also includes an input unit (not shown) for the user to perform various data input operations, and a display unit (not shown) for displaying various information. Alternatively, it is provided with a touch sensor (not shown) that also serves as an input unit and a display unit.
The controller 31 can be configured as, for example, an integrated computer including a central processing unit (CPU) and storage means such as a RAM, a ROM, and a hard disk.

Then, in the present embodiment, when the solvent to be removed is removed from the sample introduced into the sample container 11 and the sample is concentrated, the solvent is prevented from suddenly boiling, which is efficient and stable. Allows the sample to be concentrated.

[Explanation of operation of the first embodiment]
Next, the operation of the concentrator 101 according to the first embodiment will be described. FIG. 2 is a flowchart showing a processing procedure of the concentrator 101 according to the first embodiment. Of the processes shown in FIG. 2, each process other than the manual operation is executed by the controller 31.

First, in step S11 of FIG. 2, the user introduces a sample to be concentrated in the sample container 11 in preparation for operating the concentrator 101. In addition, the solvent to be removed from this sample is selected. As described above, the solvent to be removed is, for example, ethyl acetate, ethanol, methanol, methyl ethyl ketone, toluene, xylene, dichloromethane, chloroform, hexane and the like.

In step S12, the user uses the ultimate pressure P0 of the decompression pump 17 at the input unit of the controller 31, the maximum heating temperature Td that can be heated in the constant temperature liquid tank 12, and the minimum cooling temperature that can be cooled by the cooling water circulator 18. Enter Te. The ultimate pressure P0 of the decompression pump 17 refers to the minimum pressure that the decompression pump 17 can depressurize.

In step S13, the controller 31 reads the liquid temperature (hereinafter, referred to as “bath temperature Tb”) in the constant temperature liquid tank 12 detected by the bath temperature sensor 12a. Further, the temperature of the cooling water detected by the chiller temperature sensor 19a (hereinafter referred to as “chiller temperature Tc”) is read.

In step S14, the controller 31 determines whether or not the difference between the bath temperature Tb and the chiller temperature Tc is 40 ° C. (difference threshold temperature) or more, that is, whether or not “Tb−Tc> 40 ° C.”. to decide. In order to efficiently cool and recover the solvent evaporated in the sample container 11, it is desirable that the difference between the bath temperature Tb and the chiller temperature Tc is large, and in this embodiment, this difference is set to 40 ° C. .. In the process of step S14, it is determined whether or not this condition is satisfied.

If "Tb-Tc> 40 ° C." (S14; YES), the process proceeds to step S20, otherwise (S14; NO), the process proceeds to step S15.

In step S15, the controller 31 controls the heater of the constant temperature liquid tank 12 so that the bath temperature Tb is higher than the chiller temperature Tc by 40 ° C. or more.

In step S16, the controller 31 determines whether or not the bus temperature Tb has reached the maximum heating temperature Td set in the process of step S12. When the maximum heating temperature Td is reached (S16; YES), the process proceeds to step S17. If the maximum heating temperature Td is not reached (S16; NO), the process is returned to step S14.

In step S17, the controller 31 controls the cooling water circulator 18 so that the chiller temperature Tc is 40 ° C. or more lower than the bath temperature Tb. That is, if "Tb-Tc> 40 ° C." is not achieved even if the bath temperature Tb reaches the maximum heating temperature Td, control is performed to lower the chiller temperature Tc.

In step S18, the controller 31 determines whether or not the chiller temperature Tc has reached the minimum cooling temperature Te set in the process of step S12. When the minimum cooling temperature Te is reached (S18; YES), the process proceeds to step S19. If the minimum cooling temperature Te is not reached (S18; NO), the process returns to step S14.

In step S19, the controller 31 displays an error message on the display unit. That is, when "Tb-Tc> 40 ° C." cannot be achieved by increasing the bath temperature Tb and decreasing the chiller temperature Tc (when the determination in S14 is not YES), this process can be executed. Since this is not possible, an error message is displayed on the display (not shown) and this process ends.

On the other hand, when a YES determination is made in step S14, in step S20, the controller 31 sets a temperature lower than the bath temperature Tb by a predetermined temperature (20 ° C. in this embodiment) as the solvent to be removed. It is set as the target boiling point T (let this be the solvent α1). That is, it is set as "target boiling point T = Tb-20 ° C.". For example, when the bath temperature Tb is 40 ° C., the target boiling point T = 20 ° C. is set.

In step S21, the controller 31 calculates the pressure at which the target boiling point T of the solvent α1 becomes 20 ° C. using a known calculation method, and sets this as the target pressure P1.

In step S22, the controller 31 compares the target pressure P1 with the ultimate pressure P0 of the decompression pump 17 set in the process of step S12. If "P1> P0", that is, if the capacity of the decompression pump 17 can reduce the pressure to the target pressure P1 (S22; YES), the process proceeds to step S24, otherwise (S22; NO), the step. The process proceeds to S23.

In step S23, the controller 31 controls the heater of the constant temperature liquid tank 12 to raise the bath temperature Tb. After that, the process returns to step S13. That is, when the bath temperature Tb rises, the target boiling point T rises due to the above-mentioned relationship of "T = Tb-20 ° C.", and thus the target pressure P1 can be raised. As a result, the target pressure P1 can be made higher than the ultimate pressure P0 of the decompression pump 17. That is, "P1> P0" can be set.

In step S24, the controller 31 drives the rotation drive unit 14 to rotate the sample container 11 at a constant speed. Further, the pressure reducing pump 17 is operated to control the pressure in the sample container 11 to be the target pressure P1.

In step S25, the controller 31 inserts the sample container 11 into the constant temperature liquid tank 12 to heat the sample in the sample container 11. The operation of inserting the sample container 11 into the constant temperature liquid tank 12 can be performed by controlling the elevating device 22. Alternatively, it may be inserted manually.

When the liquid in the constant temperature liquid tank 12 is heated so as to reach the bath temperature Tb, the boiling point of the solvent α1 is set to be 20 ° C. lower than the bath temperature Tb as described above. The solvent α1 contained in the sample in the sample container 11 can be stably evaporated and sent to the condenser 15 without bumping.

That is, the sample in the sample container 11 can be concentrated by removing the solvent α1 to be removed from the sample introduced in the sample container 11. Further, the steam introduced into the condenser 15 is cooled by the cooling water flowing through the spiral pipe 21, condensed, and accumulated in the recovery liquid reservoir 16. Therefore, the solvent α1 can be efficiently recovered.

In step S26, the controller 31 determines whether or not the temperature fluctuation of the bus temperature Tb is within the allowable fluctuation temperature y based on the detection data of the bus temperature sensor 12a. If it is within the permissible fluctuation temperature y (S26; YES), the process proceeds to step S27, and if not (S26; NO), the process returns to step S13.

That is, when the fluctuation of the bath temperature Tb is large and exceeds the range of the allowable fluctuation temperature y, the process from step S13 is repeated to reset the bath temperature Tb. Then, the target pressure P1 is reset so that the boiling point of the solvent α1 becomes the reset target boiling point.

On the other hand, when the temperature fluctuation of the bath temperature Tb is within the allowable fluctuation temperature y, it is determined that the solvent α1 is stably evaporated, and in step S27, the user visually confirms the completion of concentration. do. After that, this process ends. In this way, the solvent α1 to be removed can be removed from the sample introduced into the sample container 11 and the sample can be concentrated.

[Explanation of the effect of the first embodiment]
In this way, in the concentrator 101 according to the first embodiment of the present invention, the pressure in the sample container 11 is controlled by the decompression pump 17, and the boiling point of the solvent α1 to be removed is determined higher than the bath temperature Tb. The temperature is set to be lower by the temperature (for example, 20 ° C.). Therefore, when the sample container 11 is inserted into the constant temperature liquid tank 12, it is possible to prevent the solvent α1 contained in the sample from suddenly boiling. Therefore, it is possible to prevent the occurrence of problems such as the contents in the sample being released to the outside, and it is possible to stably concentrate the sample.

Further, a recovery liquid reservoir 16 is provided below the condenser 15, and when the vapor of the solvent α1 is cooled and condensed, the solvent α1 is accumulated. Therefore, the solvent contained in the sample can be efficiently recovered. When the change in the bath temperature Tb (heating temperature) is large, the boiling point of the solvent α1 is reset based on the changed bath temperature Tb, and the target pressure amount P1 is reset. Therefore, even when the bath temperature Tb changes, it is possible to stably concentrate the sample by following this change.

Further, the difference between the bath temperature Tb (heating temperature) of the constant temperature liquid tank 12 (heater) and the chiller temperature Tc (cooling temperature) of the cooling water circulator 18 (cooler) is 40 ° C. (preset difference). At least one of the bath temperature Tb and the chiller temperature Tc is controlled so as to be equal to or higher than the threshold temperature). Therefore, the difference between the bath temperature Tb and the chiller temperature Tc can be reliably widened, and the solvent α1 can be efficiently evaporated and condensed.

[Explanation of the second embodiment]
Next, the second embodiment of the present invention will be described. FIG. 3 is an explanatory diagram schematically showing the configuration of the concentrator 102 according to the second embodiment. Compared with the concentrator 101 shown in FIG. 1, the concentrator 102 shown in FIG. 3 is provided with a steam temperature sensor 41 near the opening of the sample container 11, and the detection signal of the steam temperature sensor 41 is controlled. The difference is that it is supplied to the vessel 31, and the other configurations are the same as those in FIG. Therefore, the description of the configuration other than the steam temperature sensor 41 will be omitted.

The steam temperature sensor 41 detects the temperature of the steam discharged from the sample container 11. The steam temperature sensor 41 outputs the detected temperature data to the controller 31.

Next, the operation of the second embodiment will be described with reference to the flowcharts shown in FIGS. 4A and 4B. First, in step S51 of FIG. 4A, the user introduces a sample to be concentrated in the sample container 11 in preparation for operating the concentrator 102. In addition, a solvent to be removed from this sample (referred to as "solvent α1") is selected.

In step S52, the user uses the ultimate pressure P0 of the decompression pump 17 at the input unit of the controller 31, the maximum heating temperature Td that can be heated in the constant temperature liquid tank 12, and the minimum cooling temperature that can be cooled by the cooling water circulator 18. Enter Te.

In step S53, the controller 31 reads the bus temperature Tb and the chiller temperature Tc.

In step S54, the controller 31 compares the freezing point Tm of the solvent selected in the process of step S51 with the chiller temperature Tc. If "Tc> Tm" (S54; YES), the process proceeds to step S56, otherwise (S54; NO), the process proceeds to step S55.

In step S55, the controller 31 resets the chiller temperature Tc. As an example, it is set to "Tc = Tm + 5 ° C.". That is, when the freezing point Tm of the solvent is lower than the chiller temperature Tc, the possibility of the solvent solidifying in the condenser 15 increases, and in order to avoid this, the chiller temperature is set to a temperature higher than the freezing point Tm. ..

In step S56, the controller 31 determines whether or not the difference between the bath temperature Tb and the chiller temperature Tc is 40 ° C. (difference threshold temperature) or more, that is, whether or not “Tb−Tc> 40 ° C.”. judge. In order to efficiently cool and recover the solvent evaporated in the sample container 11, it is desirable that the difference between the bath temperature Tb and the chiller temperature Tc is large, and in this embodiment, this difference is set to 40 ° C. .. In the process of step S56, it is determined whether or not this condition is satisfied.
If "Tb-Tc> 40 ° C."(S56; YES), the process proceeds to step S62, otherwise (S56; NO), the process proceeds to step S57.

In step S57, the controller 31 controls the heater of the constant temperature liquid tank 12 so that the bath temperature Tb is higher than the chiller temperature Tc by 40 ° C. or more.

In step S58, the controller 31 determines whether or not the bus temperature Tb has reached the maximum heating temperature Td set in the process of step S52. When the maximum heating temperature Td is reached (S58; YES), the process proceeds to step S59. If the maximum heating temperature Td is not reached (S58; NO), the process is returned to step S56.

In step S59, the controller 31 controls the cooling water circulator 18 so that the chiller temperature Tc is 40 ° C. or more lower than the bath temperature Tb. That is, if "Tb-Tc> 40 ° C." is not achieved even if the bath temperature Tb reaches the maximum heating temperature Td, control is performed to lower the chiller temperature Tc.

In step S60, the controller 31 determines whether or not the chiller temperature Tc has reached the minimum cooling temperature Te set in the process of step S52. When the minimum cooling temperature Te is reached (S60; YES), the process proceeds to step S61. If the minimum cooling temperature Te is not reached (S60; NO), the process returns to step S56.

In step S61, the controller 31 displays an error message on the display unit. That is, when "Tb-Tc> 40 ° C." cannot be achieved by increasing the bath temperature Tb and decreasing the chiller temperature Tc (when the determination in S56 is not YES), this process can be executed. Since this is not possible, an error message is displayed on the display (not shown) and this process ends.

On the other hand, when a YES determination is made in step S56, in step S62, the controller 31 sets a temperature lower than the bath temperature Tb by a predetermined temperature (for example, 20 ° C.) to a solvent to be removed (this is solvent α1). ) Is set as the target boiling point T. That is, it is set as "target boiling point T = Tb-20 ° C.". For example, when the bath temperature Tb is 40 ° C., the target boiling point T = 20 ° C. is set.

In step S63, the controller 31 calculates the target pressure P1 at which the target boiling point T of the solvent α1 is 20 ° C. using a known calculation method.

In step S64, the target pressure P1 and the ultimate pressure P0 of the decompression pump 17 set in the process of step S52 are compared. If "P1> P0", that is, if the capacity of the decompression pump 17 can reduce the pressure to the target pressure P1 (S64; YES), the process proceeds to step S66 of FIG. 4B, otherwise (S64; NO). ), Proceed to step S65.

In step S65, the controller 31 controls the heater of the constant temperature liquid tank 12 to raise the bath temperature Tb. After that, the process returns to step S53. That is, when the bath temperature Tb rises, the target boiling point T rises due to the above-mentioned relationship of "T = Tb-20 ° C.", and thus the target pressure P1 can be raised. As a result, the target pressure P1 can be made higher than the ultimate pressure P0 of the decompression pump 17. That is, "P1> P0" can be set.

In step S66 of FIG. 4B, the controller 31 inserts the sample container 11 into the constant temperature liquid tank 12 and drives the rotation drive unit 14 to rotate the sample container 11 at a constant speed. Further, the heater of the constant temperature liquid tank 12 is operated to start heating the liquid in the constant temperature liquid tank 12.

In step S67, the controller 31 operates the decompression pump 17 and starts depressurization so that the inside of the sample container 11 reaches the target pressure P1.

In step S68, when the steam temperature Ta detected by the steam temperature sensor 41 is acquired and the steam temperature Ta reaches a temperature “T + x” (for example, x = 2 ° C.) slightly higher than the target boiling point T, the solvent α1 is charged. Start distilling.

In step S69, the controller 31 controls the decompression pump 17 to maintain the target pressure P1 in the sample container 11. Therefore, the solvent α1 contained in the sample in the sample container 11 evaporates, and the solvent α1 to be removed contained in the sample can be removed.

As described above, since the boiling point of the solvent α1 is set to be 20 ° C. lower than the bath temperature Tb, the solvent α1 contained in the sample is stably evaporated and condensed without sudden boiling. It can be sent to the vessel 15.

That is, the sample in the sample container 11 can be concentrated by removing the solvent α1 to be removed from the sample introduced into the sample container 11. Further, the steam introduced into the condenser 15 is cooled by the cooling water flowing through the spiral pipe 21 and condensed, and is accumulated in the recovery liquid reservoir 16. Therefore, the solvent α1 can be recovered.

In step S70, the controller 31 determines whether or not the temperature fluctuation of the bus temperature Tb is within the allowable fluctuation temperature y based on the detection data of the bus temperature sensor 12a. If it is within the permissible fluctuation temperature y (S70; YES), the process proceeds to step S71, and if not (S70; NO), the process returns to step S69.

That is, when the fluctuation of the bath temperature Tb is large and exceeds the range of the allowable fluctuation temperature y, the processing from the processing from step S53 is repeated to set the bath temperature Tb again.

On the other hand, when the temperature fluctuation of the bath temperature Tb is within the range of the permissible fluctuation temperature y, it is determined that the solvent α1 is stably evaporated, and the process proceeds to step S71.

In step S71, when the steam temperature Ta detected by the steam temperature sensor 41 reaches a temperature "Tx" (for example, x = 2 ° C.) slightly lower than the target boiling point T of the solvent α1, the solvent is used. The distilling of α1 is completed.

After that, in step S72, the controller 31 stops the heating of the constant temperature liquid tank 12, the decompression by the decompression pump 17, and the rotation of the sample container 11 by the rotation drive unit 14, and ends this process. In this way, the solvent α1 to be removed can be removed from the sample introduced into the sample container 11 and the sample can be concentrated.

[Explanation of the effect of the second embodiment]
In this way, the concentrator 102 according to the second embodiment prevents the solvent α1 contained in the sample from suddenly boiling when concentrating the sample in the sample container 11, as in the first embodiment described above. can do. Therefore, it is possible to prevent the occurrence of problems such as the contents in the sample being released to the outside.

Further, a steam temperature sensor 41 for detecting the steam temperature Ta of the steam discharged from the sample container 11 is provided, and the steam temperature actually measured by the steam temperature sensor 41 is set to a temperature "T + x" slightly higher than the target boiling point T. When the temperature becomes high, the distillation of the vapor α1 is started. Further, when the vapor temperature reaches a temperature "Tx" slightly lower than the target boiling point T, the distillation of the solvent α1 is completed. Therefore, it is possible to recover the solvent α1 in the sample with higher efficiency.

Further, since the temperature of the cooling water sent out from the cooling water circulator 18 is controlled to be higher than the freezing point of the solvent α1, it is possible to prevent the solvent α1 recovered by the condenser 15 from freezing. ..

[Explanation of Third Embodiment]
Next, a third embodiment of the present invention will be described. Since the device configuration is the same as that in FIG. 3 described above, the description of the configuration will be omitted. In the third embodiment, when there are a plurality of solvents to be removed contained in the sample, each solvent is removed from the sample. Hereinafter, the processing procedure of the concentrator according to the third embodiment will be described with reference to the flowcharts shown in FIGS. 5A and 5B. In the examples shown in FIGS. 5A and 5B, a case where there are three types of solvents to be removed, that is, an example in which the three types of solvents α1, α2, and α3 contained in the sample are removed to concentrate the sample will be described. do.

Of the steps in the flowcharts shown in FIGS. 5A and 5B, the same steps as those shown in FIGS. 4A and 4B are given the same step numbers, and the changed steps are suffixed. It has an "a" or a different step number.

First, in step S51a of FIG. 5A, the user introduces a sample to be concentrated in the sample container 11 in preparation for operating the concentrator. In addition, a plurality of solvents to be removed are selected from this sample. As described above, in the third embodiment, three types of solvents α1, α2, and α3 are selected.

In step S52, the user uses the ultimate pressure P0 of the decompression pump 17 at the input unit of the controller 31, the maximum heating temperature Td that can be heated in the constant temperature liquid tank 12, and the minimum cooling temperature that can be cooled by the cooling water circulator 18. Enter Te.

In step S53, the controller 31 reads the liquid temperature (bath temperature Tb) in the constant temperature liquid tank 12 detected by the bath temperature sensor 12a. Further, the temperature of the cooling water (chiller temperature Tc) detected by the chiller temperature sensor 19a is read.

In step S531, the controller 31 sets “k”, which is a parameter indicating the type of solvent, to “k = 1”.

In step S54a, the controller 31 compares the freezing point Tm of the solvent αk selected in the process of step S51 with the chiller temperature Tc. If "Tc> Tm" (S54a; YES), the process proceeds to step S56, and if not (S54a; NO), the process proceeds to step S55.

Since the processes of steps S55 to S61 are the same as the processes described with reference to FIG. 4A, the description thereof will be omitted.

In step S62a, the controller 31 sets a temperature lower than the bath temperature Tb by a predetermined temperature (for example, 20 ° C.) as the target boiling point T of the solvent αk. That is, "T = Tb-20 ° C.". For example, when the bath temperature Tb is 40 ° C., the target boiling point T = 20 ° C. is set.

In step S63a, the controller 31 calculates the pressure Pk at which the target boiling point T of the solvent αk is 20 ° C. using a known calculation method.

In step S64a, the pressure Pk and the ultimate pressure P0 of the decompression pump 17 set in the process of step S52 are compared. If "Pk> P0", that is, if the pressure can be reduced to Pk by the capacity of the pressure reducing pump 17 (S64a; YES), the process proceeds to step S66 of FIG. 5B, otherwise (S64a; NO). , Step S65 proceeds with the process.

In step S65, the controller 31 controls the heater of the constant temperature liquid tank 12 to raise the bath temperature Tb. After that, the process returns to step S53. That is, when the bath temperature Tb rises, the target boiling point T rises due to the above-mentioned relationship of "T = Tb-20 ° C.", and thus the pressure Pk can be raised. As a result, the pressure Pk can be made higher than the ultimate pressure P0 of the decompression pump 17. That is, "Pk> P0" can be set.

In step S66 of FIG. 5B, the controller 31 inserts the sample container 11 into the constant temperature liquid tank 12 and drives the rotation drive unit 14 to rotate the sample container 11 at a constant speed. Further, the heater of the constant temperature liquid tank 12 is operated to start heating the liquid in the constant temperature liquid tank 12.

In step S67a, the controller 31 operates the decompression pump 17 and starts depressurization so that the pressure in the sample container 11 becomes the pressure Pk.

In step S68, when the steam temperature Ta detected by the steam temperature sensor 41 is acquired and the steam temperature Ta reaches a temperature “T + x” (for example, x = 2 ° C.) slightly higher than the target boiling point T, the solvent αk is used. Start distilling.

In step S69a, the controller 31 controls the decompression pump 17 to maintain the pressure Pk in the sample container 11. Therefore, the solvent αk contained in the sample in the sample container 11 evaporates, and the solvent αk which is the solvent to be removed contained in the sample can be removed.

As described above, since the boiling point of the solvent αk is set to be 20 ° C. lower than the bath temperature Tb, the solvent αk contained in the sample in the sample container 11 is stable without being evaporated. Can be evaporated to and sent to the condenser 15.

That is, the solution in the sample container 11 can be concentrated by removing the solvent αk to be removed from the sample introduced in the sample container 11. Further, the steam introduced into the condenser 15 is cooled by the cooling water flowing through the spiral pipe 21 and condensed, and is accumulated in the recovery liquid reservoir 16. Therefore, the solvent αk can be recovered.

In step S70, the controller 31 determines whether or not the temperature fluctuation of the bus temperature Tb is within the allowable fluctuation temperature y based on the detection data of the bus temperature sensor 12a. If it is within the permissible fluctuation temperature y (S70; YES), the process proceeds to step S71, and if not (S70; NO), the process returns to step S53.

In step S71, when the steam temperature Ta detected by the steam temperature sensor 41 becomes a temperature “Tx” (for example, x = 2 ° C.) slightly lower than the target boiling point T of the solvent αk, the solvent The distilling of α1 is completed.

In step S711, the controller 31 determines whether or not “k = 3”. If "k = 3" (S711; YES), the process proceeds to step S72, otherwise (S711; NO), the process proceeds to step S712.

In step S712, the controller 31 returns the process to step S54a with "k" as "k + 1". That is, when the distillation of the solvent α1 is completed among the three types of solvents α1, α2, and α3, the solvent α2 is continuously distilled. Then, when the distillation of all the solvents α1, α2, and α3 is completed, the process proceeds to step S72.

In step S72, the controller 31 stops the heating of the constant temperature liquid tank 12, the decompression by the decompression pump 17, and the rotation of the sample container 11 by the rotation drive unit 14, and ends this process. In this way, a plurality of solvents (solvents α1 to α3) to be removed can be removed from the solution introduced into the sample container 11 to concentrate the solution.

[Explanation of the effect of the third embodiment]
In this way, in the concentrator according to the third embodiment, when a plurality of solvents are distilled off from the solution to be concentrated, the boiling points of the respective solvents α1 to α3 are 20 ° C. with respect to the bath temperature Tb. The pressure Pk is set so that the temperature becomes as low as possible. Therefore, it is possible to stably distill off each of the solvents α1 to α3 without bumping.

Further, as in the second embodiment described above, the steam temperature sensor 41 for detecting the steam temperature Ta of the steam discharged from the sample container 11 is provided, and the steam temperature measured by the steam temperature sensor 41 is the target boiling point. Distillation of the vapor αk (k = 1-3) is started when the temperature becomes “T + x” slightly higher than T. Further, when the vapor temperature reaches a temperature "Tx" slightly lower than the target boiling point T, the distillation of the solvent α1 is completed. Therefore, it is possible to recover the solvent α1 in the sample with a higher recovery rate.

In the third embodiment, an example in which three kinds of solvents are distilled off has been described, but the present invention is not limited to this, and two kinds or four or more kinds can be used.

Although embodiments of the present invention have been described above, the statements and drawings that form part of this disclosure should not be understood to limit the invention. Various alternative embodiments, examples and operational techniques will be apparent to those skilled in the art from this disclosure.

11 Sample container 12 Constant temperature liquid tank 12a Temperature sensor (bath temperature sensor)
13 Trap ball 14 Rotating drive unit 15 Condenser 16 Recovery liquid reservoir 17 Decompression pump 18 Cooling water circulator 19 Cooling water tank 19a Chiller temperature sensor 20 Cooling water piping 21 Spiral piping 22 Lifting device 31 Controller 41 Steam temperature sensor 101, 102 Concentrator Tb bath temperature (heating temperature)
Tc chiller temperature (cooling temperature)
Td Maximum heating temperature Te Minimum cooling temperature Tm Freezing point y Allowable fluctuation temperature

Claims (6)

A concentrator that evaporates the solvent to be removed contained in the sample and concentrates the sample.
A warmer that heats the sample container into which the sample is introduced, and
A condenser that condenses the gas evaporated in the sample container, and
A cooler that cools the condenser and
A decompression pump that decompresses the inside of the sample container and
A control unit that at least controls the heating temperature by the warmer, the cooling temperature by the cooler, and the drive of the decompression pump is provided.
The control unit
A temperature obtained by subtracting a predetermined temperature from the heating temperature is set as the target boiling point, and the pressure in the sample container is reduced to the target pressure by controlling the pressure reducing pump so that the boiling point of the solvent becomes the target boiling point. ,
A concentrator characterized in that the pressure in the sample container is set as the target pressure and the sample container is heated by the warmer to evaporate the solvent. When the heating temperature changes, the control unit resets the target boiling point based on the changed heating temperature so that the boiling point of the solvent becomes the reset target boiling point. The concentrator according to claim 1, wherein the target pressure is set. The control unit sets at least one of the heating temperature and the cooling temperature so that the difference between the heating temperature by the warmer and the cooling temperature by the cooler is equal to or higher than a preset difference threshold temperature. The concentrator according to claim 1 or 2, characterized in that it is controlled. One of claims 1 to 3, wherein the cooler controls the temperature of the cooling water so that the temperature of the cooling water for cooling the condenser becomes higher than the freezing point of the solvent. The concentrator according to item 1. Further equipped with a steam temperature sensor for detecting the temperature of steam evaporated in the sample container,
The concentrator according to any one of claims 1 to 4, wherein the control unit sets the target pressure based on the steam temperature detected by the steam temperature sensor. It is a control method of a concentrator that evaporates the solvent to be removed contained in the sample and concentrates the sample.
A step of acquiring a heating temperature by a warmer that heats a sample container into which the sample is introduced and setting a temperature obtained by subtracting a predetermined temperature from the heating temperature as the target boiling point of the solvent.
A step of controlling the pressure reducing pump so that the pressure of the sample container becomes a target pressure which is a pressure at which the boiling point of the solvent is the target boiling point.
A step of heating the sample container to evaporate the solvent contained in the sample while the inside of the sample container is at the target pressure.
A method of controlling a concentrator, which comprises the above.

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