JP7398098B2 - Concentrator and method of controlling the concentrator - Google Patents

Description

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

Conventionally, concentrators (sometimes referred to as evaporators) have been used to remove specific solvents contained in samples. In a concentrator, the sample to be concentrated is introduced into a sample container such as an eggplant flask, and the sample container is then inserted into a thermostatic bath filled with a liquid such as heated water or oil while the sample container is depressurized. , warm the sample. After some time, the temperature of the sample introduced into the sample container increases and reaches the boiling point of the solvent to be removed, which evaporates and can be removed from the sample (e.g. (See Reference 1).

However, in conventional concentrators, when the boiling point temperature of the solvent is reached during heating of the sample container, the solvent contained in the sample may bump. When bumping occurs, the content of the sample is ejected to the outside due to its force, resulting in a problem that the concentration efficiency is reduced.

Japanese Patent Application Publication No. 8-266803

As described above, in conventional concentrators, there is a problem in that when the sample container is heated to remove the solvent contained in the sample, the solvent may bump, resulting in a decrease in concentration efficiency.

The present invention was made to solve such conventional problems, and its purpose is to provide a concentrating device and a concentrating device that can prevent bumping of a solvent and improve concentration efficiency. The objective is to provide a control method for

In order to achieve the above object, a concentrating device according to the present invention is a concentrating device that evaporates a solvent to be removed contained in a sample and concentrates the sample, and heats a sample container into which the sample is introduced. a condenser that condenses the gas evaporated in the sample container; a cooler that cools the condenser; a vacuum pump that reduces the pressure inside the sample container; and a temperature heated by the warmer. , a control unit that controls at least a cooling temperature by the cooler and a drive of the decompression pump, the control unit setting a temperature obtained by subtracting a predetermined temperature from the heating temperature as a target boiling point, and controlling the temperature of the solvent. 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 sample becomes the target boiling point, and the pressure in the sample container is set to the target pressure; The method is characterized in that the sample container is heated to evaporate the solvent.

A method for controlling a concentrating device according to the present invention is a method for controlling a concentrating device for concentrating a sample by evaporating a solvent to be removed contained in a sample, the method comprising heating a sample container into which the sample has been introduced. obtaining a heating temperature by a warmer, and setting the temperature obtained by subtracting a predetermined temperature from the heating temperature as the target boiling point of the solvent; and setting the pressure of the sample container to set the boiling point of the solvent as the target boiling point. a step of controlling a pressure reducing pump so that the pressure reaches a target pressure, and heating the sample container with the inside of the sample container at the target pressure to evaporate the solvent contained in the sample. It is characterized by having a step.

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

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

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is an explanatory diagram schematically showing the configuration of a concentrator according to a 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 bath 12, a trap bulb 13, a rotation drive unit 14, a condenser 15, and a collected liquid reservoir 16. , a lifting device 22, a pressure reducing pump 17, and a cooling water circulator 18. Furthermore, it is provided with a controller 31 that controls the driving of the rotation drive unit 14, the pressure reduction pump 17, and the cooling water circulator 18, and also controls the temperature of the constant temperature liquid bath 12.

The sample container 11 is, for example, an eggplant flask, a round bottom flask, an Erlenmeyer flask, etc., into which a sample to be concentrated is introduced. The sample also 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, and hexane. Furthermore, a sample may contain a single solvent or a plurality of solvents.

The constant temperature liquid bath 12 (sometimes referred to as a "water bath" or "oil bath") is filled with liquid such as water or oil, and is heated by a heater such as an electric heating wire to bring the liquid to a desired temperature. can be adjusted to By adjusting the temperature of the liquid in the constant temperature liquid tank 12 with the sample container 11 inserted into the constant temperature liquid tank 12, the sample container 11 is heated, and thus 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). Note that the method of heating the liquid (water, oil, etc.) in the constant temperature liquid tank 12 is not limited to heating wires, and other methods may also be employed. It is also possible to directly heat the sample container 11 using a heater without using a liquid. That is, the constant temperature liquid bath 12 has a function as a heater that warms the sample container 11 into which the sample is introduced.

The constant temperature liquid bath 12 is provided with a temperature sensor 12a (hereinafter referred to as "bath temperature sensor 12a") for measuring the temperature of the liquid. Detection data from the bus temperature sensor 12a is output to the controller 31.

The trap sphere 13 accumulates liquid released due to bumping when bumping occurs within the sample container 11 .

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

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

The lifting device 22 moves the sample container 11 up and down, thereby operating the sample container 11 in and out of the constant temperature liquid bath 12 .

The cooling water circulator 18 (sometimes referred to as a "chiller") includes a cooling water tank 19 that stores cooling water, and a cooling device (not shown) that cools the cooling water in the cooling water tank 19. The cooling water tank 19 is connected via a cooling water pipe 20 to a spiral pipe 21 installed in a spiral shape inside the condenser 15 . 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. A detection signal from the chiller temperature sensor 19a is output to the controller 31.

The cooling water circulator 18 cools the inside of the condenser 15 by circulating the cooling water accumulated in the cooling water tank 19 through the spiral piping 21 via the cooling water piping 20. That is, the cooling water circulator 18 has a function as a cooler that cools and liquefies the steam in the condenser 15.

The recovered liquid reservoir 16 is provided below the condenser 15 and communicates with the condenser 15, and accumulates the liquid condensed in the condenser 15. That is, since the gas (e.g., vaporized solvent) evaporated in the sample container 11 and introduced into the condenser 15 is cooled and liquefied by the cooling water flowing through the spiral pipe 21, this liquefied liquid (e.g., (solvent to be removed).

The pressure reduction pump 17 is driven under the control of the controller 31 to reduce the pressure within the condenser 15 . Since the condenser 15 is in sealing communication with the sample container 11 via the rotation drive unit 14 and the trap bulb 13, the pressure inside the sample container 11 can be reduced by reducing the pressure inside the condenser 15. Can be done. Therefore, it is possible to arbitrarily set the boiling point of the solvent introduced into the sample container 11 within a predetermined range.

The controller 31 (control unit) controls the rotation drive unit 14, the pressure reduction pump 17, and the cooling water circulator 18. Specifically, when the concentrator 101 is in operation, the controller 31 controls the pressure reducing pump 17 so that the pressure in the condenser 15 becomes a desired pressure (lower than atmospheric pressure). The controller 31 also controls the temperature of the cooling water circulated in 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 a desired temperature. The controller 31 also includes an input section (not shown) through which the user performs input operations for various data, and a display section (not shown) that displays various information. Alternatively, a touch sensor (not shown) is provided that serves both as an input section and a display section.
The controller 31 can be configured as an integrated computer including, for example, a central processing unit (CPU) and storage means such as RAM, ROM, and hard disk.

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, bumping of the solvent is prevented and the process is carried out efficiently and stably. allows the sample to be concentrated.

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

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

In step S12, the user inputs the ultimate pressure P0 of the pressure reducing pump 17, 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 in the cooling water circulator 18 at the input part of the controller 31. Enter Te. Note that the ultimate pressure P0 of the pressure reducing pump 17 refers to the minimum pressure that the pressure reducing pump 17 can reduce.

In step S13, the controller 31 reads the liquid temperature in the constant temperature liquid tank 12 (hereinafter referred to as "bath temperature Tb") detected by the bath temperature sensor 12a. Furthermore, 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 the difference between the bus temperature Tb and the chiller temperature Tc is greater than or equal to 40°C (difference threshold temperature), that is, whether "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 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 bath 12 so that the bath temperature Tb becomes 40° C. or more higher than the chiller temperature Tc.

In step S16, the controller 31 determines whether the bath temperature Tb has reached the maximum heating temperature Td set in the process of step S12. If the maximum heating temperature Td has been reached (S16; YES), the process advances to step S17. If the maximum heating temperature Td is not reached (S16; NO), the process returns to step S14.

In step S17, the controller 31 controls the cooling water circulator 18 so that the chiller temperature Tc becomes 40° C. or more lower than the bath temperature Tb. That is, if "Tb-Tc>40°C" is not achieved even when 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 the chiller temperature Tc has reached the minimum cooling temperature Te set in the process of step S12. If the lowest cooling temperature Te has been reached (S18; YES), the process advances 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, if "Tb-Tc>40°C" cannot be achieved by increasing the bus temperature Tb and decreasing the chiller temperature Tc (if YES is not determined in S14), this process cannot be executed. Since this is not possible, an error message is displayed on the display unit (not shown) and the process ends.

On the other hand, if the determination in step S14 is YES, in step S20, the controller 31 controls the temperature of the solvent to be removed by a predetermined temperature (in this embodiment, 20° C.) lower than the bath temperature Tb. (This is set as the target boiling point T of 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 is set to 20°C.

In step S21, the controller 31 uses a known calculation method to calculate the pressure at which the target boiling point T of the solvent α1 is 20° C., 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 pressure reducing pump 17 set in the process of step S12. If "P1>P0", that is, if the pressure can be reduced to the target pressure P1 with the capacity of the pressure reducing pump 17 (S22; YES), the process proceeds to step S24; otherwise (S22; NO), the process proceeds to step S24. The process advances to S23.

In step S23, the controller 31 controls the heater of the constant temperature liquid bath 12 to increase the bath temperature Tb. Thereafter, 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 "T=Tb-20°C", which in turn makes it possible to increase the target pressure P1. As a result, the target pressure P1 can be made higher than the ultimate pressure P0 of the pressure reducing pump 17. That is, "P1>P0" can be satisfied.

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 reduction pump 17 is operated to control the pressure inside the sample container 11 to the target pressure P1.

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

When the liquid in the constant temperature liquid bath 12 is heated to 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 causing bumping.

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

In step S26, the controller 31 determines whether the temperature fluctuation of the bus temperature Tb is within the range of the allowable fluctuation temperature y based on the detection data of the bus temperature sensor 12a. If it is within the range of allowable fluctuation temperature y (S26; YES), the process proceeds to step S27; otherwise (S26; NO), the process returns to step S13.

That is, if the fluctuation in the bus temperature Tb is large and exceeds the range of allowable fluctuation temperature y, the process from step S13 is repeated to reset the bus 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, if the temperature fluctuation of the bath temperature Tb is within the range of 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 the 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.

[Description of effects of the first embodiment]
In this way, in the concentrating device 101 according to the first embodiment of the present invention, the pressure inside the sample container 11 is controlled by the pressure reducing pump 17, so that the boiling point of the solvent α1 to be removed is a predetermined value lower than the bath temperature Tb. The temperature is set to be lower by a certain amount (for example, 20° C.). Therefore, when the sample container 11 is inserted into the constant temperature liquid bath 12, it is possible to prevent the solvent α1 contained in the sample from boiling. Therefore, problems such as the contents of the sample being released to the outside can be prevented, and the sample can be stably concentrated.

Further, a recovery liquid reservoir 16 is provided below the condenser 15, and stores the solvent α1 when the vapor of the solvent α1 is cooled and condensed. Therefore, it becomes possible to efficiently recover the solvent contained in the sample. Furthermore, 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 furthermore, the target pressure amount P1 is reset. Therefore, even if the bath temperature Tb changes, it is possible to follow this change and stably concentrate the sample.

In addition, the difference between the bath temperature Tb (warming temperature) of the constant temperature liquid bath 12 (warmer) and the chiller temperature Tc (cooling temperature) of the cooling water circulator 18 (cooler) is 40°C (a preset difference At least one of the bus temperature Tb and the chiller temperature Tc is controlled so that the temperature is equal to or higher than a threshold temperature (a 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.

[Description of second embodiment]
Next, a 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. The concentrating device 102 shown in FIG. 3 differs from the concentrating device 101 shown in FIG. The difference is that it is supplied to a container 31, and the other configurations are the same as in FIG. Therefore, a description of the configuration other than the steam temperature sensor 41 will be omitted.

Steam temperature sensor 41 detects the temperature of steam released from sample container 11 . Steam temperature sensor 41 outputs detected temperature data to 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 into the sample container 11 in preparation for operating the concentrator 102. In addition, a solvent to be removed from this sample (this will be referred to as "solvent α1") is selected.

In step S52, the user inputs the ultimate pressure P0 of the pressure reducing pump 17, 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 in the cooling water circulator 18 at the input part of the controller 31. Enter Te.

In step S53, the controller 31 reads the bus temperature Tb and 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, if the freezing point Tm of the solvent is lower than the chiller temperature Tc, the possibility that the solvent will solidify in the condenser 15 increases, so 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 the difference between the bus temperature Tb and the chiller temperature Tc is greater than or equal to 40°C (difference threshold temperature), that is, whether "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 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 bath 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 the bath temperature Tb has reached the maximum heating temperature Td set in the process of step S52. If the maximum heating temperature Td has been reached (S58; YES), the process advances to step S59. If the maximum heating temperature Td is not reached (S58; NO), the process returns to step S56.

In step S59, the controller 31 controls the cooling water circulator 18 so that the chiller temperature Tc becomes 40° C. or more lower than the bath temperature Tb. That is, if "Tb-Tc>40°C" is not achieved even when 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 the chiller temperature Tc has reached the minimum cooling temperature Te set in the process of step S52. If the minimum cooling temperature Te has been reached (S60; YES), the process advances 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, if "Tb-Tc>40°C" cannot be achieved by increasing the bus temperature Tb and decreasing the chiller temperature Tc (if YES is not determined in S56), this process cannot be executed. Since this is not possible, an error message is displayed on the display unit (not shown) and the process ends.

On the other hand, if the determination in step S56 is YES, in step S62 the controller 31 lowers the temperature by a predetermined temperature (for example, 20° C.) lower than the bath temperature Tb to the solvent to be removed (this ) 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 is set to 20°C.

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

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

In step S65, the controller 31 controls the heater of the constant temperature liquid bath 12 to increase the bath temperature Tb. Thereafter, 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 "T=Tb-20°C", which in turn makes it possible to increase the target pressure P1. As a result, the target pressure P1 can be made higher than the ultimate pressure P0 of the pressure reducing pump 17. That is, "P1>P0" can be satisfied.

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

In step S67, the controller 31 operates the pressure reducing pump 17 to start reducing the pressure inside the sample container 11 to the target pressure P1.

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

In step S69, the controller 31 controls the pressure reducing 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 mentioned 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 can be stably evaporated and condensed without bumping. It can be sent to the device 15.

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

In step S70, the controller 31 determines whether the temperature fluctuation of the bus temperature Tb is within the range of the allowable fluctuation temperature y based on the detection data of the bus temperature sensor 12a. If it is within the range of allowable fluctuation temperature y (S70; YES), the process proceeds to step S71; otherwise (S70; NO), the process returns to step S69.

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

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

In step S71, the controller 31 controls the solvent when the steam temperature Ta detected by the steam temperature sensor 41 reaches a temperature "Tx" (for example, x=2° C.) that is slightly lower than the target boiling point T of the solvent α1. Finish the distillation of α1.

Thereafter, in step S72, the controller 31 stops the heating of the constant temperature liquid bath 12, the pressure reduction by the pressure reducing 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.

[Description of effects of second embodiment]
In this way, in the concentrating device 102 according to the second embodiment, as in the first embodiment described above, bumping of the solvent α1 contained in the sample is prevented when concentrating the sample in the sample container 11. can do. Therefore, it is possible to prevent problems such as the contents of the sample being released to the outside.

Furthermore, a steam temperature sensor 41 is provided to detect the steam temperature Ta of the steam released from the sample container 11, and the steam temperature actually measured by the steam temperature sensor 41 is a temperature "T+x" slightly higher than the target boiling point T. At this point, the distillation of the solvent 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 becomes possible to recover the solvent α1 in the sample with higher efficiency.

Furthermore, 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 in the condenser 15 from freezing. .

[Description of third embodiment]
Next, a third embodiment of the present invention will be described. Since the device configuration is the same as that shown in FIG. 3 described above, a description of the configuration will be omitted. In the third embodiment, when there are multiple 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. Note that the examples shown in FIGS. 5A and 5B describe a case where there are three types of solvents to be removed, that is, an example in which three types of solvents α1, α2, and α3 contained in the sample are removed to concentrate the sample. do.

Note that among the steps in the flowcharts shown in FIGS. 5A and 5B, the steps that are the same as those shown in FIGS. 4A and 4B are given the same step numbers, and the steps that have been changed are indicated by ``a'' or a different step number.

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

In step S52, the user inputs the ultimate pressure P0 of the pressure reducing pump 17, 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 in the cooling water circulator 18 at the input part of the controller 31. Enter Te.

In step S53, the controller 31 reads the liquid temperature in the constant temperature liquid tank 12 (bath temperature Tb) detected by the bath temperature sensor 12a. Furthermore, 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; otherwise (S54a; NO), the process proceeds to step S55.

The processing in steps S55 to S61 is the same as the processing explained with reference to FIG. 4A, so the explanation 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 is set to 20°C.

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

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

In step S65, the controller 31 controls the heater of the constant temperature liquid bath 12 to increase the bath temperature Tb. Thereafter, 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 as a result, the pressure Pk can be increased. As a result, the pressure Pk can be made higher than the ultimate pressure P0 of the pressure reducing pump 17. That is, "Pk>P0" can be satisfied.

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

In step S67a, the controller 31 operates the pressure reducing pump 17 to start reducing the pressure in the sample container 11 to the pressure Pk.

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

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

As mentioned 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 can be stably heated without bumping. It can be evaporated and sent to the condenser 15.

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

In step S70, the controller 31 determines whether the temperature fluctuation of the bus temperature Tb is within the range of the allowable fluctuation temperature y based on the detection data of the bus temperature sensor 12a. If it is within the range of allowable fluctuation temperature y (S70; YES), the process proceeds to step S71; otherwise (S70; NO), the process returns to step S53.

In step S71, the controller 31 controls the solvent to Finish the distillation of α1.

In step S711, the controller 31 determines whether "k=3". If "k=3" (S711; YES), the process advances to step S72; otherwise (S711; NO), the process advances to step S712.

In step S712, the controller 31 sets "k" to "k+1" and returns the process to step S54a. That is, among the three types of solvents α1, α2, and α3, when solvent α1 has been distilled off, solvent α2 is subsequently distilled off. When all the solvents α1, α2, and α3 have been distilled off, the process proceeds to step S72.

In step S72, the controller 31 stops heating the thermostatic liquid bath 12, reducing the pressure by the pressure reducing pump 17, and stopping the rotation of the sample container 11 by the rotation drive unit 14, and ends this process. In this way, it is possible to remove a plurality of solvents (solvents α1 to α3) that are the solvents to be removed from the solution introduced into the sample container 11, and to concentrate the solution.

[Description of effects of third embodiment]
In this manner, in the concentrating device according to the third embodiment, when a plurality of solvents are distilled off from a solution to be concentrated, the boiling point of each of the solvents α1 to α3 is 20°C with respect to the bath temperature Tb. The pressure Pk is set so that the temperature is as low as possible. Therefore, it is possible to stably distill off each of the solvents α1 to α3 without causing bumping.

Further, as in the second embodiment described above, a steam temperature sensor 41 is provided to detect the steam temperature Ta of the steam released from the sample container 11, and the steam temperature actually measured by the steam temperature sensor 41 is the target boiling point. When the temperature reaches "T+x" which is slightly higher than T, distillation of the solvent αk (k=1 to 3) is started. Furthermore, 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 becomes possible to recover the solvent α1 in the sample with a higher recovery rate.

Although the third embodiment describes an example in which three types of solvents are distilled off, the present invention is not limited to this, and it is also possible to use two or four or more types.

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

11 Sample container 12 Constant temperature liquid bath 12a Temperature sensor (bath temperature sensor)
13 Trap bulb 14 Rotation 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 (5)

A concentrator for concentrating the sample by evaporating a solvent to be removed contained in the sample,
a warmer that warms a sample container into which the sample is introduced;
a condenser that condenses the gas evaporated in the sample container;
a cooler that cools the condenser;
a vacuum pump that reduces the pressure inside the sample container;
A control unit that controls at least a heating temperature by the warmer, a cooling temperature by the cooler, and a drive of the decompression pump,
The control unit includes:
A temperature obtained by subtracting a predetermined temperature from the heating temperature is set as a 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 concentrating device characterized in that the pressure inside the sample container is set to the target pressure, and the sample container is heated by the heater 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 concentrating device according to claim 1, further comprising: setting the target pressure. The control unit controls 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 concentrating device according to claim 1 or 2, characterized in that: Any 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 is higher than the freezing point of the solvent. The concentrator according to item 1. A method for controlling a concentrator that evaporates a solvent to be removed contained in a sample to concentrate the sample, the method comprising:
obtaining a heating temperature by a heater 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 a target boiling point of the solvent;
controlling a pressure reduction pump so that the pressure in the sample container is a target pressure that makes the boiling point of the solvent the target boiling point;
heating the sample container while the inside of the sample container is at the target pressure to evaporate the solvent contained in the sample;
A method for controlling a concentrator, comprising :

Images