WO2013035755A1 - Concentrating device - Google Patents

Abstract

According to an embodiment of the present invention, a concentrating device has a plurality of containers for accommodating a liquid containing a volatile substance, and a discharge means for discharging the inside of the plurality of containers. The plurality of containers and the discharge means are connected via a chamber. The containers have an opening, and the opening is closed by a stopper. The stopper is connected to the chamber, a through-hole is formed so that the chamber and the containers are connected, and an outside-gas-introduction unit for introducing outside gas to the inside of the containers is formed.

Description

Concentrator

One embodiment of the present invention relates to a concentrator.

As a device for vaporizing a volatile substance in a liquid in a test tube, in recent years, a concentrating device is known in which the inside of a container is depressurized to exhaust a gas, vaporize the volatile substance, and concentrate the liquid. However, even if external gas is introduced, the inside of the container is unavoidably in a reduced pressure state. In the reduced pressure state, if the liquid is not stirred and sufficiently flows, there is a problem that bumping occurs due to the concentration of volatile substances in the liquid and uneven temperature, and as a result, the liquid scatters. .

In Patent Document 1, as a volatile substance distilling device for distilling off a volatile substance from a sample solution, one or more volatile substance distilling containers containing the sample solution and a volatile substance distilling container are provided. A configuration including a decompression means for decompressing is disclosed. At this time, the volatile substance evaporating container has a container for storing the sample solution and a volatile substance evaporating stopper for closing the opening of the sample container. In addition, the stopper is provided with a through-hole through which vaporized volatile substances are discharged, and a gas inlet to the container is provided at the upper edge of the stopper, and the gas introduced at the lower edge is introduced into the sample container. A gas outlet for contacting with the solution is provided, and a groove connecting the gas inlet and the gas outlet is formed on the side surface of the stopper.

However, it is desired that volatile substances are distilled away from a plurality of sample solutions at the same time and concentrated uniformly.

International Publication No. 2008/078765

One embodiment of the present invention provides a concentrating device capable of distilling volatile substances from a liquid containing a plurality of volatile substances at the same time and concentrating them uniformly in view of the above-described problems of the prior art. With the goal.

In one embodiment of the present invention, the concentrating device includes a plurality of containers in which a liquid containing a volatile substance is accommodated, and an exhaust unit that exhausts the inside of the plurality of containers, and the plurality of containers and the exhaust unit Are connected through a chamber, the container has an opening, the opening is closed by a stopper, the stopper is connected to the chamber, and the chamber and the container are connected to each other. A through hole is formed so as to connect each other, and an external gas introduction part for introducing an external gas into the container is formed.

According to an embodiment of the present invention, it is possible to provide a concentrating device capable of distilling volatile substances from a liquid containing a plurality of volatile substances simultaneously and concentrating them uniformly.

It is a sectional side view which shows the structure of 1st embodiment of the concentration apparatus of this invention. It is a perspective view which shows the structure of the well plate of FIG. It is a side view which shows the structure of the stopper of FIG. It is a perspective view which shows the structure of the stopper of FIG. It is a sectional side view explaining the effect | action of the concentration apparatus of FIG. It is a sectional side view which shows the modification of the concentration apparatus of FIG. It is a sectional side view which shows the modification of the baseplate of the chamber of FIG. It is a sectional side view which shows the modification of the connection part of the stopper of FIG. 1, and the bottom plate of a chamber. It is a sectional side view which shows the modification of the connection part of the stopper of FIG. 1, and the bottom plate of a chamber. It is a side view which shows an example of the stopper used for 2nd embodiment of the concentration apparatus of this invention. It is a sectional side view which shows an example of the stopper used for 2nd embodiment of the concentration apparatus of this invention. It is a sectional side view which shows an example of the stopper used for 2nd embodiment of the concentration apparatus of this invention. It is a sectional side view which shows an example of the connection method of the stopper of FIG. 8A, and a chamber. It is a sectional side view which shows an example of the connection method of the stopper of FIG. 8A, and a chamber. It is a perspective view which shows an example of the fixing method of the chamber and well plate of FIG. 9B.

Next, an embodiment for carrying out the present invention will be described with reference to the drawings.

FIG. 1 shows the structure of the first embodiment of the concentrating device of the present invention.

The concentrating device 1 has 96 microtubes 11 in which a liquid containing a volatile substance is accommodated, and a pump 40 that exhausts the insides of the 96 microtubes. The 96 microtubes 11 and the pumps 40 are Are connected via a chamber 30. The microtube 11 has an opening, and the opening is closed by a stopper 20. The plug 20 is directly connected to the chamber 30, and a through hole is formed so as to connect between the chamber 30 and the microtube 11.

The volatile substance is not particularly limited, but methanol, ethyl acetate, water, ethanol, propanol, butanol, acetone, methyl ethyl ketone, acetonitrile, acetic acid, hexane, diethyl ether, chloroform, methylene chloride, N, N-dimethylformamide (DMF) ), A solvent such as dimethyl sulfoxide (DMSO), and a metal halide such as aluminum chloride.

FIG. 2 shows the structure of the well plate 10.

The 96 microtubes 11 are a part of the well plate 10 held by the plate 12 in a state of being arranged in a grid of 12 rows and 8 columns.

The material constituting the well plate 10 is not particularly limited, and examples thereof include resins such as polypropylene, polystyrene, polytetrafluoroethylene, and fluororubber, metals such as stainless steel and titanium, and glass.

The microtube 11 has a bottomed cylindrical shape that tapers downward in the figure, and has a volume of 0.1 to several mL. The upper end of each microtube 11 protrudes slightly upward from the plate 12.

Note that the number of microtubes 11 held by the plate 12 is not limited to 96.

Also, instead of the well plate 10, a container such as a single microtube 11 or a test tube can be used.

3A and 3B show the structure of the plug 20.

The stopper 20 closes the opening of one microtube 11 of the well plate 10 and there are 96 pieces. The plug 20 has a substantially cylindrical shape as a whole, and is long in the longitudinal direction of the microtube 11.

The material constituting the stopper 20 is not particularly limited as long as it has chemical resistance and corrosion resistance, and examples thereof include glass, titanium, stainless steel, polytetrafluoroethylene, and fluororubber.

The stopper 20 has a main body portion 21 inserted into the microtube 11 and a screw portion 22 inserted into the chamber 30. A through hole 23 is formed in a region including the central axis of the stopper 20.

The through hole 23 may not be formed in a region including the central axis of the plug 20.

The screw portion 22 has a smaller diameter than the main body portion 21 and is fitted with a screw hole 32 formed in the bottom plate 31 of the chamber 30 as described later.

Note that the screw portion 22 may be omitted, and the stopper and the chamber may be connected via a pipe in the same manner as in the second embodiment of the concentrating device of the present invention described later.

The main body 21 has a columnar shape at the top, and a truncated cone shape with a tapered bottom in the figure. The difference between the outer diameter of the main body 21 and the inner diameter of the microtube 11 is usually 5% or less of the inner diameter of the microtube 11 and preferably 1% or less of the inner diameter of the microtube 11. If the difference between the outer diameter of the main body portion 21 and the inner diameter of the microtube 11 exceeds 5% of the inner diameter of the microtube 11, the gap between the microtube 11 and the main body portion 21 becomes large, making it difficult to make it airtight. As a result, much of the external gas is introduced into the inside of the microtube 11 from the gap, and the liquid containing the volatile substance in each microtube 11 may be prevented from being uniformly stirred.

In the upper part of the main body 21, a groove 24 is formed in a spiral shape in order to introduce an external gas into the microtube 11. The cross-sectional shape of the groove 24 is a square, but is not necessarily a square. The angle of the groove 24 with respect to the lower surface 21a of the main body 21, that is, the surface orthogonal to the central axis direction of the main body 21 is usually 10 to 45 °, and preferably 15 to 25 °.

As shown in FIG. 4, the plug 20 is inserted into the microtube 11 at a length of about ¼ from the bottom of the main body 21.

It is possible to use exhaust means such as an aspirator instead of the pump 40.

The chamber 30 has a quadrangular frustum shape, and has a rectangular bottom plate 31 having substantially the same dimensions as the well plate 10 and a side plate 33 inclined inwardly upward from the four sides of the bottom plate 31. The bottom plate 31 is thicker than the side plate 33.

The material constituting the chamber 30 is not particularly limited as long as it has pressure resistance, chemical resistance, and corrosion resistance, and examples thereof include stainless steel, titanium, and polytetrafluoroethylene.

The volume of the chamber 30 is usually not less than the total volume of the microtube 11 and preferably not less than three times the total volume of the microtube 11. If the volume of the chamber 30 is less than the total volume of the microtubes 11, the liquid containing the volatile substance in each microtube 11 may be prevented from being uniformly stirred. On the other hand, the volume of the chamber 30 is usually 300 times or less of the total volume of the microtube 11.

In addition to the chamber 30, a buffer tank can be installed in the vicinity of the pump 40.

A screw hole 32 is formed at a position of the bottom plate 31 corresponding to each microtube 11 of the well plate 10. The screw hole 32 is fitted with the screw portion 22 of the plug 20. When the screw portion 22 is completely fitted into the screw hole 32, the upper surface of the main body portion 21 of the plug 20 comes into contact with the lower surface of the bottom plate 31 as shown in FIG. 4.

In order to improve the adhesion between the stopper 20 and the bottom plate 31, an O-ring or gasket can be sandwiched between the upper surface of the main body 21 and the lower surface of the bottom plate 31.

Also, a sealing method in which the threaded portion 21 is processed into a taper shape and a sealing tape or the like is attached can be employed.

The pump 40 is not particularly limited, and examples thereof include a vacuum pump and a decompression pump.

The exhaust amount of the pump 40 is usually 1 to 500 L / min, and preferably 10 to 300 L / min.

In order to improve the airtightness between the stopper 20 and the well plate 10, as shown in FIG. 4, a space between the stopper 20 and each microtube 11 of the well plate 10 is sealed with a pressing plate 50 and a sealing plate 60. Has been.

The holding plate 50 is a rectangular plate having a uniform thickness, and holes are formed at positions corresponding to the microtubes 11 of the well plate 10.

The hole diameter of the pressing plate 50 is substantially equal to the diameter of the main body 21 of the stopper 20.

The material constituting the pressing plate 50 is not particularly limited, and examples include stainless steel, resin, and carbon materials (graphite and carbon fiber).

The seal plate 60 is a flexible sheet, and holes are formed at positions corresponding to the microtubes 11 of the well plate 10 as with the press plate 50.

The hole diameter of the seal plate 60 is preferably slightly smaller than the diameter of the main body 21 of the plug 20.

The material constituting the seal plate 60 is not particularly limited as long as it has flexibility, and examples thereof include silicone rubber and fluorine rubber.

The thickness of the seal plate 60 is usually 0.1 mm or more. If the thickness of the seal plate 60 is less than 0.1 mm, the sealing effect may be insufficient. On the other hand, the thickness of the seal plate 60 is usually 5 mm or less.

The main body 21 of the plug 20 is inserted into the holes arranged in the vertical direction of the holding plate 50 and the seal plate 60, and the lower surface of the seal plate 60 comes into contact with the upper surface of each microtube 11 of the well plate 10. At this time, the hole diameter of the seal plate 60 is slightly smaller than the diameter of the main body portion 21 of the stopper 20, and the seal plate 60 has flexibility. Therefore, when the main body portion 21 is inserted through the hole of the seal plate 60, The hole of the seal plate 60 is enlarged. Then, the inner peripheral surface of the hole of the seal plate 60 is brought into close contact with the main body portion 21 by a force that the hole of the seal plate 60 tends to contract. Furthermore, the pressing plate 50 presses the seal plate 60 downward in the drawing by its own weight, and improves the adhesion between the seal plate 60 and the upper surface of the microtube 11.

Next, an example of a procedure for attaching the concentrating device 1 will be described.

First, the screw portion 22 of the plug 20 is fitted into each screw hole 32 of the bottom plate 31 of the chamber 30.

Next, the presser plate 50 and the seal plate 60 are overlapped so that the presser plate 50 is on the upper side and the seal plate 60 is on the lower side in the figure, and the plugs 20 are inserted through the holes arranged vertically.

Then, a liquid containing a volatile substance is accommodated in the microtube 11 of the well plate 10, and the opening of each microtube 11 is closed with the stopper 20. The plug 20 is inserted into the microtube 11 at a length of about ¼ from the bottom of the main body 21. Then, the seal plate 60 and the holding plate 50 are slid downward in the drawing along the main body portion 21 of the stopper 20, and the lower surface of the seal plate 60 is brought into contact with the upper surface of the microtube 11.

Next, the operation of the concentration apparatus 1 will be described.

When the pump 40 is operated, the air in the chamber 30 is exhausted and the pressure in the chamber 30 is reduced. At this time, since the chamber 30 functions as a buffer tank, a sudden pressure change in the chamber 30 can be avoided, and the inside of the chamber 30 is decompressed almost uniformly. Thereby, the air in each microtube 11 is exhausted almost uniformly into the chamber 30 through the through-hole 23 of each plug 20, and the inside of the microtube 11 is decompressed almost uniformly. Then, external gas is introduced into the microtube 11 from the groove 24 of the plug 20. As shown in FIG. 4, a portion of about 2/3 from the top of the groove 24 is opened to the outside, and a portion of about 1/3 from the bottom of the groove 24 is formed by the seal plate 60, the holding plate 50, and the microtube 11. Surrounded by a spiral passage. The external gas is introduced into the microtube 11 through a spiral passage. As shown in FIG. 4, the introduced external gas is considered to rotate spirally along the inner wall of the microtube 11 by centrifugal force while colliding with the inner wall of the microtube 11. When such an air flow is generated in the microtube 11, a liquid containing a volatile substance is rolled up and stirred to form a liquid surface having a recessed center. As a result, the surface area of the liquid is increased and vaporization of the volatile substance is activated. The vaporized volatile substance is exhausted from the through hole 23 of the plug 20 into the chamber 30.

The external gas is not particularly limited, and examples thereof include air.

The external gas may not be normal pressure as long as it can be introduced into the microtube 11.

In addition, when the liquid containing a volatile substance is easy to oxidize, you may use inert gas, such as nitrogen and argon, as external gas. Specifically, a space between the bottom plate 31 of the chamber 30 and the pressing plate 50 around the main body portion 21 of the plug 20 is sealed, and a pipe extending from an inert gas source is connected to this space.

The ratio of the cross-sectional area of the groove 24 to the cross-sectional area of the main body 21 of the plug 20 is usually 0.4 to 10%, preferably 1.6 to 3.5%. When the ratio of the cross-sectional area of the groove 24 to the cross-sectional area of the main body portion 21 of the plug 20 is less than 0.4%, the external gas introduced from the groove 24 reaches the bottom of the microtube 11 and the liquid flows into the microtube. 11 may be blown up to the top. On the other hand, when the ratio of the cross-sectional area of the groove 24 to the cross-sectional area of the main body 21 of the plug 20 exceeds 10%, the external gas introduced from the groove 24 reaches only the upper part of the liquid, and the volatile substance is vaporized. The promoting effect may not be sufficient.

The cross-sectional area in the ratio of the cross-sectional area of the groove 24 to the cross-sectional area of the main body 21 of the plug 20 means the area of the cross section of the plug 20 perpendicular to the central axis direction of the main body 21.

FIG. 5 shows a modification of the concentrator 1. The concentrating device 2 has the same configuration as the concentrating device 1 except that a plug 20 ′ having a main body 21 ′ is used in place of the plug 20 and the pressing plate 50 is omitted.

The main body portion 21 ′ has the same configuration as the main body portion 21 except that a flange portion 25 protruding outward is formed. The flange portion 25 is formed so as not to block the groove 24. The lower surface of the flange portion 25 of the plug 20 is in contact with the upper surface of the seal plate 60. Thereby, the adhesiveness of the main-body part 21 'of the stopper 20 and the microtube 11 can be improved.

FIG. 6 shows a modification of the bottom plate 31 of the chamber 30.

The bottom plate 31 ′ has the same configuration as the bottom plate 31 except that a cylindrical peripheral wall 31 a ′ is formed around the screw hole 32. Thereby, even if liquid, such as a condensate of a volatile substance, exists on the baseplate 31 ', the inflow of the liquid into the screw hole 32 can be suppressed.

7A and 7B show a modified example of the connecting portion between the stopper 20 and the bottom plate 31 of the chamber 30. FIG.

In FIG. 7A, a packing 26 is disposed on the screw portion 22 of the plug 20. Thereby, the airtightness between the stopper 20 and the bottom plate 31 of the chamber 30 can be improved.

The packing 26 is not particularly limited, and examples include a washer type, an O-ring type, and a no-seal type.

In FIG. 7B, a check valve 34 is disposed in the screw hole 32 of the bottom plate 31. The check valve 34 allows gas to flow from the through hole 23 of the stopper 20 to the chamber 30 and disables gas flow in the opposite direction. Thereby, even if liquids, such as a condensate of a volatile substance, exist on the baseplate 31, the inflow from the screw hole 32 of the liquid to the through-hole 23 of the plug 20 can be suppressed. Furthermore, the rapid decompression inside the microtube 11 can be suppressed, and the inside of the microtube 11 can be gradually decompressed.

Next, a second embodiment of the concentration apparatus of the present invention will be described.

The second embodiment of the concentrator of the present invention has the same configuration as the concentrator 1 except for the shape of the stopper and the method of connecting the stopper and the chamber.

FIG. 8A, FIG. 8B, and FIG. 8C show examples of stoppers used in the second embodiment of the concentration apparatus of the present invention.

The stopper 80 </ b> A has a disc portion 81 that closes the opening of the microtube 11 and a cylindrical portion 82 that is inserted into the opening of the microtube 11. A through hole 83 is formed in a region including the central axis of the plug 80A so as to connect the chamber 30 and the microtube 11. Further, a pipe 84 for introducing external gas into the microtube 11 passes through a position away from the center of the plug 80A. An end 84a of the pipe 84 on the inner side of the microtube 11 is inclined with respect to a plane orthogonal to the central axis direction of the plug 80A.

The inclination angle of the end 84a of the pipe 84 with respect to the plane orthogonal to the central axis direction of the plug 80A is usually 10 to 45 °, and preferably 15 to 25 °.

The stopper 80 </ b> B has a disc portion 81 that closes the opening of the microtube 11 and a cylindrical portion 82 ′ that is inserted into the microtube 11. A through hole 83 is formed in the region including the central axis of the plug 80B so as to connect the chamber 30 and the microtube 11. A nozzle 85 is attached to the inner peripheral surface of the cylindrical portion 82 '. The suction port of the nozzle 85 is connected to the inner end portion of the microtube 11 of the pipe 86 that passes through the cylindrical portion 82 ′ and introduces external gas. The blowing angle of the nozzle 85 is inclined with respect to a plane orthogonal to the central axis direction of the plug 80B.

The inclination angle of the blowing angle of the nozzle 85 with respect to the plane orthogonal to the central axis direction of the plug 80B is usually 10 to 45 °, and preferably 15 to 25 °.

The plug 80 </ b> C has a disc portion 81 that closes the opening of the microtube 11 and a cylindrical portion 82 ′ that is inserted into the microtube 11. A through hole 83 is formed in a region including the central axis of the plug 80C so as to connect the chamber 30 and the microtube 11. A pipe 87 for introducing an external gas passes through the cylindrical portion 82 '. An end 87a on the inner side of the micro tube 11 of the pipe 87 is disposed along the inner wall of the cylindrical portion 82 '. An end portion 87a of the pipe 87 is inclined with respect to a plane orthogonal to the central axis direction of the plug 80C.

The inclination angle of the end portion 87a of the pipe 87 with respect to the plane perpendicular to the central axis direction of the plug 80C is usually 10 to 45 °, and preferably 15 to 25 °.

In the plugs 80A, 80B, and 80C, a pipe communicating with the chamber 30 is inserted into the through hole 83. When the inside of the microtube 11 is exhausted through the pipe inserted into the through hole 83, external gas is introduced into the microtube 11 from the pipes 84, 87 or the nozzle 85. At this time, the external gas is considered to rotate spirally along the inner wall of the microtube 11 by centrifugal force while colliding with the inner wall of the microtube 11, as in the concentration device 1. When such an air flow is generated in the microtube 11, a liquid containing a volatile substance is rolled up and stirred to form a liquid surface having a recessed center. As a result, the surface area of the liquid is increased and vaporization of the volatile substance is activated. The vaporized volatile substance is exhausted into the chamber 30 through a pipe inserted into the through hole 83 of the plugs 80A, 80B, and 80C.

9A and 9B show an example of a method for connecting the stopper 80A and the chamber. The plugs 80B and 80C can be connected to the chamber in the same manner as the plug 80A.

In FIG. 9A, a pipe 90 is hermetically inserted into the through hole 83 of the plug 80A. The end of the pipe 90 opposite to the plug 80A is inserted and welded into a hole 32A formed in the bottom plate 31 of the chamber 30A.

In FIG. 9B, the pipe 90 is inserted airtightly into the through hole 83 of the plug 80A. A hole 32B is formed in the bottom plate 31 of the chamber 30B, and a one-touch joint 35 is attached to the hole 32 '. The end of the pipe 90 opposite to the plug 80A is connected to the one-touch joint 35. Since the one-touch joint 35 has a generally airtight structure, the pipe 90 can be connected to the bottom plate 31 in an airtight manner.

In the present embodiment, the sealing plate 60 (see the drawing) can also be used as in the concentration device 2. Further, similarly to the bottom plate 31 ', a cylindrical peripheral wall 31a' (see FIG. 6) can be formed around the hole 32A (or 32B) of the bottom plate 31 of the chamber 30A (or 30B).

FIG. 10 shows an example of a method for fixing the chamber 30B and the well plate 10. The chamber 30A can also be connected to the well plate 10 in the same manner as the chamber 30B.

On the three side surfaces of the plate 12 of the well plate 10, overhang portions 13 projecting outward are formed. Each overhang portion 13 is formed with a through hole in a direction substantially perpendicular to the plate 12. In addition, overhanging portions 36 projecting outward are also formed on the three side surfaces of the bottom plate 31 of the chamber 30B. In each overhang portion 36, a through hole is formed in a direction substantially perpendicular to the plate 12.

The guide rod 100 is inserted through the through holes of the overhang portions 13 and 36. When the plate 12 of the well plate 10 is raised along each guide rod 100, the plug 80A that closes each microtube 11 of the well plate 10 is connected to the one-touch joint 35 attached to each hole 32B of the bottom plate 31 of the chamber 30B. Connecting. By using the guide rod 100, each microtube 11 of the well plate 10 and each hole 32B of the chamber 30B can be positioned accurately, and both can be connected or disconnected.

In particular, by using three guide rods 100, the plate 12 of the well plate 10 can be reliably raised and lowered while being held substantially parallel to the bottom plate 31 of the chamber 30B.

Note that four or more overhang portions 13 and 36 may be formed, and four or more guide rods 100 may be used.

This international application claims priority based on Japanese Patent Application 2011-193664 filed on September 6, 2011, and the entire contents of Japanese Patent Application 2011-193664 are incorporated herein by reference. .

1, 2 Concentrator 10 Well plate 11 Micro tube 12 Plate 20 Plug 23 Through hole 24 Groove 30, 30A, 30B Chamber 40 Pump 80A, 80B, 80C Plug 83 Through hole 84, 86, 87 Pipe 85 Nozzle 90 Pipe

Claims (6)

A plurality of containers containing liquids containing volatile substances;
An exhaust means for exhausting the interior of the plurality of containers;
The plurality of containers and the exhaust means are connected via a chamber, the container has an opening, and the opening is closed by a stopper,
The stopper is connected to the chamber, a through hole is formed so as to connect between the chamber and the container, and an external gas introduction part for introducing an external gas into the container is formed. A concentrating device characterized by that. The concentration device according to claim 1, wherein a ratio of a volume of the chamber to a volume of the plurality of containers is 3 or more. The concentrating device according to claim 1, wherein the external gas introduction part is a pipe line. The concentrator according to claim 1, wherein the external gas introduction part is a groove formed in a spiral shape along a side surface of the stopper. The concentrator according to claim 1, wherein the stopper and the chamber are connected via a conduit. The container is a microtube;
The concentration apparatus according to claim 1, further comprising a well plate in which the plurality of microtubes are held in a state of being arranged in a lattice pattern by the plate.

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