JP2015085295A - Centrifugal vacuum concentrator - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a centrifugal vacuum concentration device which directly and uniformly heats a sample solution and efficiently condenses and dries the sample solution in a short time.SOLUTION: A centrifugal vacuum concentration device includes: a cup shaped vacuum vessel 11 having a lid member 11 for opening and closing an upper opening; a metal rotary heating element 12 which is rotatably provided in the vacuum vessel; rotary driving means 13 which rotates the rotary heating element; exhaust means 14 which decompresses the vacuum vessel; a sample vessel holding part 15 provided at the rotary heating element; and a magnet 16 which generates an eddy current in the rotary heating element by electromagnetic induction to cause the heating element to produce heat.

Description

  The present invention relates to a centrifugal vacuum concentration apparatus, and more particularly, to a centrifugal vacuum concentration apparatus for concentrating the sample solution or drying the sample by heating the sample solution while applying a centrifugal force in a decompressed vacuum container. .

  The centrifugal vacuum concentrator (centrifugal evaporator) evacuates the vacuum vessel while rotating the vacuum vessel in a state where the sample vessel into which the sample solution is injected is supported on a rotating body provided rotatably in the vacuum vessel. By rotating the rotating body at a high speed, the sample solution is concentrated and the sample is dried. By arranging a heater on the inner peripheral surface of the vacuum vessel, the sample solution during the concentration operation can be heated. (For example, refer to Patent Document 1). Further, as a means for heating the object to be heated in the metal container, a rotating body is disposed so as to surround the metal container, and a plurality of permanent magnets are alternately arranged with N poles and S poles on the rotating body. Such an arrangement is known (for example, see Patent Document 2).

JP 2002-331120A JP 2004-76992 A

  However, in the case where the heater is disposed on the inner peripheral surface of the vacuum vessel, the inside of the vacuum vessel is in a reduced pressure state, and the heater and the rotating body are not in contact with each other. ), And only the outer peripheral surface of the vacuum vessel of the sample container is heated, so that sufficient heat cannot be transferred to the sample solution, which may cause uneven heating and uneven evaporation. There were difficulties in efficiency.

  Moreover, although the heating means described in Patent Document 2 is effective for an apparatus in which a sample solution is directly stored in a metal container, it is possible to heat the sample solution held by the rotating body in the vacuum container. In addition, since only the peripheral wall of the vacuum vessel is heated, the heating efficiency of the sample solution in the centrifugal vacuum concentration apparatus cannot be improved.

  Accordingly, an object of the present invention is to provide a centrifugal vacuum concentration apparatus that can directly and evenly heat a sample solution and can efficiently concentrate and dry the sample solution in a short time.

  To achieve the above object, the centrifugal vacuum concentrator of the present invention opens and closes an upper opening in a centrifugal vacuum concentrator for concentrating the sample solution by applying a centrifugal force to the sample solution in a vacuumed vacuum vessel. A bottomed cylindrical vacuum vessel having a lid member, a metal rotary heating element rotatably provided in the vacuum vessel, a rotation driving means for rotating the rotary heating element, and the inside of the vacuum vessel An exhaust means for reducing the pressure, a sample container holding portion provided in the rotary heating element, and a magnet for generating heat by generating an eddy current by electromagnetic induction in the rotary heating element are provided.

  Furthermore, the centrifugal vacuum concentrator of the present invention is characterized in that the rotating heating element is formed of an aluminum alloy, a copper alloy or low carbon steel, and the sample container holding portion is provided on the rotating heating element. It is characterized in that it is a cylindrical container holding part or a container holding hole drilled in the rotary heating element. Furthermore, the magnet is provided on the outer periphery of the vacuum vessel, or is provided below the bottom surface of the vacuum vessel.

  According to the centrifugal vacuum concentrator of the present invention, the rotating heating element is heated by the eddy current generated by electromagnetic induction, so that the sample solution is efficiently heated via the sample container holding portion provided in the generated heating heating element. be able to. Thereby, even a solvent having a high boiling point can be evaporated in a short time, so that concentration and drying of the sample solution can be performed efficiently and in a short time.

It is a schematic sectional drawing which shows the 1st form example of the centrifugal vacuum concentration apparatus of this invention. It is a schematic sectional drawing which shows the 2nd form example of the centrifugal vacuum concentration apparatus of this invention.

  FIG. 1 is a schematic cross-sectional view showing a first embodiment of a centrifugal decompression / concentration device of the present invention. The centrifugal decompression / concentration device is a bottomed cylindrical vacuum vessel 11 and rotates inside the vacuum vessel 11. Provided to the rotary heating element 12, the rotary heating element 12 that can be provided, a driving means 13 that rotates the rotary heating element 12, a vacuum pump 14 that is an exhaust means for reducing the pressure inside the vacuum vessel 11, and the rotary heating element 12. A plurality of sample container holding portions 15 and a permanent magnet 16 provided outside the vacuum container 11 are provided.

  The vacuum vessel 11 is formed of a nonmagnetic material, for example, a nonmagnetic metal such as an austenitic stainless alloy so as not to be affected by the permanent magnet 16. A lid member 11a capable of airtightly closing the upper opening is provided at the upper opening of the vacuum container 11 so as to be openable and closable. A driving means for mounting the driving means 13 at the center of the bottom of the vacuum container 11 is provided. The mounting part 11b is open.

  The rotary heating element 12 is formed of a metal that generates heat due to Joule heat of eddy current generated by an induced current caused by a change in magnetic flux, and is preferably formed of a metal having low electrical resistance and high thermal conductivity. The center of the rotary heating element 12 is detachably attached to the upper part of the rotary shaft 17 that is rotated by the driving means 13, and the sample container holding part 15 is provided on the inner and outer peripheral parts of the rotary heating element 12. Bottomed cylindrical container holding cylinders 15a and 15b are provided at equal intervals on the inner and outer circumferences.

  The container holding cylinders 15a and 15b are provided obliquely with the bottom portion facing the outer peripheral side, and are usually made of the same type of metal as the rotary heating element 12 and integrally formed with the rotary heating element 12 by welding or the like. It has an inner surface shape that can accommodate the sample container 18 into which the sample solution has been injected.

  The drive means 13 includes an upper drive part 19 that is airtightly attached to the drive means attachment part 11b, and a lower drive part 21 that is disposed on the upper drive part 19 with a partition wall 20 therebetween. The drive unit 19 and the lower drive unit 21 accommodate disc-shaped magnet couplings 22a and 22b, respectively, and the lower drive unit 21 is provided with a motor 23 that rotates the lower magnet coupling 22b.

  Further, the rotating shaft 17 connected to the upper magnet coupling 22a passes through the upper center of the upper drive unit 19. Further, vent holes 24a and 24b are respectively provided in the upper wall portion and the side wall portion of the upper drive portion 19, and the inside of the vacuum vessel 11 and the vacuum pump 14 are connected via the vent holes 24a and 24b and the exhaust pipe 25. Is in a state of communication.

  The permanent magnet 16 is disposed on the outer periphery of the rotating heat generator 12 by an appropriate support means 16a, so that a change in magnetic flux can be applied to the rotating heater 12 rotating on the inner periphery side of the permanent magnet 16. I have to.

  When the sample solution is concentrated using the centrifugal vacuum concentrator thus formed, first, the lid member 11a is opened, and an appropriate number of sample containers 18 into which an appropriate amount of sample solution has been injected are placed in a predetermined container holding cylinder. Inserted in 15a and 15b, respectively. After the lid member 11a is closed and the vacuum pump 14 is operated to exhaust the gas in the vacuum container 11, the inside of the vacuum container 11 is brought into a predetermined reduced pressure state (vacuum state), and then the motor 23 is operated to rotate the heating element. 12 is rotated.

  The rotating heating element 12 rotates at high speed inside the permanent magnet 16, so that the magnetic flux rapidly changes at the outer periphery of the rotating heating element 12, and an eddy current is generated by the induced current. The outer peripheral portion of the rotary heating element 12 generates heat and the temperature rises. At this time, when the rotary heating element 12 is formed of a metal material having a low electrical resistance such as an aluminum alloy, a copper alloy, or low carbon steel, the eddy current is increased and the amount of Joule heat generated is increased. The body 12 can be effectively heated.

  The temperature rise at the outer peripheral portion of the rotary heating element 12 is transmitted to the entire rotary heating element 12 by conduction, and the container holding cylinders 15a and 15b are also uniformly heated by conduction heat. Heat is transferred by radiation to the sample solution in the sample container 18 from the container holding cylinders 15a and 15b whose temperature has risen, but at least the sample solution storage part in the sample container 18 or the sample container 18 is the container holding cylinder. Since it is inserted into 15a and 15b, the sample solution in the sample container 18 can be directly and evenly heated by radiation from the entire inner peripheral surface of the container holding cylinders 15a and 15b. Can be eliminated. Furthermore, the sample solution can also be heated by heat transfer through the sample container 18 in contact with the inner peripheral surfaces of the container holding cylinders 15a and 15b.

  Accordingly, since the sample solution during the concentration operation can be effectively heated, even a solvent having a high boiling point can be evaporated in a short time, and the sample solution can be concentrated and the sample can be efficiently dried in a short time. Further, the inner surface of the vacuum vessel 11 including the lid member 11a and the upper drive unit 19 is in a metallic luster state, and in particular, by applying a mirror finish to the vacuum vessel 11 from the rotating heating element 12 whose temperature has increased. The heat transfer amount of the sample solution can be suppressed, the heat loss can be reduced, and the heating efficiency of the sample solution can be further improved. Further, by interposing a heat insulating material between the rotating heat generating body 12 and the rotating shaft 17, heat transfer from the rotating heat generating body 12 to the rotating shaft 17 can also be suppressed. From these things, compared with the case where a heater is provided in the inner peripheral surface of the vacuum vessel 11, the operation efficiency in the centrifugal decompression and concentration apparatus can be greatly improved, and the power consumption can be reduced.

  FIG. 2 is a schematic sectional view showing a first embodiment of the centrifugal vacuum concentrator of the present invention. In the following description, the same components as those of the centrifugal decompression and concentration apparatus shown in the first embodiment are denoted by the same reference numerals, and detailed description thereof is omitted.

  The centrifugal vacuum concentration apparatus shown in the present embodiment is basically the same as the centrifugal vacuum concentration apparatus shown in the first embodiment except for the structure of the rotary heating element and the arrangement of the magnets. It has become.

  In the present embodiment, the permanent magnet 31 is disposed below the bottom surface of the vacuum container 11 via an appropriate support means 31a, and the rotating heat generating element 32 has a sample container holding portion 33 that holds the sample container 18. A main body portion 32a having bottom cylindrical container holding holes 33a and 33b, a disc-shaped heat generating portion 32b disposed so as to face the permanent magnet 31 across the bottom surface of the vacuum vessel 11, a main body portion 32a, A heat transfer section 32c that connects the heat generating section 32b is provided. The container holding holes 33a and 33b are holes having a predetermined shape formed in the main body 32a using the thickness of the main body 32a. The depth and inner diameter are set according to the sample container 18 to be held. Yes.

  When the rotary heating element 32 is rotated by the driving means 13, the heat generating portion 32b disposed opposite to the permanent magnet 31 generates heat due to the eddy current Joule heat generated by the induced current caused by the change in magnetic flux, and the heat generating portion 32b is heated. Heat is transferred from the heat transfer portion 32c to the main body portion 32a by conduction, the inner surfaces of the container holding holes 33a and 33b are uniformly heated, and the sample in the sample container 18 is irradiated by radiation from the inner surfaces of the container holding holes 33a and 33b. The solution is heated.

  Accordingly, similar to the first embodiment, the sample solution in the sample container 18 can be directly and evenly heated, and the sample solution during the concentration operation can be effectively heated. Can be efficiently dried in a short time.

  As the structure of each part of the apparatus, an optimal structure can be adopted as appropriate according to various conditions such as the shape of the sample container and the number of sample containers held. Further, the number of magnets arranged is arbitrary as long as the rotary heating element can generate heat, and a yoke for improving the magnetic force can be provided. Furthermore, not only permanent magnets but electromagnets may be used. Further, the heating amount (heating temperature) of the sample solution may be adjusted by adjusting the position of the magnet, adjusting the current amount of the electromagnet, or adjusting the rotation speed of the rotating heating element.

  Furthermore, the sample container holding part can be formed in an arbitrary shape according to the shape and size of the sample container to be held. For example, when a ridge is provided on the sample container, the sample container You may make it open | release the bottom part of a holding | maintenance part, let a sample container holding part be a through-hole, and hold | maintain a sample container using a collar.

DESCRIPTION OF SYMBOLS 11 ... Vacuum container, 11a ... Lid member, 11b ... Driving means mounting part, 12 ... Rotating heating element, 13 ... Driving means, 14 ... Vacuum pump, 15 ... Sample container holding part, 15a, 15b ... Container holding cylinder, 16 ... Permanent magnet, 16a ... support means, 17 ... rotating shaft, 18 ... sample container, 19 ... upper drive unit, 20 ... partition wall, 21 ... lower drive unit, 22a, 22b ... magnet coupling, 23 ... motor, 24a, 24b DESCRIPTION OF SYMBOLS ... Vent hole, 25 ... Exhaust pipe, 31 ... Permanent magnet, 31a ... Support means, 32 ... Rotating heat generating body, 32a ... Main body part, 32b ... Heat generating part, 32c ... Heat transfer part, 33 ... Sample container holding part, 33a, 33b ... Container holding hole

Claims (6)

  In a centrifugal vacuum concentration apparatus for concentrating the sample solution by applying a centrifugal force to the sample solution in a vacuumed vacuum vessel, the bottomed cylindrical vacuum vessel having a lid member that opens and closes the upper opening, and the vacuum A metal rotating heating element provided rotatably in the container, a rotation driving means for rotating the rotating heating element, an exhaust means for reducing the pressure in the vacuum container, and a sample container provided in the rotating heating element A centrifugal decompression and concentration apparatus comprising: a holding unit; and a magnet that generates heat by generating an eddy current by electromagnetic induction in the rotating heating element.   2. The centrifugal vacuum concentrator according to claim 1, wherein the rotary heating element is made of an aluminum alloy, a copper alloy, or low carbon steel.   3. The centrifugal decompression and concentration apparatus according to claim 1, wherein the sample container holding part is a cylindrical container holding part provided on the rotary heating element.   The centrifugal decompression and concentration apparatus according to claim 1 or 2, wherein the sample container holding part is a container holding hole formed in the rotary heating element.   The centrifugal vacuum concentration apparatus according to any one of claims 1 to 4, wherein the magnet is provided on an outer periphery of the vacuum vessel.   The centrifugal decompression / concentration device according to any one of claims 1 to 4, wherein the magnet is provided below a bottom surface of the vacuum vessel.

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