JP2012223689A - Device and method for classification of particulate - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a device and method for precisely classifying particulates by a sedimentation velocity method.SOLUTION: The device 1 for classification of particulates uses a centrifugation system comprising separating from a particulate sample, the particulate P being an object to be separated in a carrier liquid phase by the sedimentation velocity method in a separation flow path 3 in which the supply and collection of the carrier liquid phase and those of the particulate sample are performed in a time continuous manner in a centrifugal rotor 30. A pocket 35 in which the particulate P can be housed is provided on at least one of a flow path outer wall 3b positioned outside the radial direction of the separation flow path 3, and a flow path inner wall 3a positioned inside the radial direction.

Description

  The present invention relates to a fine particle classification apparatus and a fine particle classification method for classifying fine particles having a particle size of from micron to nano range.

  As fine particle classification methods, there are a classification method in a gas phase (or vacuum) and a classification method in a liquid phase. Among them, the method of classification in the gas phase has a problem that it is difficult to classify by the true particle size because the processing capacity is small and the fine particles are easily associated.

  On the other hand, in the case of classification in the liquid phase, unlike in the gas phase, the fine particles are less likely to associate, and a large resistance is generated when the fine particles move in the dispersion medium, and the resistance is sensitive to the particle size. Therefore, it is possible to easily classify the fine particles according to the true particle size. Therefore, attention has been focused on a method for classification in the liquid phase from these viewpoints.

  As a method for classifying the fine particles in the liquid phase, a method using centrifugation is typical, and the centrifugation method includes a sedimentation equilibrium method and a sedimentation rate method. The sedimentation equilibrium method is a method for classifying the fine particles based on the difference in the floating density, and the sedimentation rate method is a method for classifying the fine particles based on the difference in the sedimentation rate.

  In the sedimentation velocity method, each sample particle settles in the liquid phase at a sedimentation velocity according to the inherent sedimentation velocity coefficient, and after a certain amount of time has elapsed since the start of sedimentation, it exists at a different sedimentation position depending on the sedimentation velocity coefficient. To do. The sedimentation rate coefficient of the sample particles is determined by the density of the sample particles and the effective particle size. If the sample density is the same, the sample particles can be classified by the effective particle size. In manufacturing processes and laboratory preparation operations, it is often desirable to separate samples of the same density according to particle size.

  There are three methods for collecting fine particles: a batch method, a semi-continuous method, and a complete continuous method. The batch method is a method of classifying target fine particles for each operation using a processing container having a tube or other shape. In batch method, only small amount of processing can be performed, and the conditions are slightly different for each operation (from rotation start to acceleration, constant rotation, rotation deceleration and stop). There is a problem of being slightly different.

  On the other hand, in the semi-continuous method and the complete continuous method, the sample throughput can be increased by performing continuous operation compared to the batch method, and by stabilizing the operation conditions, a constant particle size can be obtained from start to finish. It is possible to recover the diameter.

  The inventor of the present application has developed a fine particle classification method and apparatus using a centrifugal separation method in which a fine particle sample in a carrier liquid phase is separated continuously and at a high resolution by a sedimentation velocity method in a separation channel in a centrifugal rotor. (See Patent Document 1).

  In the fine particle classification method and apparatus of Patent Document 1, a continuous density gradient forming device using a density gradient material is provided at the inlet of the separation channel, and the solution density of the carrier liquid phase is the radial diameter of the centrifugal rotor in the separation channel. A continuous density gradient that continuously increases toward the outside in the direction is formed, and the supply of raw materials and the collection of classified fine particles are performed in a completely continuous manner.

  The method and apparatus of Patent Document 1 uses “natural providence” in which molecules of a density gradient material diffuse due to molecular motion, and is highly reliable. The density gradient formed by the diffusion of the density gradient material. It is not difficult to obtain a profile by numerical simulation or the like.

  The continuous density gradient former used in this method and apparatus is configured to greatly compress the carrier liquid phase in the radial direction of the rotor and restore the compression in the radial direction on the downstream side (enhance static diffusion of density gradient material) By this method, a rapid continuous density gradient (density gradient that is not jerky like a staircase) is formed. The presence of this continuous density gradient on the carrier liquid phase suppresses the generation of turbulent flow in the separation channel (spatial ordering is ensured).

Japanese Patent No. 4247390

  As a result of further earnest research, the inventors of the present application have found a fine particle classification device and a fine particle classification method having the same effect and practicality as or more than the fine particle classification device of Patent Document 1.

  An object of the present invention is to provide a fine particle classification device and a fine particle classification method that can classify fine particles continuously and efficiently with high resolution by a sedimentation rate method.

  The fine particle classifying device of the present invention that solves the above problems is a separation channel in which the supply and recovery of the carrier liquid phase and the supply and recovery of the fine particle sample are continuously performed in the centrifugal rotor, and are separated from the fine particle sample. A fine particle classifying apparatus using a centrifugal separation method that separates the fine particles to be separated in a carrier liquid phase by a sedimentation velocity method, the flow path outer wall located on the radially outer side of the separation flow path and the movement of the separation flow path A pocket capable of accommodating the fine particles is provided on at least one of the inner walls of the flow channel located on the radially inner side.

  According to the fine particle classification apparatus of the present invention, the fine particle sample is separated from at least one of the flow channel outer wall located on the outer side in the radial direction of the separation flow channel and the flow channel inner wall located on the inner side in the radial direction of the separation flow channel. A pocket that can accommodate fine particles is provided, so that fine particles that have reached different flow channel outer wall positions or flow channel inner wall positions depending on the particle size are retained in the pocket as they are, and flow direction Can be prevented. Therefore, after a continuous operation for a certain period of time, the operation is stopped (referred to as semi-continuous operation), and fine particles having a desired particle size precisely classified are collected by a method of collecting fine particles accumulated in the pocket during the continuous operation. Can be easily obtained.

  The fine particle classification device of the present invention preferably has a configuration in which a plurality of pockets are arranged with a predetermined pitch in the flow direction of the separation flow path to form a pocket row.

  According to the present invention, since a plurality of pockets are arranged at a predetermined pitch in the flow direction of the separation flow path to form a pocket row, fine particles having a desired particle size precisely classified Can be accommodated in each pocket of the pocket row by particle size. In this way, by arranging a pocket row in which a plurality of pockets are arranged in the flow direction of the separation flow path, it is possible to simultaneously receive and collect many fractions separated and developed by the particle size. Become. Therefore, it is possible to obtain a large number of fractions with small sample loss and slightly different particle size values (but sharp with little overlap between fractions) at a time without reducing the resolution. Therefore, the fine particle sample can be efficiently and precisely classified, the sample processing capacity is large, and the recovery rate is high.

  The fine particle classification device of the present invention preferably has a configuration in which the pocket rows are continuously arranged from the upstream portion to the downstream portion of the separation channel.

  The precaution of such a continuous separation apparatus is a precipitate in the middle of the separation channel. If sediment is present, the effective cross-sectional area of the separation channel becomes smaller as the deposition progresses, so the flow velocity in the separation channel increases and the residence time of the sample particles in the separation channel decreases accordingly. The conditions will change. According to the present invention, since the pocket row is continuously arranged from the upstream portion to the downstream portion of the separation channel, even if a deposit occurs in the middle of the separation channel, it is dropped into the pocket, The effective cross-sectional area of the separation channel does not change. In addition, if deposits occur, the solid phase is lost from the carrier liquid phase, but in exchange, a liquid phase with a volume just equal to the volume of the lost solid phase is sprinkled from the inside of the pocket. Since it comes out, there is no volume change of the entire mobile phase (resulting in subtle changes in the flow velocity) due to the generation of deposits. As described above, even if deposits are present, it is possible to prevent separation conditions from changing during continuous operation, and precise classification can be performed.

  The fine particle classification device of the present invention has a configuration in which a block which is detachably attached to a rotor body of a centrifugal rotor and forms a part of the outer wall of the separation flow channel, and a pocket is provided on the surface of the block. It is preferable to have.

  According to the present invention, since the pocket is provided on the surface of the block that is detachably attached to the rotor body of the centrifugal rotor and forms a part of the flow path outer wall of the separation flow path or a part of the flow path inner wall, Specifications such as the size and shape of each pocket can be easily changed by exchanging the blocks. Therefore, the fineness of the recovered fraction can be easily adjusted without changing the rotor body. Further, since the entire block can be removed from the rotor body, sample collection, pocket cleaning, apparatus maintenance, and the like are facilitated. Therefore, the operability as a total including sample handling can be improved when a large number of sample fractions are handled simultaneously.

  The fine particle classification device of the present invention may have a configuration in which the pocket has a groove shape extending in the direction along the rotation center axis of the centrifugal rotor, and the pocket has a predetermined interval in the direction along the rotation center axis of the centrifugal rotor. Alternatively, a plurality of configurations may be provided.

  The fine particle classification device of the present invention preferably has a disposal container that is detachably placed on the surface of the pocket.

  According to the present invention, since the disposal container that is detachably placed on the surface of the block is provided, the operability such as sample collection, arrangement and storage, block cleaning, and apparatus maintenance can be significantly improved.

  In the fine particle classification device of the present invention, it is preferable that the despo container has a shape in which a pocket is partitioned in a direction along the rotation center axis of the centrifugal rotor to form a plurality of storage chambers.

  According to the present invention, the despo container has a shape in which the inside of the pocket is partitioned in the direction along the rotation center axis of the centrifugal rotor to form a plurality of storage chambers. Even if there is a difference in the classification conditions of the microparticle sample depending on the direction position, and even if the occurrence of the difference varies depending on the sample particle and the separation conditions, the microparticles corresponding to the difference can be stored in each storage chamber and easily handled I can do it. Moreover, the decoupling of the liquid phase motion between the separation channel and each storage chamber can be performed more reliably.

  The fine particle classification method of the present invention is a fine particle classification method using a centrifugal separation method in which a fine particle to be separated from a fine particle sample is separated in a carrier liquid phase by a sedimentation velocity method in a separation flow path in a centrifugal rotor. The continuous density gradient forming device provided in the upstream portion of the separation channel forms a continuous density gradient in a state where there is no flat portion with respect to the radial density gradient of the carrier liquid phase. The supply and recovery of the carrier liquid phase and the supply and recovery of the fine particle sample are performed continuously in time. The fine particles are collected by storing the fine particles that have reached the outer wall of the separation channel in a pocket provided on the outer wall of the channel. The semi-continuous method of collecting from the pocket after stopping the rotation of the centrifugal rotor is characterized.

  According to the present invention, fine particles that reach different flow channel outer wall positions or flow channel inner wall positions depending on the particle diameter are allowed to remain in the pockets as they are and are prevented from moving in the flow path direction or the like. Thus, fine particles having a desired particle size that is precisely classified can be easily obtained.

  In the fine particle classification method of the present invention, the two fine particle classifiers described above are used to perform the first classification treatment in which the fine particle separation is performed by the first fine particle classification device, and the second fine particle classification device is used to separate the fine particles. It is characterized in that two classification processes are alternately performed. According to the present invention, it is possible to operate in a completely continuous mode in terms of time.

  In the fine particle classification method of the present invention, during the first classification treatment, fine particles are collected from the pockets of the second fine particle classification device, and the second fine particle classification device is rotated by a centrifugal rotor at a constant rotational speed. A step of setting the carrier liquid phase to a standby state in which the liquid phase is supplied at a constant flow rate; a step of switching the supply destination of the fine particle sample from the first fine particle classification device to the second fine particle classification device; During the two-classification process, the step of collecting the fine particles from the pocket of the first fine particle classification device and setting the first fine particle classification device to the standby state, and the supply destination of the fine particle sample from the second fine particle classification device to the first And switching to the fine particle classifier, and performing the first classification process in order. According to the present invention, it is possible to operate in a completely continuous mode in time and to maintain high separation accuracy of fine particles.

  According to the fine particle classification apparatus having the above-described configuration, the fine particle sample is separated from at least one of the flow channel outer wall located on the outer side in the radial direction of the separation flow channel and the flow channel inner wall located on the inner side in the radial direction of the separation flow channel. Since the pockets that can store the collected fine particles are provided, the fine particles that reach the flow channel outer wall or the flow channel inner wall according to the particle size can be stored in the pocket as they are, and can remain in the place, such as the flow direction Can be prevented from moving to. Therefore, by collecting the fine particles from the pocket after stopping the rotation of the centrifugal rotor, it is possible to obtain fine particles having a desired particle size precisely classified.

The perspective view of the separation flow path and continuous density gradient forming device of a fine particle classification device. The figure which showed a mode that the separation flow path and the continuous density gradient former were arrange | positioned to the centrifugal rotor. FIG. 3 is a sectional view taken along line AA in FIG. 2. The figure explaining the difference in the movement to the flow-path outer wall by the magnitude | size of microparticles | fine-particles. The figure explaining Example 1 of a continuous-density gradient former. The figure explaining Example 2 of a continuous-density gradient former. FIG. 7 is a partially enlarged view of FIG. 6. The figure explaining Example 3 of a continuous-density gradient former. FIG. 9 is a partially enlarged view of FIG. 8. The figure explaining Example 4 of a continuous-density gradient former. FIG. 11 is a partially enlarged view of FIG. 10. The figure which looked at the continuous density gradient former of Example 4 from the upper direction of the rotor rotating shaft direction. The figure explaining the stirring action of the carrier liquid phase by a slit. The front view explaining the structure of a slit. The graph which shows the relationship between a radial direction position and a density gradient. The perspective view which shows an example of the centrifugal rotor in this Embodiment. The perspective view which shows one specific example of a pocket row. FIG. 18 is a plan view of a pocket row. The perspective view which shows the other specific example of a pocket row. The figure which shows in cross section another example of the block with which the disposal container was covered The figure which shows the state which removed the disposal container of FIG. 20 from the block, and was made to hold | maintain on an exclusive stand.

<First embodiment>
Next, the present embodiment will be described below with reference to the drawings.
FIG. 1 is a perspective view showing a separation channel and a continuous density gradient forming device of the fine particle classification apparatus according to the present embodiment, and FIG. 2 shows a state in which the separation channel and the continuous density gradient forming device are arranged in a centrifugal rotor. 3 is a cross-sectional view taken along line AA in FIG.

  The fine particle classification apparatus and method of the present invention is a separation channel in which the supply and recovery of a carrier liquid phase and the supply and recovery of a fine particle sample are performed continuously in time in the centrifugal rotor 2, and the separation target is separated from the fine particle sample. Using a centrifugal separation method in which fine particles to be separated are separated by a sedimentation velocity method in a carrier liquid phase.

  The fine particle classification device 1 according to the present embodiment includes a centrifugal rotor 2 that is rotatably supported up and down, and a drive motor (not shown) that rotationally drives the centrifugal rotor 2 at a high speed.

  The centrifuge rotor 2 is connected to a plurality of flow paths by rotating seals or the like from both ends of the rotation axis along the rotation axis. Through the plurality of flow paths, the carrier liquid phase and the particulate sample are supplied and classified. The carrier liquid phase and fine particles are collected.

  As shown in FIGS. 1 and 2, the centrifugal rotor 2 is provided with a separation flow path 3 extending in an arc shape along the circumferential direction of the centrifugal rotor 2, and an upstream portion of the separation flow path 3. The continuous density gradient generator 4 is connected to each other.

  As shown in FIG. 2, the separation channel 3 can flow the carrier liquid phase from the upstream side toward the downstream side. For example, as shown in FIG. 3, the inner wall of the flow channel having a closed cross-sectional shape and having a predetermined height width and curved around the rotation center (the flow channel inside the radial direction of the separation flow channel 3 A wall) 3a, a flow path outer wall (flow path outer wall in the radial direction of the separation flow path 3) 3b facing the radially outer side of the flow path inner wall 3a, an upper end portion of the flow path inner wall 3a, and a flow path outer wall 3b. The upper surface wall 3c extending in a planar manner between the upper end of the lower surface wall 3d and the lower surface wall 3d extending in a planar shape between the lower end of the flow channel inner wall 3a and the lower end of the flow channel outer wall 3b. Have

  The continuous density gradient generator 4 is connected to the upstream portion of the separation channel 3 and controls the liquid phase density by changing the concentration of the solute dissolved in the carrier liquid phase (called density gradient material). Do. For example, as shown in FIG. 2, two or more liquid phase supply tubes are connected to the upstream portion (inlet) of the continuous density gradient former 4, and at least different bulk densities are passed through these liquid phase supply tubes. Two or more density gradient material solutions are continuously supplied (carrier liquid phase supply means). For example, a carrier liquid phase having a low bulk density is supplied inside in the radial direction, and a carrier liquid phase having a high bulk density is supplied outside in the radial direction. The bulk density is not limited to two types, and may be three or more types.

  From the downstream part of the continuous density gradient forming device 4, the carrier liquid phase has a density gradient (continuous density gradient) that continuously increases toward the changing direction of the radial direction r of the centrifugal rotor 2, that is, outward in the radial direction. Will come out. The continuous density gradient generator 4 has a length in the rotor circumferential direction (flow direction) necessary to form a continuous density gradient of the carrier liquid phase (smooth the discontinuous density change as necessary). .

  When two types of carrier liquid phases having different densities are continuously supplied from the upstream portion of the continuous density gradient former 4, these continuous density gradient formers 4 pass through the continuous density gradient former 4 while passing through the continuous density gradient former 4. Two types of carrier liquid phases are merged with each other, and the density gradient in the radial direction is changed to a state where there is no flat portion to form a continuous density gradient, and the carrier liquid phase having the continuous density gradient is separated by a flow path. 3 is supplied continuously to the upstream part of time 3. The internal configuration of the continuous density gradient generator 4 will be described later.

  A sample injection port 5 for injecting a fine particle sample into the separation channel 3 is provided upstream of the separation channel 3. The sample injection port 5 is disposed upstream of the separation channel 3 and in the vicinity of the channel inner wall 3a.

  The sample injection port 5 is disposed at a position close to the channel inner wall 3a of the separation channel 3 in the sedimentation mode in which the particles P are heavier than the carrier liquid phase as in the present embodiment, but the particles P are lighter than the carrier liquid phase. In the levitation mode, the separation channel 3 is disposed near the channel outer wall 3b. The sample injection port 5 is connected to a sample pump (not shown) via a sample supply tube, and continuously supplies a particulate sample made of a sample solution containing the particulate P to the upstream portion of the separation channel 3. It has become.

  The carrier liquid phase and the particulate sample supplied continuously from the upstream portion of the separation channel 3 are several minutes to several tens of minutes from the upstream side to the downstream side in the separation channel 3 of the centrifugal rotor 2 rotating at high speed. Move over.

  FIG. 4 is a diagram illustrating the principle of the separation flow path 3 in the centrifugal rotor 2 viewed from the same direction as in FIG. 2, and is displayed in an orthogonal coordinate system for simplicity. The rotor rotation shaft is located in the upper part of the figure, and centrifugal force is acting toward the outer side in the radial direction that is the direction from the upper side to the lower side in the vertical axis direction.

  The carrier liquid phase is converted to a state in which there is no flat portion with respect to the radial density gradient by the continuous density gradient forming device 4 and is continuously continuous in time from the upstream to the downstream in the separation channel 3 in a state where the carrier density is a continuous density gradient. The fine particle sample is supplied from the sample injection port 5 continuously for a time.

  The fine particle P of the fine particle sample injected into the separation channel 3 from the sample injection port 5 moves from the upstream to the downstream together with the carrier liquid phase flowing in the separation channel 3, and moves in the separation channel 3 by centrifugal force. Move in the radial direction. And while moving the separation flow path 3, the fine particles P having a larger particle diameter are quickly settled outward and reach the flow path outer wall 3 b of the separation flow path 3.

  The collection of the fine particles P is performed continuously for a time, for example, a complete continuous system in which fine particles having a target size are recovered from a target sample recovery port 6 provided in the separation channel 3 may be used. The fine particles P deposited on the flow channel outer wall 3b are collected after the rotation of the centrifugal rotor 2 is stopped while collecting the carrier liquid phase from the liquid phase (and other fraction of fine particles) collection port provided in the downstream portion of the passage 3. A semi-continuous method may be used, and both a complete continuous method and a semi-continuous method may be employed.

  For example, as shown in FIG. 4, the target sample collection port 6 can be completed at one place, and can be provided at a plurality of places. The sample injection port 5 and the target sample recovery port 6 have a narrow width (small Δr) in the radial direction in order to reduce the difference between the fine particles P regarding the settling (or flying) distance.

Next, the configuration of the continuous density gradient generator 4 will be described with reference to FIGS.
As shown in FIG. 5 and the like, the continuous density gradient forming device 4 includes a flow path portion 11 in which the carrier liquid phase flows from the upstream side toward the downstream side, and a stirring unit 12 for stirring the carrier flowing in the flow path portion 11. Have. The stirring means 12 converts a part of the flow energy of the carrier liquid phase flowing in the flow path portion 11 into stirring energy, and actively promotes the diffusion of the density gradient material, whereby the radial direction of the carrier liquid phase The density gradient of the step is from a stepped shape (a state in which a flat portion exists in the radial gradient of the carrier liquid phase) to a continuous portion (a portion in which the density gradient in the radial direction of the carrier liquid phase is flat) To a mode that does not promptly change).

  The agitation means 12 includes a part that blocks the flow of the carrier liquid phase and a part through which the carrier liquid phase can pass in a cross section of the flow path 11 cut by a plane perpendicular to the direction in which the carrier liquid phase flows. And has a non-uniform structure that exerts a non-uniform action on the carrier liquid phase to be passed. Due to this heterogeneous structure, the carrier liquid phase may be blocked depending on which position in the cross section of the flow path is going to pass compared to the case where no structure is present in the cross section of the flow path. Alternatively, the stirring means 12 is subjected to a significantly different action, such as being allowed to pass through.

  For example, the agitation means 12 includes a partition part that partitions the flow path part 11 into an upstream side and a downstream side, and a passage part that is provided in the partition part at a predetermined interval in the radial direction and through which a carrier liquid phase can pass. The carrier liquid phase is agitated by utilizing the fact that the flow of the carrier liquid phase is disturbed when passing through the passage portion.

  For such a non-uniform structure, the flow of the carrier liquid phase is completely blocked by the partition and the carrier liquid phase is allowed to freely pass by the passage, but for example, the flow path cross section of the passage with respect to the partition The non-uniformity can be further increased by reducing the area ratio (corresponding to the aperture ratio) in the area. It is understood that the flow velocity at the partition portion becomes zero, whereas the flow velocity at the passage portion increases as the aperture ratio decreases, that is, the contrast between the partition portion and the passage portion increases accordingly. it can.

  FIG. 5 is a diagram illustrating Example 1 of a continuous density gradient former. The flow path portion 11 of the continuous density gradient former 4 has substantially the same cross-sectional shape as that of the separation flow path 3, and for convenience of explanation, FIG.

  For example, the continuous density gradient forming device 4 of Example 1 shown in FIG. 5 arranges round bars (columns) 13 which are a plurality of rod-like members in the flow path portion 11 at predetermined intervals in the radial direction. A plurality of round bars 13 arranged in the radial direction are set as one set, and the plurality of sets are provided so as to be continuous at a predetermined interval in the flow direction of the carrier liquid phase. The positions of the pairs of round bars 13 facing the upstream side and the downstream side are alternately arranged in the radial direction so as not to overlap the flow direction of the carrier liquid phase.

  Therefore, the flow path portion 11 is partitioned into the upstream side and the downstream side by the plurality of round bars 13 arranged in the radial direction so that a partition portion is formed, and a gap formed between the round bars 13 is formed. To form a passage. According to the continuous density gradient forming device 4, the carrier liquid phase is allowed to pass between the respective round bars 13, whereby agitation can be selectively caused in a direction perpendicular to the axial direction of the round bars 13.

  Therefore, even if the length of the flow path portion 11 in the flow path direction is short, the carrier liquid phase flowing in the flow path section 11 can be sufficiently stirred in the radial direction, and the density gradient in the radial direction is stepped. A continuous density gradient can be formed by quickly converting from continuous to continuous.

  FIG. 6 is a diagram illustrating Example 2 of the continuous density gradient forming device, and the inside of the flow path portion is viewed from above in the rotor rotation axis direction. FIG. 7 is an enlarged view of a part of FIG.

  The continuous density gradient former 4 of Example 2 shown in FIG. 6 has a configuration in which a plurality of round bars 13 are arranged more densely than that shown in FIG. In the structure in which a plurality of round bars 13 are arranged more closely, as shown in FIG. 7, the carrier liquid phase is more agitated in the radial direction when passing between the round bars 13. Radial mixing can be actively promoted. Each round bar 13 is formed such that the diameter of the round bar 13 increases as it moves toward the outside in the radial direction in order to correspond to the curve of the flow path portion 11. In the first and second embodiments, the case of a round bar has been described as an example of the bar-like member. However, the bar is not limited to a round bar, and a square bar such as a regular square, a regular hexagon, or a regular octagon is used for the cross section. Other rod shapes may be used.

  FIG. 8 is a view showing a third embodiment of the continuous density gradient former, and FIG. 9 is a partially enlarged view of FIG. The continuous density gradient forming device 4 of Example 3 shown in FIG. 8 has a partition plate 21 that partitions the inside of the flow path portion 11 into an upstream side and a downstream side, and the partition plate 21 has a predetermined radial direction. Circular holes (holes) 22 are provided at intervals.

  A plurality of circular holes 22 are provided at predetermined intervals in the direction of the channel width W and the channel height H of the channel unit 11. The partition plate 21 is disposed so as to extend along the radial direction, and a plurality of the partition plates 21 are provided at predetermined intervals in the flow direction of the flow path portion 11.

  According to the continuous density gradient former 4 of Example 3 having the above-described configuration, by passing the carrier liquid phase through the circular hole 22, as shown in FIG. Can be stirred evenly. Therefore, even if the length of the flow path portion 11 in the flow path direction is short, the carrier liquid phase flowing in the flow path section 11 can be sufficiently stirred in the radial direction, and the density gradient in the radial direction is stepped. A continuous density gradient can be formed by quickly converting from continuous to continuous.

  Accordingly, the length of the continuous density gradient forming device 4 in the longitudinal direction can be shortened, and the length of the separation flow path 3 can be increased by that amount, so that restrictions on the rotor dimensions can be relaxed. . Moreover, compared with the stirring method (Examples 1 and 2) using the round bar 13 shown in FIG. 5 to FIG. An increase in the linear velocity of the flow inside can be suppressed. In addition, a simpler and more robust structure (centrifugal resistance) than the round bar 13 can be achieved.

  FIG. 10 is a diagram illustrating a continuous density gradient forming device according to a fourth embodiment, FIG. 11 is a partially enlarged view of FIG. 10, and FIG. 12 illustrates the continuous density gradient forming device according to the fourth embodiment from above in the rotor rotation axis direction. FIG. And FIG. 13 is a figure explaining the stirring action of the carrier liquid phase by a slit, and FIG. 14 is a figure explaining the structure of a slit.

  The continuous density gradient former 4 of Example 4 shown in FIG. 10 is provided with slits (holes) 23 in the partition plate 21 instead of the circular holes 22 shown in FIGS. As shown in FIGS. 10 and 14, the slit 23 has a shape extending in a direction orthogonal to the radial direction (parallel to the rotor rotation axis direction), and a plurality of slits are spaced at a predetermined interval in the radial direction. Has been placed. The slit 23 can cause stirring in the direction perpendicular to the longitudinal direction of the slit 23 from the slit 23 as shown in FIGS. 11 and 13 by passing the carrier liquid phase.

  Therefore, stirring can be selectively caused in the radial direction (centrifugal force direction) in which stirring is required, and stirring can be performed with less flow resistance compared to the circular hole 22 of Example 3. . Therefore, sufficient stirring force can be generated in the radial direction while suppressing the flow resistance generated by the partition plate 21.

  As shown in FIG. 13, when the carrier liquid phase passes through two slits 23 adjacent to each other in the radial direction, it flows in a direction approaching each other along the radial direction, and is perpendicular to the longitudinal direction of the slit 23. Cause agitation in the direction. Therefore, the radial stirring of the carrier liquid phase can be further promoted (by Coriolis force with respect to the movement of the carrier liquid phase).

  The outer dimension of the partition plate 21 is mainly determined by the cross-sectional dimension of the separation channel 3. Stirring (liquid phase merging) efficiency per one partition plate, flow resistance, structure, etc., based on the linear velocity of the flow (determined by the movement policy of the entire system) and the parameters a to d (specific dimensions) shown in FIG. Strength is determined.

  For example, when the carrier liquid phase slowly flows through the separation channel 3 having a total length of 90 cm over 30 minutes, the flow rate in the separation channel 3 is 0.5 mm / second. Therefore, if the continuous density gradient forming device 4 has the partition plate 21 in which the slits 23 having a width of 0.2 mm are arranged at intervals of 4 mm in the radial direction, the aperture ratio is (total hole area / partition plate area). Becomes 5% or less, and the flow rate when the carrier liquid phase passes through the slit 23 becomes 10 mm / second or more. If the disturbance by the continuous density gradient generator 4 is insufficient, the disturbance can be further increased by further increasing the slit distance d in the radial direction or by reducing the slit width b. it can.

  In the fourth embodiment, as shown in FIG. 14, the case where the slit 23 is divided into three stages in the rotor rotation axis direction has been described as an example. However, the present invention is not limited to this embodiment. If the structural strength can be obtained so that the distortion of the slit under the action of the force falls within a predetermined range, the structure is divided into two steps, or the structure extends between the upper end and the lower end without being divided up and down. It is good.

  Thus, according to the continuous density gradient forming device 4 of Example 4, even if the length of the flow path portion 11 in the flow path direction is short, the carrier liquid phase flowing in the flow path portion 11 is sufficient in the radial direction. The density gradient in the radial direction can be rapidly changed from a step-like one to a continuous one to form a continuous density gradient.

  Therefore, the carrier liquid phase can be merged more effectively than in the third embodiment, and the length of the continuous density gradient former 4 in the longitudinal direction can be further shortened. Compared with the stirring method using the round bar 13 shown in FIGS. 4 and 5, the rate of decrease in the actual volume of the gap portion of the flow path portion 11 is small, and the linear velocity of the flow in the flow path portion 11 is reduced. The rise can be suppressed. In addition, a simpler and more robust structure (centrifugal resistance) than the round bar 13 can be achieved.

  In addition, the partition plates 21 of Examples 3 and 4 are detachably provided in the flow path portion 11. For example, when the partition plates 21 are inserted and removed, the number of the partition plates 21, the size of the circular holes 22 and the slits 23 are increased. , Parameters such as width, number and distribution can be freely adjusted. With this parameter adjustment function, it is possible to easily optimize the separation conditions such as the density gradient depth.

  In each of the above-described embodiments, at least the thickness, shape, number, and arrangement interval in the radial direction of the round bars 13, or the size, width, number, and distribution of the circular holes 22 and the slits 23 of the partition plate 21 are used. One can be changed according to the arrangement position in the flow direction in the flow path section 11.

  For example, the case where there are two types of carrier liquid phases supplied to the continuous density gradient forming device 4 will be described as an example. The upstream portion of the continuous density gradient forming device 4 (the portion soon after the merging process of two carrier liquid phases starts). ), There is a steep liquid phase density gradient in the radial direction intermediate position in the flow path. In order to promote diffusion at a site where the gradient of the liquid phase density is steep, generally a strong stirring force is required.

  On the other hand, the liquid phase density is almost flat in the vicinity of the outer wall 3b on the radially outer side and the inner wall 3a on the inner side in the radial direction. There is no point in promoting it.

  Therefore, in the upstream portion of the continuous density gradient forming device 4, the flow where the density gradient of the carrier liquid phase becomes steep in the stirring force generation site such as the hole (circular hole 22 or slit 23) of the partition plate 21. A continuous density gradient can be efficiently formed by concentrating as appropriate at the intermediate position in the radial direction of the road portion.

  The present invention is based on the principle that a part of the flow energy is used after being converted to the stirring energy, and the stirring energy is limited. Therefore, the efficiency of forming a continuous density gradient can be increased by concentrating and arranging the stirring force generation sites where stirring energy is required as described above.

Next, a method for collecting a sharp particle size fraction from a fine particle sample having a wide particle size distribution at a high recovery rate will be described.
As shown in FIGS. 6 and 12, a partition wall 24 that partitions the inside of the flow channel 11 into the inner side and the outer side in the radial direction is provided at the downstream portion of the continuous density gradient former 4. The partition wall portion 24 is spatially continuous from the sample injection port 5 toward the upstream side to the midway position of the flow channel portion 11 of the continuous density gradient former 4, and spans the rotor rotation axis direction of the flow channel portion 11. It partitions without gaps, blocking the mass transfer in the radial direction in this section.

  Therefore, stirring of the carrier liquid phase in the flow path portion 11 between the radially inner side and the radially outer side through the partition wall 24 is performed from the upstream end to the downstream end (position of the sample injection port) of the partition wall portion 24. And a step of density gradient can be generated at the sample injection position.

  FIG. 15 is a graph showing the relationship between the radial direction position and the density gradient, and the density gradient profile shown by the solid line in FIG. 15 shows the density gradient generated when the partition wall portion 24 is provided, and FIG. A density gradient profile indicated by a dotted line indicates a density gradient generated when the partition wall portion 24 is not provided.

  By providing the partition wall 24, as shown by a solid line in FIG. 15, the allowable range of the bulk density of the carrier liquid phase at the sample injection position can be expanded. Therefore, the bulk density of the fine particle sample and the bulk density of the carrier liquid phase at the sample injection position can be easily matched, and the broadening of the bandwidth of the fine particle sample can be prevented. Therefore, the radial width of the sample injection port can be made sufficiently narrower than the settling distance, and a very sharp particle size fraction can be recovered at a high recovery rate from an original sample with a wide particle size distribution. Can do.

  According to the continuous density gradient forming device 4 having the above-described configuration, the energy of the flow of the carrier liquid phase carrying the fine particle sample in a dispersed manner can be converted and utilized for the active diffusion process of the density gradient material, and a shorter distance can be obtained. A continuous density gradient can be formed. Therefore, the external dimensions can be kept compact, and the flexibility of the design of the entire apparatus can be greatly improved.

Next, a method for collecting the fine particles P in the present embodiment will be described.
The recovery of the fine particles P includes a completely continuous method for recovering the fine particles P having a target size from a target sample recovery port 6 provided in the separation channel 3 and a liquid phase recovery provided in the downstream portion of the separation channel 3. Both semi-continuous systems are used in which the fine particles P deposited on the flow channel outer wall 3b are collected after the centrifugal rotor 2 stops rotating while collecting the carrier liquid phase from the port.

  Then, as a semi-continuous method, a method is adopted in which a pocket which is a depression is recessed in the flow channel outer wall 3b of the separation flow channel 3, and the fine particles P reaching the flow channel outer wall 3b are accommodated in the pocket and collected. Yes.

  FIG. 16 is a perspective view showing an example of a centrifugal rotor in the present embodiment. The same components as those described in the above embodiment are denoted by the same reference numerals, and detailed description thereof is omitted.

  The centrifugal rotor 30 has a rotor body 31 and a lid 41. The rotor body 31 has a disk shape having a predetermined thickness made of a metal material such as an aluminum alloy, and a concave groove 32 is provided on the upper surface thereof. The concave groove 32 is formed in a circumferential shape around the rotation center of the centrifugal rotor 30.

  The lid 41 is a transparent plate made of, for example, acrylic or glass and is made of a disc having a predetermined thickness. The lid 41 is overlaid on the upper surface of the rotor body 31 to close the upper side of the groove 32 and cooperate with the body. The separation channel 3 is formed in the centrifugal rotor 30 by working.

  On the upper surface of the rotor body 31, seal grooves are respectively provided on the outer peripheral side and the inner peripheral side of the concave groove 32, and a small-diameter O-ring 33 and a large-diameter O-ring 34 are mounted. It comes to seal closely.

  A continuous density gradient forming device 4 corresponding to the above-described fourth embodiment is provided in the upstream portion of the concave groove 32, and the separation channel 3 is formed on the downstream side of the continuous density gradient forming device 4. Although not particularly illustrated, the lid 41 has a supply port for supplying a carrier liquid phase upstream of the continuous groove 32 at the upstream portion of the concave groove 32, and a carrier liquid phase at the downstream portion of the concave groove 32. A recovery port is provided for recovering the water.

  The continuous density gradient former 4 is not limited to the configuration of the fourth embodiment, and the static diffusion promotion type in addition to the configurations of the first to third embodiments and the dynamic diffusion promotion type may be adopted. Good.

  The separation channel 3 has a sample injection port 5 attached to the upstream portion and a target sample recovery port 6 attached to the downstream portion. The flow path outer wall 3b of the separation flow path 3 is provided with a pocket row 35A which is a characteristic configuration of the present invention.

  The pocket row 35A is formed by arranging a plurality of pockets 35 so as to be arranged at predetermined intervals in the flow path direction. The pocket 35 has a well shape that is recessed by a predetermined depth in the radial direction from the flow path outer wall 3b, and has a size that can accommodate the fine particles that have reached the flow path outer wall 3b.

  FIG. 17 is a perspective view showing one specific example of the pocket row, FIG. 18 is a plan view of the pocket row, and FIG. 19 is a perspective view showing another specific example of the pocket row.

  The separation channel 3 is configured such that an arc-shaped block 36 can be fitted into the groove wall surface on the outer side in the radial direction of the concave groove 32. The block 36 is detachably attached to the rotor body 31 and constitutes a part of the flow path outer wall 3 b of the separation flow path 3. The block 36 is provided with a plurality of pockets 35. Each pocket 35 is formed on the surface of the block 36 so as to form a pocket row 35 </ b> A with a predetermined pitch in the flow direction of the separation flow path 3 with the block 36 attached to the rotor body 31. . The pocket row 35A is continuously arranged from the upstream portion to the downstream portion of the separation channel 3.

  The pockets 35 shown in FIG. 17 have a groove shape extending in the direction along the rotation center axis of the centrifugal rotor 30 (the depth direction of the concave groove 32), and nine rows are provided in one block. . And the pocket 35 shown in FIG. 19 has the shape which forms the some storage chamber 35a which divided the inside of the groove | channel further in the direction along the rotation center axis line, and is a total of 9 rows 7 steps | paragraphs in one block. 36 accommodation chambers 35a are provided.

  As shown in FIG. 18, each pocket 35 can sink the fine particles P reaching the outer wall 3 b of the flow path and store the fine particles P in the pocket 35, and can stay in the place, and move in the flow path direction or the like. Can be prevented.

  In this way, by arranging the pocket row 35A in which a plurality of pockets 35 are arranged in the flow path direction of the separation flow path 3, many fractions separated and developed according to the particle diameter are received and collected simultaneously. Multiple fractions can be collected simultaneously. Therefore, it is possible to obtain a large number of fractions with small sample loss and slightly different particle size values (but sharp with little overlap between fractions) at a time without reducing the resolution.

  And since it has the some storage chamber 35a divided in the direction along the rotation center axis line of the centrifugal rotor 30 according to the pocket 35 shown in FIG. 19, the rotation center of the centrifugal rotor 30 in the separation flow path 3 Even if there is a difference in the classification conditions of the fine particles P depending on the position along the axis (the position in the depth direction of the groove 32), and even if the occurrence of the difference differs depending on the sample particles and separation conditions, the difference The fine particles P corresponding to the above can be accommodated in the respective accommodating chambers 35a and can be easily handled. In addition, the decoupling of the liquid phase motion between the separation channel 3 and each storage chamber 35a is more reliable.

  Further, since the block 36 in which the pocket 35 is provided is fitted into the groove wall surface of the concave groove 32, specifications such as the size and shape of each pocket 35 can be easily changed by replacing the block 36. Therefore, it is possible to easily adjust the fineness of the collection fraction without changing the rotor body 31. In addition, sample collection, pocket 35 cleaning, and apparatus maintenance are facilitated. Therefore, the operability as a total including sample handling can be improved when a large number of sample fractions are handled simultaneously.

  In addition, although the flow path outer wall 3b is not a smooth curved surface by forming the pocket row 35A by the plurality of pockets 35, the order of the separation field where sedimentation occurs is protected by the continuous density gradient. Even if a disturbance occurs in the separation channel 3 due to 35A, it does not affect the sedimentation process.

  The place where the pocket 35 is provided is not limited to the flow channel outer wall 3b of the separation flow channel 3, but is provided on the flow channel inner wall 3a instead of the flow channel outer wall 3b, or on both the flow channel outer wall 3b and the flow channel inner wall 3a. Also good. For example, when a microparticle sample containing microparticles having a density lower than that of the carrier liquid phase is centrifuged, the microparticles float without being settled (called floating separation). In principle, it is exactly the same as sedimentation separation. Therefore, a pocket can be provided in the flow path inner wall 3a, and fine particles that have reached the flow path inner wall 3a by floating separation can be accommodated in the pocket.

  Further, a detachable container made of resin or the like may be detachably placed on the surface of the pocket 35 to further improve operability such as sample collection, arrangement and storage, block 36 cleaning, and apparatus maintenance. By using the disposal container, work such as scraping of the sample from the pocket 35 and cleaning of the instrument wall can be made unnecessary, and work efficiency can be improved. Further, the shape of the block 36 and the disposal container can be freely set, and molding and the like are facilitated. And it can respond to the break of the block 36 by the convenience of manufacture, and can prevent a cross contamination.

  In addition to the shape corresponding to the surface shape of the pocket 35 shown in FIGS. 17 and 19, for example, the disposal container 37 covers the inside of the pocket 35 when covered with the surface of the pocket 35 having the groove shape shown in FIG. It is good also as a shape which partitions on the direction (groove depth direction of the ditch | groove 32) along the rotation center axis line of the centrifugal rotor 30, and forms several storage chambers.

  20 is a cross-sectional view showing another example of a block covered with a disposal container, and FIG. 21 is a cross-sectional view showing a state where the disposal container of FIG. 20 is detached from the block and held on a dedicated stand.

  In this embodiment, the groove width of the pocket 35 is gradually narrowed as it moves in the bottom direction (the radial direction). Further, in the inlet portion of the pocket 35, the partial wall surface 36a located on the upstream side in the liquid phase flow direction F has a shape that is chamfered in a flat shape, and the fine particles P that have flowed from the upstream side are pocketed from the inlet portion. 35 is actively introduced. The disposal container 37 covers the surface of the pocket 35 without any gap.

  Then, as shown in FIG. 21, by removing the disposal container 37 from the block 36 and holding it on the dedicated stand 38, it is possible to easily collect the fine particles P stored in the storage chambers 37a. In addition, by suppressing with a lid lined with fluoro rubber or the like, the airtightness in the storage chamber 37a can be maintained, and it can be stored even if the disposal container 37 is deformed by centrifugation.

  The sample is collected from the storage chamber 37a of the pocket 35 or the disposal container 37 by scraping with a dedicated jig, or by injecting the liquid phase with a dropper and suspending the sample in the liquid phase for inhalation. It is performed by the method.

  Since the centrifugal rotor 30 collects samples in an integrated manner by the pocket rows 35A provided on the flow channel outer wall 3b of the separation flow channel 3, the particle size distribution of the collected sample can be accurately evaluated. As shown in FIG. 16, the centrifugal rotor 30 has a plurality of blocks 36 arranged continuously from a position near the sample injection port 5 to a position near the target sample recovery port 6. Separation conditions are stabilized.

  In the case of the complete continuous system or the semi-continuous system, coarse particles are deposited on the flow path outer wall 3b of the separation flow path 3, so that the effective flow path width of the separation flow path 3 is gradually reduced. Since the linear velocity at which the carrier liquid phase on which the sample is placed is controlled by the volume flow velocity injected into the separation channel 3, a narrow effective channel width means an increase in the linear velocity of the flow and continuous operation. During this period, the separation conditions will change. The deposition on the flow channel outer wall 3b is particularly affected when the flow channel width of the separation flow channel 3 is narrow, and may affect the precise evaluation of the particle size distribution.

  On the other hand, in this apparatus, since the pocket row 35A is provided from the upstream portion to the downstream portion of the separation flow path 3, even if a deposit is generated in the separation flow path 3, it is dropped in each pocket 35. Thus, the effective cross-sectional area of the separation channel 3 does not change. When a deposit is generated, the solid phase is lost from the carrier liquid phase, but in exchange, a liquid phase having a volume equal to the volume of the lost solid phase is generated from the inside of the pocket 35. Since it comes out, the volume of the whole mobile phase does not change.

  Therefore, the effective channel width of the separation channel 3 is always kept constant, the separation condition in the separation channel 3 is stabilized, and the separation condition can be prevented from changing during continuous operation. Precision classification can be performed.

  In the above-described embodiment, the case where the pocket row 35A is used for collecting the fine particles P has been described as an example. However, the present invention is not limited to this. For example, the pocket row 35A is not used for collecting the sample. It may be used only for stabilizing the separation conditions. Further, in the completely continuous sample collection method, the pocket row 35A can be used for both the stabilization of the separation conditions and the collection of the fine particles.

  According to the fine particle classification apparatus in the present embodiment, the pocket 35 that can accommodate the fine particles P separated from the fine particle sample is provided on the flow channel outer wall 3b located outside the separation flow channel 3 in the radial direction. The fine particles P that reach the flow path outer wall 3b according to the particle diameter can be accommodated in the pocket 35 as they are, and can remain in the place, and can be prevented from moving in the flow path direction or the like. Therefore, by collecting the fine particles P from the pocket 35 after the rotation of the centrifugal rotor 30 is stopped, it is possible to obtain the fine particles P having a precisely classified desired particle diameter.

  In the above-described embodiment, the particle classification method using one particle classification apparatus has been described. However, the present invention is not limited to this. For example, the first particle classification using two particle classification apparatuses is possible. A method of alternately performing a first classification process in which fine particles are separated by an apparatus and a second classification process in which fine particles are separated by a second fine particle classification apparatus may be employed.

  For example, during the first classification process, the fine particles are collected from the pockets of the second fine particle classifier, and the second fine particle classifier is rotated at a constant rotation speed and the carrier liquid phase is at a constant flow rate. In the standby state supplied in step 2, the step of switching the supply destination of the fine particle sample from the first fine particle classifier to the second fine particle classifier, performing the second classification process, and during the second classification process, Collecting the fine particles from the pocket of the first fine particle classifier and setting the first fine particle classifier to the standby state, and switching the supply destination of the fine particle sample from the second fine particle classifier to the first fine particle classifier. Then, the step of performing the first classification process is repeated in order. Thereby, it is possible to operate in a completely continuous mode with respect to time and to maintain high separation accuracy of the fine particles.

  For example, in the case of batch operation, there is an acceleration process of the centrifugal rotor at the beginning of the operation and a deceleration process of the centrifugal rotor at the end of the operation, and it is difficult to accurately reproduce the centrifugal conditions in these portions. However, if there is only a settling (constant speed) rotation part, the accuracy of the timekeeping function in the mechanism that detects and feeds back the rotation speed is extremely high, so that the rotation speed can be reproduced with high accuracy. In addition, the geometric dimensions of the centrifugal rotor can be aligned with high accuracy between the first particle classification device and the second particle classification device, or the carrier liquid phase liquid feed pump for the first particle classification device can be used. It is also possible to mutually calibrate the flow rate and the flow rate of the carrier liquid phase liquid feed pump for the second fine particle classifier in advance. It is also possible to use one carrier liquid phase pump by switching between the first particle classification device and the second particle classification device. In this way, it is possible to align the separation conditions between the first particle classification device and the second particle classification device with high accuracy. Alternatively, the sample of the first particle classifier and the sample of the second particle classifier may be collected separately. By the above method, it is not necessary to strictly align the sample separation conditions between the first particle classification device and the second particle classification device.

<Second Embodiment>
Next, a second embodiment will be described.
In the first embodiment described above, a density gradient is formed in the carrier liquid phase by changing the concentration of the density gradient material dissolved in the carrier liquid phase. It is characterized by forming a density gradient in the carrier liquid phase by forming a temperature gradient in the phase. Specifically, at the upstream side of the continuous density gradient forming device or at the inlet (upstream portion), at least two or more carrier liquid phases having different temperatures are used instead of the density gradient materials having different concentrations in the first embodiment. In order to promote thermal diffusion in the radial direction. In the first embodiment, the transport of the density gradient material occurs in parallel with the movement of the liquid phase molecules, whereas in this embodiment, the heat transport occurs in parallel with the movement of the liquid phase molecules.

  For example, at least two or more carrier liquid phases having different temperatures are continuously supplied through two or more liquid phase supply tubes connected to the upstream portion (inlet) of the continuous density gradient generator 4 (carrier liquid). Phase supply means). In the present embodiment, a high-temperature carrier liquid phase is supplied to the rotation center side of the centrifugal rotor 2, that is, the inner side in the radial direction, and a low-temperature carrier is supplied to the outer side of the centrifugal rotor 2, that is, the outer side in the radial direction. Supply liquid phase.

  The continuous density gradient former 4 actively stirs the carrier liquid phase by using the flow of the carrier liquid phase flowing in the flow path section 11 by the stirring means 12. The stirring means 12 converts a part of the flow energy with the carrier liquid phase into stirring energy, and generates a continuous density gradient by a dynamic diffusion promotion system that actively promotes thermal diffusion in the radial direction of the carrier liquid phase. Form.

  Therefore, a carrier liquid phase having a density gradient (continuous density gradient) that continuously increases toward the outside in the radial direction of the centrifugal rotor 2 comes out from the downstream portion of the continuous density gradient forming device 4.

  As described above, when the two types of carrier liquid phases having different temperatures in the radial direction are continuously supplied from the upstream portion of the continuous density gradient former 4, the continuous density gradient former 4 While passing through 4, these two high and low temperature carrier liquid phases are merged with each other to form a temperature gradient in the radial direction of the carrier liquid phase, and there is a flat portion with respect to the radial density gradient. The continuous liquid density gradient is formed, and the carrier liquid phase having the continuous density gradient can be continuously supplied to the upstream portion of the separation channel 3 in time.

  According to the present embodiment, since it is not necessary to use a density gradient material, an operation of removing the density gradient material after classification of the sample can be omitted, and the sample processing process can be simplified. In addition, economic efficiency and environmental friendliness can be improved.

  In the first embodiment described above, a case where two types of carrier liquid phases having different bulk densities are supplied to the upstream portion of the continuous density gradient forming device 4 will be described as an example. In the second embodiment, high temperature and low temperature are supplied. The case where two types of carrier liquid phases are supplied to the upstream portion of the continuous density gradient forming device 4 has been described as an example. However, the types of carrier liquid phases are not limited to two types, and may be three or more.

  In the first embodiment described above, a case where a carrier liquid phase having a low bulk density is supplied to the inner side in the radial direction and a carrier liquid phase having a higher bulk density is supplied to the outer side in the radial direction will be described as an example. In the second embodiment described above, the case where the hot carrier liquid phase is supplied to the inside in the radial direction and the low temperature carrier liquid phase is supplied to the outside in the radial direction has been described as an example. The place to supply should just be an upstream part of the continuous density gradient forming device 4, and is not specifically limited.

  Whatever the position is mechanically supplied, a high density material is automatically moved radially outward by a strong centrifugal force to form a continuous density gradient. In addition, a carrier liquid phase having a low bulk density or a low temperature carrier liquid phase is supplied to the inside in the radial direction, and a carrier liquid phase having a high bulk density or a high temperature carrier liquid phase is supplied to the outside in the radial direction so that the radial direction It is also possible to form a continuous density gradient by exchanging the positions.

DESCRIPTION OF SYMBOLS 1 Fine particle classification device 2 Centrifugal rotor 3 Separation flow path 4 Continuous density gradient formation device 11 Flow path part 12 Stirring means 13 Round bar 21 Partition plate 22 Circular hole (hole part)
23 Slit (Hole)

Claims (13)

A separation flow path in which the supply and recovery of the carrier liquid phase and the supply and recovery of the fine particle sample are continuously performed in the centrifugal rotor, and the settling velocity method for the fine particles to be separated from the fine particle sample in the carrier liquid phase A fine particle classifier using a centrifugal separation method,
A pocket capable of accommodating the fine particles is provided on at least one of a flow channel outer wall located on the outer side in the radial direction of the separation flow channel and a flow channel inner wall located on the inner side in the radial direction of the separation flow channel. Fine particle classifier.   2. The fine particle classifier according to claim 1, wherein a plurality of the pockets are arranged at a predetermined pitch in the flow direction of the separation channel to form a pocket row.   The fine particle classifier according to claim 1 or 2, wherein the pocket row is continuously arranged from an upstream portion to a downstream portion of the separation channel. A block which is detachably attached to the rotor body of the centrifugal rotor and constitutes a part of the outer wall of the separation channel or a part of the inner wall of the channel;
The fine particle classifier according to any one of claims 1 to 3, wherein the pocket is provided on a surface of the block.   5. The fine particle classification device according to claim 1, wherein the pocket has a groove shape extending in a direction along a rotation center axis of the centrifugal rotor.   The fine particle classification device according to any one of claims 1 to 4, wherein a plurality of the pockets are provided at predetermined intervals in a direction along a rotation center axis of the centrifugal rotor.   The fine particle classification device according to any one of claims 4 to 6, further comprising a disposal container that is detachably placed on a surface of the pocket.   The fine particle classification according to claim 7, wherein the disposal container has a shape that divides the inside of the pocket in a direction along a rotation center axis of the centrifugal rotor to form a plurality of storage chambers. apparatus.   A continuous density gradient generator connected to the upstream portion of the separation channel and configured to form a continuous density gradient that is a state in which there is no flat portion of the radial gradient of the carrier liquid phase. Item 9. The fine particle classifier according to any one of Items 1 to 8.   The continuous density gradient former has a flow path portion in which the carrier liquid phase flows from the upstream side toward the downstream side, and stirring means for stirring the carrier liquid phase flowing in the flow path portion at least in the radial direction, The continuous flow is promoted by an active diffusion promoting method in which a part of the flow energy of the carrier liquid phase flowing in the flow path is converted into stirring energy by the stirring means, and the diffusion of the density gradient material in the carrier liquid phase is actively promoted. The fine particle classifier according to claim 9, wherein a density gradient is formed. A fine particle classification method using a centrifugal separation method in which a fine particle to be separated from a fine particle sample is separated in a carrier liquid phase by a sedimentation velocity method in a separation flow path in a centrifugal rotor,
By the continuous density gradient forming device provided upstream of the separation channel, a continuous density gradient is formed in which there is no flat portion with respect to the radial density gradient of the carrier liquid phase,
In the separation channel, supply and recovery of the carrier liquid phase, and supply and recovery of the particulate sample are performed continuously in time,
The fine particles are collected in a semi-continuous method in which fine particles that reach the flow path outer wall of the separation flow path are accommodated in a pocket provided in the flow path outer wall, and are collected from the pocket after the centrifugal rotor stops rotating. A fine particle classification method characterized.   A first classification process in which two fine particle classifiers according to claim 1 are used to separate the fine particles by a first fine particle classifier, and a second classification in which the fine particles are separated by a second fine particle classifier. A fine particle classification method characterized by alternately performing treatment. During the first classification process, the fine particles are collected from the pockets of the second fine particle classifier, and the second fine particle classifier is rotated by the centrifugal rotor at a constant rotational speed, and the carrier liquid phase A standby state in which is supplied at a constant flow rate;
Switching the supply destination of the fine particle sample from the first fine particle classifier to the second fine particle classifier and performing the second classification process;
Collecting the fine particles from the pockets of the first fine particle classifier during the second classification process, and setting the first fine particle classifier to the standby state;
The step of performing the first classification process by switching the supply destination of the fine particle sample from the second fine particle classification device to the first fine particle classification device is performed in order. The fine particle classification method described.

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