JP5087486B2 - Diffraction / scattering particle size distribution analyzer - Google Patents

Description

  The present invention irradiates a group of particles dispersed in a cell with light, and the particles based on the intensity distribution of diffraction and / or scattered light (hereinafter referred to as scattered light unless otherwise distinguished) generated at that time. The present invention relates to a so-called diffraction / scattering particle size distribution measuring apparatus for measuring the particle size distribution of a group.

  There are a plurality of types of cells used in this type of particle size distribution measuring apparatus for each measurement method, and representative examples thereof include batch cells, wet flow cells, and dry cells. Conventionally, in a particle size distribution measuring apparatus, usually only one cell is held exchangeably in a cell holder screwed to the apparatus main body. However, in order to replace the cell with a different type, the cell holder must be replaced. When replacing the cell holder, it is taken out of the main body of the device by loosening or unscrewing the fixed cell holder, or the cell is accommodated. It is necessary to fix the cell holder used for the measurement again with screws after being retracted in the sample chamber so that it does not get in the way, which requires considerable work. In particular, a wet flow type cell holder is connected by a pipe with a pretreatment mechanism such as an ultrasonic probe for dispersion, a stirring blade, a circulation pump, etc., which is arranged at a different location in the apparatus body. When removing it, it is necessary to remove the pipe and remove the screw that fixes the cell holder to the apparatus, which is very troublesome.

  On the other hand, as shown in Patent Document 1, a flexible material such as a silicon tube or a tube that can be bent or stretched is used for the pipe, and the cell holder is obstructed inside the sample chamber while the pipe and the cell holder are connected. Some are designed to be evacuated to a position that does not. However, since other types of cell holders (dry type cell holders, batch type cell holders, etc.) need to be taken out of the apparatus main body when not needed, it is also necessary to remove the fixing screw to the apparatus main body when replacing the cell holder. . Thus, a lot of labor is required when exchanging cells, particularly when exchanging with a different type of cell.

Furthermore, since the software installed in the conventional particle size distribution measuring device supports only one type of cell measurement method, even if it is replaced with a cell of a different type, the replaced cell type Another corresponding software must be set again, which is problematic in terms of workability and may cause an erroneous operation due to forgetting to replace the software. Such a problem becomes particularly prominent when the cells are replaced with different types of cells, but can be generated not only when the cells are replaced with the same type of cells (contents are different).
JP 2002-243622 A

  Therefore, the present invention has been made to solve the above problems all at once, and in this type of particle size distribution measuring apparatus, the work required for the replacement of the cell is saved, and the operation of the apparatus is accompanied by the replacement. The intended task is to automatically change the program to be controlled according to the cell or cell type.

  That is, the particle size distribution measuring apparatus according to the present invention includes a cell, a light source for irradiating light to the particle group accommodated in the cell, and light of diffracted light and / or scattered light generated from the light-irradiated particle group. A particle size distribution measuring device comprising: a plurality of photodetectors for detecting intensity; and an information processing device for calculating a particle size distribution of the particle group based on a light intensity signal output from each of the photodetectors. A movable holding means for holding a plurality of cells movably between a light irradiation position where the light is irradiated and a retreat position set at a position different from the light irradiation position; A stop means for stopping the cell is provided.

  With such a configuration, it is possible to irradiate the cells with light only by selectively moving one of the cells to the light irradiation position while holding the plurality of cells in the movement holding means. Therefore, the time required to change the cell can be reduced, and the work burden on the operator at that time can be reduced.

  Here, the replacement of cells includes not only switching to a different type of cell but also switching to a different cell of the same type.

  If the cell at the light irradiation position is withdrawn, other cells automatically move to the light irradiation position, and in order to further simplify the cell replacement work, the particle size distribution measuring device uses the plurality of cells. It is preferable that a cell support member that supports the cell support member is further provided, and the movement holding unit moves the cell support member along a predetermined track.

  In order to be able to replace even different types of cells such as batch cells, wet flow cells, dry cells, etc., the moving and holding means must be configured to hold a plurality of different types of cells. Is desirable.

  As a specific aspect of the moving and holding means, there may be mentioned one provided with a rail arranged along a track and configured to move the cell along the rail.

  Further, if the stop means uses a latch mechanism, the cell can be positioned accurately and easily.

  More preferably, the position of the photodetector is set to a position where diffracted light and / or scattered light generated from the particle group irradiated with light is not blocked by the cell at the retracted position.

  More preferably, the exile portion measuring device further includes cell identifying means for identifying the cell at the light irradiation position and outputting the identification signal, and the information processing device measures the particle size distribution for each cell. An operation control program storage unit storing an operation control program which is a program for controlling the operation of the apparatus, and an operation control corresponding to the cell indicated by the cell identification signal received from the identification means What is necessary is just to have a program switching means for automatically switching to a program.

  If it is such, it can switch to the program which controls the action | operation of the authority distribution measuring apparatus corresponding to the cell automatically with replacement | exchange of a cell, and can aim at reduction of an operator's work burden and an erroneous operation.

  In addition, for the cell identification, a mechanism such as reading the shape of the cell itself or a barcode attached to the cell may be used. However, in order to identify the cell more easily and without affecting the measurement, the identification is performed. It is desirable that the means outputs the cell identification signal by identifying the cell holder holding the cell at the light irradiation position.

  Thus, according to the present invention, the particle size distribution measuring apparatus that can replace the complicated mounting and detaching operations from the particle size distribution measuring apparatus in the cell replacement operation with a simple movement operation along the movement holding means. Can be provided. Therefore, the time required to change the measurement can be shortened, and further, the burden on the operator can be reduced.

  Embodiments of the present invention will be described below with reference to the drawings.

  The particle size distribution measuring apparatus 1 according to the present embodiment utilizes the fact that the scattering pattern (angle distribution of scattered light intensity) of the scattered light LS generated when the particle group is irradiated with the irradiation light L is determined by the particle diameter, By detecting the scattering pattern, the particle size distribution is measured from the MIE scattering theory. A schematic overview of the particle size distribution measuring apparatus 1 is shown in FIGS. In the figure, reference numerals C1, C2, and C3 denote cells that contain a sample in which a measurement target particle group is dispersed in a dispersion medium. The dispersion medium is generally water in the case of wet and air in the case of dry. Reference numeral 2 denotes a light source that irradiates the cells C1, C2, and C3 with irradiation light L. In this embodiment, for example, a semiconductor laser that emits coherent laser light is used as the light source. Reference numerals 31 and 32 are photodetectors arranged around the cells C1, C2, and C3. Then, the light intensity of the scattered light LS generated from the particle group irradiated with the light L is detected. Reference numeral 4 denotes a signal processing unit including a buffer, an amplifier, and the like that receive the scattered light intensity signals output from the photodetectors 31 and 32 and perform processing such as conversion. Reference numeral 5 denotes an information processing apparatus that calculates the particle size distribution of the particle group based on the value of each scattering intensity signal processed by the signal processing unit 4. Reference numeral 8 denotes a convex lens that is set so that the transmitted light L converges at the center of the light receiving surface of the photodetector 32.

  Therefore, in this embodiment, the cell support member 9 that integrally supports a plurality of different types of cells C1, C2, and C3 in a cell storage chamber (not shown) is provided, and the movement holding means 6 is further provided.

  The cell support member 9 has, for example, a long plate shape, and holds the cells C1, C2, and C3 on the upper surface thereof in a straight line along the long side. Specifically, the cells C1, C2, and C3 are detachably held by cell holders C1h, C2h, and C3h. In FIG. 2, the cell support member 9 holds the three different types of cells C1, C2, and C3 in FIG. 2, but it is also possible to hold a plurality of the same type of cells.

  Here, the cell holders C1h, C2h, and C3h are for holding the cells C1, C2, and C3 on the cell support member 9, and have, for example, a rectangular plate shape. The long side has a width larger in the optical axis direction than the width of the cell support member 9 attached to the lower surface of the cell holders C1h, C2h, C3h, and the cells C1, C2, C3 can be attached to and detached from the upper surface. It is attached.

  The cell C1 is of a dry type and is integrated with the cell holder C1h. As shown in FIG. 2, a sample inlet C1t for introducing particles is provided at the upper part, and a suction pipe C1v for sucking particles is attached to the lower part, and dispersed in a dispersion medium such as air in the meantime, A window C1w such as a circle for irradiating the dropped particle group with the irradiation light L is provided.

  The cell C2 is of the wet flow type, and the upper and lower sides are held on the cell support member 9 by the wet cell holder C2h. The cell C2 is provided on the liquid circulation channel together with a particle agitation device such as a circulation pump and an ultrasonic probe (not shown) in order to disperse the particles in a liquid solvent such as water. In the figure, reference numerals C2a and C2b are pipes C2a and C2b that form the liquid circulation flow path and are respectively connected to the lead-in / out ports of the cell C2.

  The cell C3 is a so-called batch type suitably used for measuring a small amount of sample, and the lower part thereof is held on the cell support member 9 by a batch type cell holder C3h.

  The movement holding means 6 holds the cell support member 9 movably on a rail 11 disposed on the floor surface of the cell storage chamber along a track 10 which is a straight line orthogonal to the optical axis 12. Accordingly, the cells C1, C2, and C3 can be moved between a light irradiation position P that is a portion where the optical axis 12 and the orbit 10 intersect and a retreat position that is the other portion.

  At this time, in order to prevent the cells C1, C2, C3 in the retracted position from blocking the scattered light LS incident on the photodetectors 31, 32, for example, the photodetectors 31, 32 positions are set.

  Further, as a mechanism for stopping the cells C1, C2, and C3 that have moved to the light irradiation position P at the position P, stop means (not shown) using a latch mechanism using a spring or the like is provided.

  Furthermore, the particle size distribution measuring apparatus 1 according to the present embodiment is provided with cell identifying means 7 for identifying the cells C1, C2, C3 at the light irradiation position P and outputting the identification signal. Then, the information processing device 5 receives the cell identification signal, and the program is switched so that the operation of the particle size distribution measuring device 1 corresponds to the cell type.

  As shown in FIG. 3, the cell identification means 7 has a Hall sensor 71, and identifies the identified portion 72 of the cell holders C1h, C2h, C3h. Here, the identified portion 72 is provided with a plurality of holes 73 on a straight line at equal intervals in the end portions of the cell holders C1h, C2h, C3h to which the cells C1, C2, C3 are not attached. A magnet 74 is arranged in a different hole 73 for each cell type. Further, the Hall sensor 71 is arranged so as to correspond to each hole 73 provided in the cell holder C1h, C2h, C3h when any of the cells C1, C2, C3 is arranged at the light irradiation position P. It is installed below the cell holders C1h, C2h, C3h. Then, the cells C1, C2, and C3 are identified by detecting the identified portion 72 of the cell holder at the light irradiation position P, and a cell identification signal is output.

  As shown in FIG. 4, the information processing apparatus 5 is a general-purpose or dedicated computer having a CPU, a memory, an input / output interface, and the like. As shown in FIG. 5, the functions of the operation control program storage unit 51, the program switching means 52, and the like are also exhibited.

  The operation control program storage unit 51 stores an operation control program which is a program for controlling the operation corresponding to the cell type of the particle size distribution measuring apparatus 1. In the present embodiment, a dry cell measurement program storage unit 511 storing a measurement program corresponding to the dry cell C1, a wet flow cell measurement program storage unit 512 storing a measurement program corresponding to the wet flow cell C2, and a batch cell. A batch type measurement program storage unit 513 that stores a measurement program corresponding to C3.

  The dry cell measurement program displays the measurement screen 13 in FIG. 6 and the condition setting dialog 14 in FIG. 7 on the screen of the particle size distribution measuring apparatus 1, and further sets the dry processing, initialization processing, and dry measurement sequence. I do. The measurement screen 13 is a screen for performing dry measurement 131, blank measurement 132, optical axis adjustment 133, and the like. The condition setting dialog 14 is used to make detailed settings for dry measurement. Specific condition settings include conditions such as temperature setting 141, automatic print or automatic save setting 142, sample adjustment (sieving speed setting 143, suction setting 144, compression air pressure setting 145), blank measurement time setting 146, etc. There is a setting.

  The wet flow cell measurement program displays the measurement screen 15 in FIG. 8 and the condition setting dialog 16 in FIG. 9 on the screen of the particle size distribution measuring apparatus 1, and further sets the wet operation processing, initialization processing, and wet measurement sequence. I do. The measurement screen 15 includes wet measurement 150, optical axis adjustment 151, blank measurement 152, drainage 153, partial drainage 154, defoaming 155, automatic dispersion medium injection 156, partial dispersion medium automatic injection 157, cleaning 158, It is a screen for performing automatic dilution 159 of a sample. The condition setting dialog 16 is used to make detailed settings for wet measurement. Specific condition settings include temperature setting 161, automatic print or automatic save setting 162, blank measurement time setting 163, sample adjustment (circulation speed setting 164, ultrasonic time / intensity setting 165, 166), and washing frequency setting. There are condition settings such as 167.

  The batch type measurement program displays the measurement screen 17 of FIG. 10 on the screen, and performs settings such as calculation processing, initialization processing, or measurement sequence. The measurement screen 17 is for performing batch type measurement 171, optical axis adjustment 172, blank measurement 173, and the like.

  The program switching means 52 receives the cell identification signal output from the cell identification means 7 and identifies the cell type by the cell identification signal. Then, the program is changed so that the particle size distribution measuring apparatus 1 has an operation specification corresponding to the cell type. Thereby, the screen display or processing conditions can be automatically changed.

  Next, an example of a particle size distribution measurement procedure using the apparatus 1 will be described below.

  First, the operator slides the cell support member 9 on the rail 11, and moves a desired cell (for example, C2) to the light irradiation position P. This state is the state shown in FIG. Whether or not the cell C2 exists at the light irradiation position P can be determined by a click stop feeling by the latch mechanism. And as shown in FIG. 11, the cell identification means 7 identifies a cell, and outputs a cell identification signal (step S1). The output cell identification means 7 is received by the program switching means 52 (step S2), and a program corresponding to the cell C2 is selected and activated (step S3). And based on the selected program, it displays on the screen of the particle size distribution measuring apparatus 1 as shown in FIG. 8 and FIG. 9, and sets (changes) the processing conditions and the like (step S4). Then, if measurement is started as usual (step S5), the particle size distribution of the particle group accommodated in the cell C2 is obtained.

  When measuring the particle groups of the other cells C1 and C3, the cell support member 9 may be slid as described above.

  The pipes C1v, C2a, and C2b are connected to the cells C1 and C2, respectively. However, since the pipes C1v, C2a, and C2b have some or all of the flexibility as described above, the cell C1 Since it is deformed with the movement of C2, it is easy to attach and detach, and the movement of the cells C1 and C2 is not hindered.

  FIG. 13 shows the dry cell C1, and FIG. 14 shows the state where the batch cell C3 has been moved from the retracted position to the light irradiation position P. FIG.

  As described above, according to the present embodiment, the cells C1, C2, and C3 only need to be slid using the movement holding means 6 when replacing the cells, and it is not necessary to attach or remove them, so that workability is hindered. Never do. In addition, the program for controlling the operation of the apparatus can be automatically changed according to the cell type in accordance with the replacement. Therefore, the time required for changing the measurement can be shortened, and further, the burden on the operator can be reduced, and whether the desired cells C1, C2, and C3 are set at the irradiation position P is only on the screen. Therefore, it is possible to prevent erroneous operation.

  Further, since the latch mechanism is provided, the cells C1, C2, and C3 can be accurately and easily positioned at the light irradiation position P.

  Further, a plurality of cells C1, C2, C3 are held by one cell support member 10, and the cells C1, C2, C3, C1, C2, C3 are retracted from the light irradiation position P to the light irradiation position P at a time. The movement of C3 can be performed.

  In addition to the above, in the present embodiment, the cells C1, C2, and C3 moved at the retracted position by making the rail 12 of the movement holding means 6 linear are arranged in a straight line, and therefore the cells C1 and C2 that block the scattered light LS. , C3 can be reduced, and the area where the photodetector 3 can be arranged can be widened.

  The present invention is not limited to the above embodiment.

  For example, even if the cells are of the same type, the setting (for example, setting of the refractive index) may be different if the measurement object accommodated in the cell is different. You may make it change automatically to the program corresponding to.

  In the above embodiment, the particle size distribution measuring apparatus using a dry cell, a wet flow cell, and a batch cell is shown. However, the combination of the cells is not limited to these, and for example, a dry cell and a wet flow cell are used. But it ’s okay. Or what used two kinds, a wet flow cell and a batch type cell, may be used.

  The identified portion of the cell identifying means is not limited to the one in which the magnet is disposed in the hole, but may be a barcode or the like, or the identified portion may be provided on the side surface of the cell holder in the light incident direction.

  Furthermore, although the number of holes in the embodiment is four, for example, holes may be provided as many as the number of cell types, or the number of holes in which magnets are arranged may be changed.

  Further, the trajectory is not limited to a straight line, and may be, for example, a curved one.

  The moving and holding means includes not only those using rails but also, for example, robot arms and belt conveyors.

  In addition, if an actuator for moving the cell is provided, it is not necessary for the operator to move the cell by itself, and the replacement of the cell or the cell holder can be further saved.

  In addition, as long as the cell support member can be attached to and detached from the measurement apparatus main body and can be attached to a plurality of cells, and a plurality of cell support members can be connected, it is possible to provide as many cells as necessary, and the light irradiation position. And movement between the retreat positions and fixation at each position can be performed simultaneously.

  Furthermore, various types of cells or cell holders can be used depending on the purpose as long as it is possible to attach a replaceable adapter that fixes the cell support member and various cells at appropriate distances so that the irradiation light irradiates the sample. It is possible to prepare, and it is possible to cope with the use of an existing cell or an unknown cell that will appear in the future.

  Of course, the information processing device, the signal processing unit, the control unit of the particle size distribution measuring device, and the device main body are not integrated. For example, the signal processing unit and the information processing device are outside the particle size distribution measuring device main body. The one in Alternatively, the information processing device, the signal processing unit, and the control unit of the particle size distribution measuring device may be provided outside the apparatus main body. In addition, the present invention can be variously modified without departing from the spirit of the present invention.

1 is a schematic overall view showing a configuration of a particle size distribution measuring apparatus according to an embodiment of the present invention. The perspective view which showed the movement holding means vicinity in the same embodiment. The schematic diagram which shows the structure of the cell identification means in the same embodiment. The equipment block diagram which shows the equipment structure of the information processing apparatus in the embodiment. The functional block diagram which shows the function structure of the information processing apparatus in the embodiment. The figure which shows the measurement screen corresponding to the dry cell in the same embodiment. The figure which shows the condition setting dialog corresponding to the dry cell in the same embodiment. The figure which shows the measurement screen corresponding to the wet flow cell in the embodiment. The figure which shows the condition setting dialog corresponding to the wet flow cell in the embodiment. The figure which shows the measurement screen corresponding to the batch type cell in the same embodiment. The flowchart which shows the switching of the action | operation of the particle size distribution measuring apparatus in the embodiment. The top view which shows the case where the wet flow cell is selected in the same embodiment. The top view which shows the case where the dry type cell is selected in the same embodiment. The top view which shows the state by which the batch type cell was selected in the same embodiment.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Particle size distribution measuring device C1, C2, C3 ... Cell 2 ... Light source 31, 32 ... Photodetector 5 ... Information processing device 51 ... Operation control program storage part 52- ··· Program switching means 6 ··· Moving and holding means 7 ··· Cell identifying means 9 ··· Cell support member 10 ··· Track 11 ··· Rail 12 ··· Optical axis L ··· Light LS ··· .Diffraction and / or scattered light P ... light irradiation position

Claims (7)

Detect the light intensity of the diffracted light and / or scattered light generated from the cell, the light source that irradiates the particle group accommodated in the cell, and the light irradiated particle group , and calculate the angular distribution of the light intensity Diffraction / scattering type particle size distribution measurement comprising: a plurality of photodetectors for performing measurement; and an information processing device for calculating a particle size distribution of the particle group based on a light intensity signal output from each of the photodetectors In the device
A movement holding means for holding a plurality of cells movably between a light irradiation position where the light is irradiated along a predetermined trajectory and a retreat position set at a position different from the light irradiation position;
Stop means for selectively stopping any one cell at the light irradiation position,
A diffraction / scattering particle size distribution measuring apparatus, wherein positions of a plurality of detectors for calculating an angular distribution of the light intensity are set in a plane perpendicular to the orbit. The diffraction / scattering particle size distribution measuring apparatus according to claim 1, wherein one of the cells is a flow cell in which a part or all of the cells are connected to a flexible pipe. The cell support member that integrally supports the plurality of cells is further provided, and the movement holding means moves the cell support member along a predetermined trajectory. The diffraction / scattering particle size distribution measuring apparatus as described. 4. The diffraction / scattering type particle size distribution measuring apparatus according to claim 1, wherein the moving and holding means is capable of holding a plurality of different types of cells. 5. The diffraction / scattering type according to claim 1, wherein the movable holding means includes a rail arranged along a track, and moves the cell along the rail. Particle size distribution measuring device. 6. The diffraction / scattering type particle size distribution measuring apparatus according to claim 1, wherein the stopping means uses a latch mechanism. The position of the photodetector is set to a position where diffracted light and / or scattered light generated from a group of particles irradiated with light is not blocked by the cell at the retracted position. The diffraction / scattering particle size distribution measuring apparatus according to 1, 2, 3, 4, 5 or 6.