JP6984501B2 - Particle measuring device - Google Patents

Description

The present invention relates to a particle measuring device for measuring a physical quantity of a sample particle.

Generally, when confirming the properties, quality, etc. of a powder product at the time of development or manufacturing, the physical quantity (for example, particle size distribution, surface state, constituent elements, etc.) of the sample particles, which are powders, is measured. ing. For example, a laser scattering / diffraction method or an image analysis method is used for measuring the particle size distribution. In the laser scattering / diffraction method, the particle size distribution is measured (calculated) by irradiating the sample particles with parallel light such as laser light and measuring and analyzing the pattern of the light diffracted and scattered by the sample particles. In the image analysis method, the particle size distribution is calculated by photographing a sample particle group with a CCD (Charged-coupled devices) camera or the like and performing image analysis.

An image analysis type particle size distribution measuring device is described in, for example, Patent Document 1. Patent Document 1 describes a device that photographs a group of falling sample particles with a CCD camera or the like to perform image analysis, and measures the particle size distribution using a statistical method. Such an image analysis type particle size distribution measuring device has come to be able to perform highly accurate measurement by increasing the speed of a computer, increasing the resolution of an image capturing device, and the like.

In the image analysis method, since the outer diameter, shape, etc. of the sample particles are measured from the captured image, a plurality of sample particles are prevented from overlapping at the time of imaging. Specifically, when the particle concentration of the turbid liquid (slurry) as a dispersion containing the sample particles as a dispersoid is high, it is necessary to sufficiently dilute the slurry to disperse the sample particles to be measured. ..

As a method of supplying the sample particles to be measured, there are an offline method in which the sample particles taken out from the powder manufacturing device in advance are sent to the particle size distribution measuring device, and an in-line method in which the slurry is taken out directly from the powder manufacturing device and sent to the particle size distribution measuring device. be.

The in-line method is advantageous for measuring the particle size distribution at an early stage in the particle manufacturing process. In the in-line method, the slurry containing the sample particles is flowed in the transfer tube laid from the powder manufacturing apparatus to the particle size distribution measuring apparatus, and the slurry is transferred to the particle size distribution measuring apparatus. In the in-line method, when the slurry containing the sample particles is transferred through the transfer tube, many sample particles may settle in the transfer tube. Therefore, the measured value of the physical quantity of the sample particle may vary, and the physical quantity of the sample particle may not be measured accurately.

Japanese Unexamined Patent Publication No. 11-258141

An object of the present invention is to provide a particle measuring device capable of accurately measuring a physical quantity of sample particles in a slurry.

According to one aspect of the invention
The first container to store the slurry and
A second container for the diluent and
A third container containing the diluted solution obtained by diluting the slurry with the diluted solution, and
It has a circulation tube for circulating the slurry in the first container outside the first container.
A first pipe that supplies at least the slurry into the third container is connected to the circulation pipe by using a first pipe connecting member that is a branch joint member.
On the downstream side of the first pipe from the first pipe connecting member, a second pipe that supplies the diluting liquid in the second container into the third container via the first pipe branches. It is connected using the second pipe connecting member, which is a joint member, and is connected.
The first pipe connecting member and the second pipe connecting member are each provided as a particle measuring device so that the height position of the second pipe connecting member is higher than the height position of the first pipe connecting member. Is provided.

According to the present invention, the physical quantity of the sample particles in the slurry can be accurately measured.

It is a figure which shows the structural example of the particle measuring apparatus which concerns on one Embodiment of this invention. It is an enlarged schematic diagram around the 1st tube connecting member and the 2nd tube connecting member in the particle measuring apparatus which concerns on one Embodiment of this invention. It is an enlarged block diagram which shows typically the support member which the particle measuring apparatus which concerns on one Embodiment of this invention has. It is a figure which shows the structural example of the particle measuring apparatus which concerns on other embodiment of this invention.

<One Embodiment of the present invention>
Hereinafter, an embodiment of the present invention will be described with reference to the drawings.

(1) Configuration of Particle Measuring Device FIG. 1 shows a schematic view of the particle measuring device 100 according to the present embodiment, and FIG. 2 shows an enlarged schematic view of the periphery of the first tube connecting member and the second tube connecting member. .. The arcuate solid arrows in FIGS. 1 and 2 indicate the direction of rotation of the pump. The particle measuring device 100 is a device for measuring a physical quantity of a sample particle. In the present embodiment, a case where the particle size measuring device 100 is an in-line type particle size distribution measuring device for measuring the particle size distribution of the sample particles will be described as an example.

The sample particles to be measured are, for example, metal-based particles having a relatively large specific gravity. The sample particles have a particle size of approximately 0.1 μm to several hundred μm. The sample particles may be, for example, an inorganic powder containing a ceramic material. In the following, a case where the sample particles are metallic particles will be described as an example. There are no particular restrictions on the measurement items of the sample particles. It is possible to measure the physical quantities of the sample particles such as the particle size distribution of the sample particles, the surface state of the sample particles, and the constituent elements (for example, the ratio of the constituent elements) of the sample particles. For example, a laser scattering / diffraction method or an image analysis method is used for measuring the particle size distribution of sample particles. In particular, in the image analysis method, not only the particle size distribution but also the outer diameter, area, angle of protrusions on the contour, center of gravity, perimeter, etc. can be measured. Image analysis also has the advantage that the time required for measurement is relatively short. Therefore, in the following, the measurement of the particle size distribution using the image analysis method will be described as an example.

As shown in FIG. 1, the particle measuring device 100 includes a tank 38 as a first container for accommodating the slurry 21, a tank 39 as a second container for accommodating the diluting liquid 22, and a diluting liquid 22 for the slurry 21. It has a tank 2b as a third container for accommodating the diluted solution 23 diluted with. The particle measuring device 100 automatically measures the particle size distribution of the sample particles collected from the slurry 21.

The slurry 21 can be obtained by mixing a predetermined amount of a dispersion medium or the like with the metal-based particles as the dispersoid. As the diluting liquid 22, for example, the same liquid as the dispersion medium of the slurry 21 can be used. Pure water or the like may be used as the diluting liquid 22. In this embodiment, pure water is used as the diluting liquid 22. The diluting liquid 23 is produced by diluting the slurry 21 with the diluting liquid 22 to, for example, about 1/100 to 1/40000.

The slurry 21 exists in the tank 38 in a state of being dispersed by stirring. A circulation tube (circulation tube) C10 for circulating the slurry 21 in the tank 38 outside the tank 38 is connected to the tank 38. The circulation pipe C10 is configured such that the slurry 21 pumped out from the tank 38 flows in the pipe and then returns to the inside of the tank 38.

The circulation pipe C10 is provided with a pump (slurry pump) 10. As the pump 10, for example, a tube pump can be used. The pump 10 is configured to rotate at a constant rotational speed and provide a constant discharge flow rate. By rotating (operating) the pump 10, the slurry 21 can be pumped from the inside of the tank 38 into the circulation pipe C10 (outside the tank 38), and the slurry 21 flowing in the circulation pipe C10 can be returned to the inside of the tank 38. That is, the slurry 21 can be circulated in the circulation tube C10.

Since the metal particles (sample particles) to be measured contained in the slurry 21 have a relatively large specific gravity as described above, they easily precipitate unless the slurry 21 is circulated at a certain flow velocity. In addition, the sample particles to be measured may be partially solidified by drying. In order to prevent precipitation, solidification, etc. of the sample particles, it is preferable to constantly rotate the pump 10 and constantly circulate the slurry 21 in the tank 38 in the circulation tube C10 while the particle measuring device 100 is in operation. The flow velocity of the slurry 21 circulating in the circulation pipe C10 can be adjusted, for example, by adjusting the rotation speed of the pump 10.

A pipe (tube) C11 as a first pipe is connected to the downstream side of the circulation pipe C10 on the downstream side of the pump 10 by using a first pipe connecting member 31 (hereinafter, also referred to as a connector 31) which is a branch joint member. ing. As the connector 31, for example, a three-way cheese joint (T joint) or a Y joint can be used. The connector 31 constitutes a connection point at which the tube C11 is connected to the circulation tube C10.

The pipe C11 is provided with a pump (supply pump) 11. As the pump 11, for example, a tube pump can be used. The pump 11 is configured to rotate at a constant rotational speed and provide a constant discharge flow rate. By rotating (operating) the pump 11, the slurry 21 flowing in the circulation pipe C10 can be drawn into the pipe C11, and the drawn slurry 21 can be supplied (transferred) into the tank 2b. When the rotation of the pump 11 is stopped, the flow of the fluid such as the slurry 21 in the pipe C11 is stopped, and the fluid in the pipe C11 is completely blocked in the pipe C11.

A pipe (tube) C12 as a second pipe is connected to the tank 39. The downstream end of the pipe C12 is connected to the downstream side of the connector 31 of the pipe C11 by using a second pipe connecting member 32 (hereinafter, also referred to as a connector 32) which is a branch joint member. As the connector 32, for example, a T joint or a Y joint can be used. The connector 32 constitutes a connection point at which the pipe C12 is connected to the pipe C11.

The pipe C12 is provided with a pump (diluting liquid pump) 12. As the pump 12, for example, a tube pump can be used. The pump 12 is configured to rotate at a constant rotational speed and provide a constant discharge flow rate. By rotating (operating) the pump 12, the diluting liquid 22 can be pumped from the tank 39 into the pipe C12 and supplied (transferred) into the tank 2b via the pipe C11. When the rotation of the pump 12 is stopped, the flow of the diluting liquid 22 in the pipe C12 is stopped, and the diluting liquid 22 in the pipe C12 is completely blocked in the pipe C12.

From the viewpoint of reducing the slurry 21 consumed in step 2 (sampling) described later, it is preferable that the distance D1 (see FIG. 2) between the connector 31 and the connector 32 is as short as possible. The distance D1 in the present specification is the length of the tube C11 (hereinafter, the tube C11 in this portion is also referred to as the tube C11a) located between the connector 31 and the connector 32, that is, the tube C11 and the circulation tube C10. It refers to the length from the connection point (upstream end of the pipe C11) to the connection point between the pipe C12 and the pipe C11. The distance D1 is preferably, for example, 0.05 meters (5 cm) or less. When the distance D1 is 5 cm, the amount of slurry 21 retained in the tube C11a is, for example, 0.63 ml.

Even when the distance D1 is shortened as much as possible, if the height position of the connector 31 and the height position of the connector 32 are the same, the slurry 21 stays in the tube C11a and the measurement particles in the slurry 21. Precipitates in the tube C11a. If sample particles settle in the tube C11a, it may not be possible to measure an accurate physical quantity.

Therefore, in the present embodiment, as shown in FIG. 2, the connector 32 is provided so that its height position is higher than the height position of the connector 31. As a result, when the slurry 21 is not supplied to the downstream side of the connector 32 in the pipe C11 due to the operation of the pump 12, the slurry 21 in the pipe C11a flows back (discharged) into the circulation pipe C10. .. Therefore, even when the sample particles in the slurry 21 are settled in the tube C11a, the settled sample particles are discharged into the circulation tube C10 together with the discharge of the slurry 21, and the sample particles in the slurry 21 are discharged in the tube C11a. Sample particles are less likely to remain. As a result, when measuring the physical quantity of the sample particles, it is possible to measure the physical quantity more accurately than when the height positions of the connectors 31 and 32 are the same.

When the arrangement angle of the tube C11a is 0 ° when the connector 31 and the connector 32 are provided at the same height position, the arrangement angle of the tube C11a is, for example, 5 to 90 ° (5 ° or more and 90). It is preferable that the connector 31 and the connector 32 are provided so as to be within the range of °). From the viewpoint of discharging the slurry in the pipe C11a into the circulation pipe C10 when the pump 12 is operated, the arrangement angle of the pipe C11a is preferably closer to 90 °, most preferably 90 °. However, it is practical to set the arrangement angle within the range of about 15 to 50 ° due to the shapes of the connectors 31 and 32 and the like. It is most practical to set the arrangement angle to about 45 °, and the connector 31 and the connector 32 can be easily arranged.

As shown in FIG. 3, the connector 31 and the connector 32 are supported by the support member 40. The support member 40 includes a first plate-shaped member 41 to which a connector 31 is mounted, and a second plate-shaped member 42 mounted on the first plate-shaped member 41 and having a supported surface 45. The support member 40 is arranged on the mounting table so that the supported surface 45 is in contact with the mounting table (not shown). The support member 40 is configured so that the height position of the connector 31 with respect to the supported surface 45 can be adjusted by sliding the positional relationship between the first plate-shaped member 41 and the second plate-shaped member 42 in the vertical direction. There is. In the support member 40 illustrated in FIG. 3, a screw hole is formed in the first plate-shaped member 41, and a long hole (long screw hole) 43 for inserting a long screw in the height direction is formed in the second plate-shaped member 42. It is formed. Then, after adjusting the height position of the connector 31 by sliding the first plate-shaped member 41 in the vertical direction, the first plate is screwed by inserting the screw 44 into the screw hole and the elongated hole 43. The shaped member 41 is fixed to the second plate-shaped member 42.

As shown in FIG. 1, a transfer unit (circulation unit) 7 which is a functional element for transferring various fluids is mainly composed of a tank 38, a circulation pipe C10, a pipe C11, a pipe C12, a connector 31, and a connector 32. Will be done. The tank 39 and the pumps 10 to 12 may be included in the transfer unit 7. The pump 11 and the pump 12 form a sampling pump unit. Further, the diluting unit 2 is mainly composed of the tank 2b.

A circulation tube (circulation tube) C1 for circulating the diluted solution 23 in the tank 2b outside the tank 2b is connected to the tank 2b. The circulation pipe C1 is configured such that the diluting liquid 23 pumped out from the tank 2b flows in the pipe and then returns to the inside of the tank 2b.

The circulation pipe C1 is provided with a pump (circulation pump) 3a. As the pump 3a, for example, a tube pump can be used. The pump 3a is configured to rotate at a constant rotational speed and provide a constant discharge flow rate. By rotating (operating) the pump 3a, the diluting liquid 23 is pumped from the inside of the tank 2b into the circulation pipe C1 (outside of the tank 2b), and the diluting liquid 23 flowing in the circulation pipe C1 is returned to the inside of the tank 2b. That is, the diluent 23 can be circulated in the circulation tube C1.

A flow cell 36 is provided on the downstream side of the circulation pipe C1 with respect to the pump 3a. The flow cell 36 is an optical cell through which the diluent 23 (fluid containing sample particles) flows. In the present embodiment, the surface facing the camera 35 described later and the surface facing the lighting device 37 described later are configured to be optically transparent. The diluted solution 23 drawn into the circulation tube C1 passes through the flow cell 36 when circulating in the circulation tube C1.

A lighting device 37 that irradiates the flow cell 36 with a predetermined light is arranged. As the lighting device 37, for example, a surface light emitting type light emitting diode can be used. The lighting device 37 is configured so that the light emission (strobe light emission) timing is controlled by the calculation unit 5 described later. The lighting device 37 may be configured to emit light constantly.

A camera 35 is arranged at a position facing the lighting device 37 with the flow cell 36 in between. The camera 35 is a photographing device that photographs sample particles contained in the diluent 23 flowing in the flow cell 36 and transmits (outputs) the captured particle image to the calculation unit 5 described later. For example, the camera 35 captures an image of the sample particles in the diluent 23 in the flow cell 36 by receiving the light irradiated by the lighting device 37 and transmitted through the flow cell 36. The camera 35 is composed of a photographing element such as a CCD camera and a CMOS (Complementary metal-axis-semiconductor). The camera 35 has a lens 35a. As the lens 35a, it is preferable to use, for example, a telecentric lens. As a result, even if the distance between the sample particles to be photographed and the lens 35a in the direction of the optical axis of the camera 35 changes, the size of the image of the sample particles in the photographed image does not change.

Mainly, the circulation tube C1, the camera 35, the flow cell 36, and the lighting device 37 constitute a measurement unit 3 which is a data acquisition unit for acquiring data regarding sample particles in the diluent 23. The pump 3a may be included in the measuring unit. The measuring unit 3 acquires, for example, data necessary for measuring the particle size distribution of the sample particles in the diluent 23.

A discharge pipe C2 for discharging the diluted solution 23 in the tank 2b is connected to the tank 2b. The discharge pipe C2 extends from the tank 2b to the outside of the particle measuring device 100. The discharge pipe C2 is provided with a pump (discharge pump) 4a as a discharge device. By rotating (operating) the pump 4a, the diluting liquid 23 can be drawn from the tank 2b into the discharge pipe C2. The diluted solution 23 in the tank 2b is discharged to the outside of the particle measuring device 100 after passing through the discharge pipe C2. The discharge section 4 is mainly composed of the discharge pipe C2 and the pump 4a.

The main body 1 is mainly composed of the diluting section 2, the measuring section 3, and the discharging section 4.

The arithmetic unit 5, which is a control unit, is configured as a computer including a CPU (Central Processing Unit), a volatile storage device, a non-volatile storage device, an input / output interface (input / output device), and the like. The calculation unit 5 is a functional element that executes various operations. The calculation unit 5 is isolated from the main body unit 1, the transfer unit 7, and the like, and is installed in a separate room 6 (office or the like) that is not affected by mist, dust, or the like. This eliminates the need for special measures such as dust.

The calculation unit 5 is connected to the above-mentioned pumps 10-12, 3a, 4a, a camera 35, a lighting device 37, and the like. The calculation unit 5 is configured to control the start, stop, and rotation speeds of the pumps 10 to 12, 3a, 4a, the shooting timing of the camera 35, the light emission timing of the lighting device 37, and the like. For example, the calculation unit 5 is configured to control the shooting timing of the camera 35 and the light emitting timing of the lighting device 37 so that the lighting device 37 emits strobe light in synchronization with the shooting timing of the camera 35.

The calculation unit 5 is configured to record, for example, an image taken by the camera 35, analyze the image, calculate and store data necessary for measuring the particle size distribution of the sample particles. Further, the calculation unit 5 is configured to calculate and store the particle size distribution of the sample particles based on the calculated data. Further, the calculation unit 5 is configured to output the calculated particle size distribution or the like by using an output device such as a speaker or a display.

(2) Particle Physical Quantity Measurement Process A process for measuring the physical quantity (for example, particle size distribution) of particles in the slurry 21 will be described using the particle measuring device 100 described above. In the following description, the operation of each unit constituting the particle measuring device 100 is controlled by the arithmetic unit 5.

[Step 1: Stirring of slurry]
The rotation of the pump 10 is started to circulate the slurry 21 in the circulation pipe C10. In order to prevent the sample particles from settling, solidifying, etc. in the tank 38, the rotation of the pump 10 is continuously performed at least until the completion of step 2 described later.

[Step 2: Sampling]
After a predetermined time has elapsed from the start of rotation of the pump 10, the slurry 21 and the diluting liquid 22 are supplied into the tank 2b, and the diluting liquid 23 is generated in the tank 2b.

Specifically, with the rotation of the pump 12 stopped, the rotation of the pump 11 is started, and the slurry 21 is drawn from the inside of the circulation pipe C10 to the downstream side of the connector 32 in the pipe C11. After a predetermined time (for example, 1 to 6 seconds) has elapsed from the start of rotation of the pump 11, the rotation of the pump 12 is started while the rotation of the pump 11 is maintained, and the diluting liquid 22 is drawn into the pipe C12. When the pump 11 and the pump 12 are operating at substantially the same discharge flow rate, the slurry 21 circulating in the circulation pipe C10 is hardly drawn into the portion downstream of the connector 32 in the pipe C11. .. The diluting liquid 22 drawn into the tube C12 is transferred into the tank 2b via the connector 32 and the tube C11.

When the diluting liquid 22 flows in the pipe C11, the diluting liquid 22 flows in the pipe C11 while pushing the slurry 21 previously drawn into the pipe C11. As a result, the slurry 21 is supplied into the tank 2b, and then the diluted solution 22 is supplied. In the tank 2b, the diluting liquid 23 in which the slurry 21 is diluted by the diluting liquid 22 is accumulated.

When the predetermined time elapses and the slurry concentration in the diluent 23 becomes a concentration suitable for measuring the particle size distribution and the amount of the diluent 23 in the tank 2b reaches a desired amount, the pumps 11 and 12 are rotated at the same time. Stop and stop the transfer of the diluting liquid 22 to the tank 2b. The operating time of the pumps 11 and 12 is calculated from the inner diameter, length, etc. of the pipe C11.

As described above, in the particle measuring device 100, the connectors 31 and 32 are provided so that the height position of the connector 32 is higher than the height position of the connector 31, respectively. Therefore, when the rotation of the pump 12 is started and the slurry 21 in the pipe C11a is not drawn downstream from the connector 32 in the pipe C11, the slurry 21 in the pipe C11a flows back into the circulation pipe C10 (discharge). Will be). As a result, even when the sample particles in the slurry 21 are precipitated in the tube C11a, the precipitated sample particles are discharged into the circulation tube C10 together with the discharge of the slurry 21, and the sample particles remain in the tube C11a. Can be suppressed.

[Step 3: Imaging / particle size distribution measurement and diluent discharge]
When the step 2 is completed, the rotation of the pump 3a is started, and the diluted solution 23 in the tank 2b is transferred into the flow cell 36 via the circulation pipe C1.

Then, the diluent 23 passing through the flow cell 36 is photographed by the camera 35. At this time, the lighting device 37 emits strobe light in synchronization with the shooting timing of the camera 35. The camera 35 repeats shooting at predetermined intervals (for example, several times per second) over a predetermined time (for example, 6 minutes).

The camera 35 transmits the captured image to the calculation unit 5. When the calculation unit 5 receives an image from the camera 35, the calculation unit 5 acquires particle measurement information such as the outer diameter, area, angle of protrusions on the contour, center of gravity, and perimeter of each particle in the captured image by image processing. And record. In order to obtain highly accurate particle size distribution information, it is preferable to continuously perform the measurement until about 4000 or more particle measurement information is acquired.

When the acquisition of the particle measurement information of the predetermined number of particles is completed, the rotation of the pump 3a is stopped. After that, the rotation of the pump 4a is started, and all the diluted liquids 23 in the tank 2b are discharged to the outside of the particle measuring device 100 via the circulation pipe C1, the flow cell 36, and the discharge pipe C2. When all the diluted solution 23 in the tank 2b is discharged, the rotation of the pump 4a is stopped.

[Step 4: Viewing particle size distribution results]
The particle size distribution measurement result obtained in step 3 is stored in the calculation unit 5. A user terminal such as a personal computer can communicate with the calculation unit 5 via a computer network such as a LAN, draw a graph using the particle size distribution measurement result, and calculate an aggregated value such as an average particle size. .. The calculation unit 5 may have a web server function. In this case, the user terminal can confirm the particle size distribution measurement result on the web browser. Further, the calculation unit 5 may be configured to automatically update and present the transition of the average particle size over a predetermined time (for example, several hours). This step may be performed at least in parallel with step 3 described above.

(3) Effects obtained by the present embodiment According to the present embodiment, one or more of the following effects can be obtained.

(A) By providing the connector 31 and the connector 32 so that the height position of the connector 32 is higher than the height position of the connector 31, the operation of the pump 12 causes the connector 32 to be higher than the connector 32 in the pipe C11. When the slurry 21 is no longer supplied to the downstream side, the slurry 21 in the pipe C11a is discharged into the circulation pipe C10. Therefore, even when the sample particles in the slurry 21 are settled in the tube C11a, the settled sample particles are discharged into the circulation tube C10 together with the discharge of the slurry 21, and the sample particles in the slurry 21 are discharged in the tube C11a. Sample particles are less likely to remain. As a result, the influence of the physical quantity such as the particle size distribution on the measurement result can be reduced. The present inventors should arrange the pipe C11a so that the height position of the connector 32 is higher than the height position of the connector 31 so that the arrangement angle of the pipe C11a is 45 °. It has been confirmed that the variation in the measurement result of the average particle size is smaller than that in the case of 0 °.

(B) The above-mentioned effect can be similarly obtained when metal-based particles having a particularly large particle size and a relatively large specific gravity, such as nickel (Ni) particles, are used as the sample particles. As described above, the present invention is particularly effective when metal-based particles having a relatively large specific gravity are used as sample particles.

(C) By setting the arrangement angle of the tube C11a within the range of 5 to 90 °, the influence on the measurement result of the physical quantity can be surely reduced.

(D) By supporting the connector 31 to the support member 40 described above, it is possible to easily adjust the height position of the connector 31.

<Other embodiments>
The embodiment of the present invention has been specifically described above. However, the present invention is not limited to the above-described embodiment, and various modifications can be made without departing from the gist thereof.

In the above-described embodiment, the case where the particle measuring device 100 has one transfer unit 7 has been described. However, the particle measuring device may have a plurality of transfer units 7 as shown in FIG. The particle measuring device 100A shown in FIG. 4 is the same as the above-described embodiment except that it has a plurality of transfer units 7. Therefore, in the following, the same components as those in the above-described embodiment are designated by the same reference numerals, and the description thereof will be omitted.

The particle measuring device 100A has two transfer units 7, that is, a first transfer unit 7f and a second transfer unit 7s. The particle measuring device 100A may have three or more transfer units 7. The particle measuring device 100A includes a tank 39 for accommodating the diluting liquid 22, a main body 1 (that is, a diluting unit 2, a measuring unit 3, and a discharging unit 4), and a calculation unit 5 includes a first transfer unit 7f and a second transfer unit. It is shared with 7s.

The first transfer unit 7f and the second transfer unit 7s have a tank 38, a circulation pipe C10, a pipe C11, a pipe C12, a connector 31, and a connector 32, respectively. In the first transfer unit 7f and the second transfer unit 7s, the connector 31 and the connector 32 are provided so that the height position of the connector 32 is higher than the height position of the connector 31, respectively. Thereby, the same effect as that of the above-described embodiment can be obtained.

Further, it is preferable to arrange the arrangement angle of the pipe C11a between the first transfer portion 7f and the second transfer portion 7s. As a result, the measurement conditions can be made uniform between the first transfer unit 7f and the second transfer unit 7s. The present inventors house the slurry 21 having the same sample particles in the respective tanks 38 of the first transfer unit 7f and the second transfer unit 7s, and when the average particle size of the sample particles is measured, the average particle size is measured. It has been confirmed that the measurement results of the above are substantially the same among the plurality of transfer units 7. By using the support member 40, the present inventors can easily align the arrangement angle of the pipe C11a between the first transfer portion 7f and the second transfer portion 7s.

Further, when the tank 39 and the diluting unit 2 are shared by the first transfer unit 7f and the second transfer unit 7s as in the present embodiment, the tank 39 and the tank 2b are the first transfer unit 7f and the second transfer unit 7s. It is preferable that the pipe C11 and the pipe C12 are provided at a position where the total length of the pipe C11 is as short as possible. For example, it is preferable that the tank 39 and the tank 2b are provided at substantially intermediate positions between the tank 38 of the first transfer unit 7f and the tank 38 of the second transfer unit 7s. As a result, it is possible to prevent the particle measuring device 100A from becoming large.

A plurality of tanks 39 and 2b may be provided for each transfer unit 7. However, from the viewpoint of reducing the size of the particle measuring device 100A, it is preferable that the tank 39 and the tank 2b are shared by a plurality of transfer units 7.

In the following, regarding the process of measuring the physical quantity of the sample particles in the slurry 21 using the particle measuring device 100A, after measuring the physical quantity of the slurry 21 transferred from the tank 38 of the first transfer unit 7f, the second transfer unit The case of measuring the physical quantity of the slurry 21 transferred from the tank 38 of 7s will be described as an example. In the following description, the same procedure as that of the above-described embodiment will be omitted.

[Step 1: Stirring of slurry]
First, the rotation of each of the pumps 10 of the first transfer unit 7f and the second transfer unit 7s is started. The rotation of each pump 10 of the first transfer unit 7f and the second transfer unit 7s is continuously performed at least until the end of step 3B. This is to maintain the circulation of the slurry 21 in each of the circulation pipes C10 of the first transfer section 7f and the second transfer section 7s, and to prevent the sample particles from settling and solidifying in each tank 38.

[Step 2A: First sampling]
After a predetermined time has elapsed from the start of rotation of the pump 10, the rotation of the pump 11 of the first transfer unit 7f is started with the rotation of the pump 12 of the first transfer unit 7f and the pumps 11 and 12 of the second transfer unit 7s stopped. Then, the slurry 21 in the tank 38 of the first transfer portion 7f is drawn from the inside of the circulation pipe C10 to the downstream side of the connector 32 in the pipe C11. After a predetermined time (for example, 1 to 6 seconds) has elapsed from the start of rotation of the pump 11, the rotation of the pump 12 of the first transfer unit 7f is started while the rotation of the pump 11 is maintained, and the diluting liquid 22 is drawn into the pipe C12. .. Then, the diluting liquid 23 in which the slurry 21 is diluted by the diluting liquid 22 is stored in the tank 2b. When the predetermined time elapses, the slurry concentration in the diluent 23 becomes a concentration suitable for measuring the particle size distribution, and the amount of the diluent 23 in the tank 2b reaches a desired amount, the pump 11 of the first transfer unit 7f , 12 rotation is stopped at the same time, and the transfer of the diluting liquid 22 to the tank 2b is stopped.

[Step 3A: Imaging / particle size distribution measurement and diluted solution discharge]
When step 2A is completed, the same steps as in step 3 described above are performed.

[Step 2B: Second sampling]
When step 3A is completed, the rotation of the pump 11 of the second transfer unit 7s is started with the rotation of the pumps 11 and 12 of the first transfer unit 7f and the pump 12 of the second transfer unit 7s stopped, and the circulation pipe C10 is started. The slurry 21 in the tank 38 of the second transfer portion 7s is drawn from the inside to the downstream side of the connector 32 in the pipe C11. After a predetermined time (for example, 1 to 6 seconds) has elapsed from the start of rotation of the pump 11, the rotation of the pump 12 of the second transfer unit 7s is started while the rotation of the pump 11 is maintained, and the diluting liquid 22 is drawn into the pipe C12. .. Then, the diluting liquid 23 in which the slurry 21 is diluted by the diluting liquid 22 is stored in the tank 2b. When the predetermined time elapses, the slurry concentration in the diluent 23 becomes a concentration suitable for measuring the particle size distribution, and the amount of the diluent 23 in the tank 2b reaches a desired amount, the pump 11 of the second transfer unit 7s , 12 rotation is stopped at the same time, and the transfer of the diluting liquid 22 to the tank 2b is stopped.

[Step 3B: Imaging / particle size distribution measurement and diluted solution discharge]
When step 2B is completed, the same steps as in step 3 described above are performed.

[Step 4: Viewing particle size distribution results]
The same steps as in step 4 described above are performed.

In the particle measuring device 100A, the transfer routes of the slurry 21 and the diluting liquid 22 transferred into the tank 2b can be switched by the pumps 11 and 7s of the transfer units 7f and 7s, respectively, without providing a valve for switching the transfer routes. This is done by controlling the rotation and rotation stop of the twelve. As a result, it is possible to suppress the complexity of the measurement procedure and reduce the cost of the device.

Further, in the present embodiment, the tank 2b, the circulation pipe C1, the flow cell 36, and the like may be washed after the step 3A and before the step 2B. As a result, the mixing of the previously measured slurry sample can be suppressed, and the physical quantity of the sample particles can be measured more accurately.

Further, in the present embodiment, the process of measuring the physical quantity of the sample particles in the slurry 21 may be performed in the order of step 1 → step 2B → step 3B → step 2A → step 3A → step 4. In this case, the above-mentioned washing may be performed after performing step 3B and before performing step 2A.

In the above-described embodiment, the cases where the pumps 11 and 12 are installed in the main body 1 have been described as an example, but the present invention is not limited thereto. For example, the pumps 11 and 12 may be installed outside the main body 1.

<Preferable Aspect of the Present Invention>
Hereinafter, preferred embodiments of the present invention will be described.

(Appendix 1)
According to one aspect of the invention
The first container to store the slurry and
A second container for the diluent and
A third container containing the diluted solution obtained by diluting the slurry with the diluted solution, and
It has a circulation tube for circulating the slurry in the first container outside the first container.
A first pipe that supplies at least the slurry into the third container is connected to the circulation pipe by using a first pipe connecting member that is a branch joint member.
On the downstream side of the first pipe from the first pipe connecting member, a second pipe that supplies the diluting liquid in the second container into the third container via the first pipe branches. It is connected using the second pipe connecting member, which is a joint member, and is connected.
The first pipe connecting member and the second pipe connecting member are each provided as a particle measuring device so that the height position of the second pipe connecting member is higher than the height position of the first pipe connecting member. Is provided.

(Appendix 2)
The particle measuring device of Appendix 1, preferably.
The first pipe connecting member and the second pipe connecting member have an arrangement angle of the first pipe located between the first pipe connecting member and the second pipe connecting member within a range of 5 to 90 °. Each is provided so as to be.

(Appendix 3)
The particle measuring device of Appendix 1 or 2, preferably.
It has a plurality of transfer portions including the first container, the circulation pipe, the first pipe, the second pipe, the first pipe connecting member, and the second pipe connecting member.

(Appendix 4)
The particle measuring device of Appendix 3, preferably.
The arrangement angle of the first pipe located between the first pipe connecting member and the second pipe connecting member is the same among the plurality of transfer portions.

(Appendix 5)
The particle measuring device according to any one of Supplementary note 1 to 4, preferably.
It has a support member including a first plate-shaped member to which the first pipe connecting member is mounted, and a second plate-shaped member mounted to the first plate-shaped member and having a supported surface.
The support member can adjust the height position of the first pipe connecting member with respect to the supported surface by sliding the positional relationship between the first plate-shaped member and the second plate-shaped member in the vertical direction. It is configured.

2b tank (third container)
7,7f, 7s Transfer section 21 Slurry 22 Diluting liquid 23 Diluting liquid 31 Connector (first pipe connecting member)
32 Connector (second pipe connecting member)
C10 circulation pipe C11 pipe (first pipe)
C12 pipe (second pipe)
38 tanks (first container)
39 tanks (second container)
100,100S particle measuring device

Claims (5)

The first container to store the slurry and
A second container for the diluent and
A third container containing the diluted solution obtained by diluting the slurry with the diluted solution, and
It has a circulation tube for circulating the slurry in the first container outside the first container.
A first pipe that supplies at least the slurry into the third container is connected to the circulation pipe by using a first pipe connecting member that is a branch joint member.
On the downstream side of the first pipe from the first pipe connecting member, a second pipe that supplies the diluting liquid in the second container into the third container via the first pipe branches. It is connected using the second pipe connecting member, which is a joint member, and is connected.
The first pipe connecting member and the second pipe connecting member are each provided as a particle measuring device so that the height position of the second pipe connecting member is higher than the height position of the first pipe connecting member. .. The first pipe connecting member and the second pipe connecting member have an arrangement angle of the first pipe located between the first pipe connecting member and the second pipe connecting member within a range of 5 to 90 °. The particle measuring device according to claim 1, which is provided for each of the above. 1. 2. The particle measuring device according to 2. The particle measuring device according to claim 3, wherein the arrangement angle of the first pipe located between the first pipe connecting member and the second pipe connecting member is the same among the plurality of transfer portions. It has a support member including a first plate-shaped member to which the first pipe connecting member is mounted, and a second plate-shaped member mounted to the first plate-shaped member and having a supported surface.
The support member can adjust the height position of the first pipe connecting member with respect to the supported surface by sliding the positional relationship between the first plate-shaped member and the second plate-shaped member in the vertical direction. The particle measuring device according to any one of claims 1 to 4, which is configured.

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