Particle size distribution measurement device, particle size distribution measurement method, and program for particle size distribution measurement device

Abstract

The present invention is a particle size distribution measurement device, wherein is provided a history data management part 33 that facilitates integrated recognition of various stored operations, states of devices, and instantaneous values of particle size measurement results, and that causes a history data storage part D1 to store an operation history indicating the history of operations performed on the particle size distribution measurement device 100 by an operator, a measurement result history indicating the history of particle size measurement results, or a device state history indicating the history of the state of the particle size distribution measurement device 100, in a format that can be displayed as a time-series graph.

Description

Particle size distribution measuring device, particle size distribution measuring method, and program for particle size distribution measuring device

[0001] The present invention relates to a particle size distribution measuring device, a program for the particle size distribution measuring device, and a particle size distribution measuring method.

[0002] In recent years, data integrity is sometimes required for particle size distribution measuring devices such as those disclosed in Patent Document 1, from the viewpoint of preventing falsification of measurement results and ensuring validity.

[0003] For this reason, particle size distribution measurement devices use audit trails to verify data integrity. These audit trails store events that occur in the particle size distribution measurement device, correlating them with the date, time, and user.

[0004] However, while the audit trail described above allows for confirmation of events that have occurred (such as operations or error occurrences), it does not allow for subsequent confirmation of the background or appropriateness of actions such as "I visually confirmed bubbles in the sample, so I extended the ultrasonic time by one minute."

[0005] Japanese Patent Application Laid-Open No. 2017-167081

[0006] The present invention has been made in view of the above-mentioned problems, and its main object is to make it easier to comprehensively recognize various stored operations, device states, and instantaneous values ​​of particle size measurement results in a particle size distribution measuring device.

[0007] That is, the particle size distribution measuring device according to the present invention is a particle size distribution measuring device that irradiates a particle group that is a measurement target with light, detects the secondary light generated thereby, and calculates the particle size distribution of the particle group based on the detection data, and is characterized by comprising a history data management unit that stores in a memory an operation history that indicates a history of operations performed on the particle size distribution measuring device by an operator, a measurement result history that indicates a history of particle size measurement results, or an apparatus status history that indicates a history of the status of the particle size distribution measuring device in a format that can be displayed as a time-series graph.

[0008] Such a particle size distribution measuring device stores the operation history and the measurement result history or the device status history in a format that can be displayed as a time series graph, and can display the operation history and the measurement result history or the device status history as a time series graph, thereby making it easier to recognize the various stored operations, device status, and instantaneous values ​​of particle size measurement results in an integrated manner in the particle size distribution measuring device.

[0009] In a specific embodiment, the particle size distribution measuring device of the present invention preferably further comprises a display control unit that displays a time series graph of the operation history and a time series graph of the measurement result history or a time series graph of the device status history on a display so that they can be compared. Note that history data including the operation history and the measurement result history or the device status history stored in the memory can be transmitted to an external information processing device and displayed on the display of the external information processing device.

[0010] It is desirable that the display control unit displays the time series graph of the operation history and the time series graph of the measurement result history or the time series graph of the device status history with the horizontal or vertical axis scale indicating time aligned. It is also desirable that the display control unit synchronizes and displays the time series graph of the operation history with the time series graph of the measurement result history or the time series graph of the device status history. This configuration makes it even easier to recognize the particle size measurement results or device status corresponding to the various stored operations. For example, by displaying the time series graph of the operation history and the time series graph of the measurement result history or the time series graph of the device status history one above the other when the horizontal axis is the time axis, or by displaying them one below the other when the vertical axis is the time axis, it is possible to recognize at a glance the correspondence between the various operations and the measurement results or device status corresponding to the operations.

[0011] It is desirable that the display control unit displays the time series graph of the operation history and the time series graph of the measurement result history or the time series graph of the device status history on the same graph. With this configuration, the time series graph of the operation history and the time series graph of the measurement result history or the time series graph of the device status history are displayed on the same graph, making it possible to recognize at a glance the correspondence between various operations and the measurement results or device status corresponding to those operations.

[0012] It is desirable that the display control unit sequentially updates and displays trend information including operations performed by the operator on the particle size distribution measurement device and particle size measurement results or the status of the particle size distribution measurement device in real time. With this configuration, the operator can view the trend information displayed in real time and determine whether preprocessing has been performed appropriately, whether measurement conditions are appropriate, etc.

[0013] The particle size distribution measuring device of the present invention may be a laser diffraction / scattering type. That is, the particle size distribution measuring device of the present invention preferably includes a cell that contains a sample in which a particle group to be measured is dispersed in a dispersion medium, a laser light source that irradiates the cell with laser light, a photodetector that detects diffracted / scattered light generated in the sample, and a particle size distribution calculation unit that calculates the particle size distribution of the particle group based on detection data obtained by the photodetector.

[0014] Examples of operations performed on the particle size distribution measuring device include introduction of a particle group, defoaming, optical axis adjustment, blank measurement, main measurement, abnormality detection, or change of device state, etc. Therefore, the operation history includes at least one of introduction of a particle group, defoaming of a sample, optical axis adjustment, blank measurement, main measurement, abnormality detection, or change of device state.

[0015] Examples of the state in the particle size distribution measuring device include circulation system parameters including the water level or circulation speed of the dispersion medium, ultrasonic parameters including the intensity or application time of ultrasonic waves, agitator parameters such as the intensity or operation time of the agitator, etc. Therefore, the device state history includes at least one of circulation system parameters including the water level or circulation speed of the dispersion medium, ultrasonic parameters including the intensity or application time of ultrasonic waves, or agitator parameters such as the intensity or operation time of the agitator.

[0016] Furthermore, a program for a particle size distribution measuring device according to the present invention is a program used in a particle size distribution measuring device that irradiates a particle group to be measured with light, detects the secondary light generated thereby, and calculates the particle size distribution of the particle group based on the detection data, and is characterized in that the program has a function as a history data management unit that stores in memory, in a format that can be displayed as a time-series graph, an operation history that indicates a history of operations performed on the particle size distribution measuring device by an operator, a measurement result history that indicates a history of particle size measurement results, or an apparatus status history that indicates a history of the status of the particle size distribution measuring device.

[0017] Furthermore, a particle size distribution measuring method according to the present invention is a particle size distribution measuring method that irradiates a particle group to be measured with light, detects secondary light generated thereby, and calculates the particle size distribution of the particle group based on the detection data, and is characterized in that an operation history indicating a history of operations performed on the particle size distribution measuring device by an operator, a measurement result history indicating a history of particle size measurement results, or an apparatus status history indicating a history of the status of the particle size distribution measuring device are saved in a format that can be displayed as a time-series graph.

[0018] According to the present invention as described above, it is possible to easily recognize the various operations, the state of the device, and the instantaneous values ​​of the particle size measurement results that are stored in the particle size distribution measuring device in an integrated manner.

[0019] 1 is an overall schematic diagram of a particle size distribution measuring device according to one embodiment of the present invention; FIG. 2 is a functional configuration diagram of a calculation device according to the embodiment; FIG. 3 is a time series graph of operation history and measurement result history according to the embodiment; FIG. 4 is a time series graph of operation history and measurement result history according to the embodiment; FIG. 5 is a time series graph of operation history and device status history according to the embodiment; FIG. 6 is a schematic diagram showing a real-time display screen according to the embodiment; FIG. 7 is a schematic diagram showing a real-time display screen according to a modified embodiment; FIG. 8 is a schematic diagram showing a display mode of a time series graph of operation history and a time series graph of measurement result history according to a modified embodiment.

[0020] <One embodiment of the present invention> Hereinafter, one embodiment of a particle size distribution measuring device according to the present invention will be described with reference to the drawings. Note that in all of the drawings shown below, parts are appropriately omitted or exaggerated for ease of understanding. Identical components are assigned the same reference numerals, and descriptions thereof will be omitted as appropriate.

[0021] <Basic Configuration of Particle Size Distribution Measuring Apparatus 100> The particle size distribution measuring apparatus 100 of this embodiment utilizes the fact that the light intensity distribution corresponding to the spread angle of diffracted / scattered light generated when particles are irradiated with light is determined by the particle size according to MIE scattering theory, and measures the particle size distribution by detecting the diffracted / scattered light.

[0022] Specifically, as shown in FIG. 1, the particle size distribution measuring device 100 includes a device main body 2 that performs various processes related to actual measurement, and an arithmetic control unit 3 that controls each process in the device main body 2 and calculates the particle size distribution.

[0023] As shown in FIG. 1 , the device main body 2 includes a cell 21 that contains a sample in which a particle group to be measured is dispersed in a dispersion medium, a laser light source 22 that irradiates laser light onto the cell 21, and a plurality of photodetectors 23 that detect the intensity distribution of transmitted light that has passed through the cell 21 and diffracted / scattered light that has been diffracted and / or scattered by the cell 21.

[0024] The cell 21 is transparent and contains a sample in which a particle group is dispersed in a dispersion medium such as water. The cell 21 in this embodiment is a circulating wet type and is provided on the sample circulation flow path L1.

[0025] On this sample circulation flow path L1, there are provided a mixing bath 10 having a particle group inlet 10a for mixing the dispersion medium and the particle groups, a stirrer 11 for stirring the dispersion medium and the particle groups in the mixing bath 10, a circulation pump 12 for circulating the sample, an ultrasonic oscillator 13 for breaking down agglomerations of the particle groups and dispersing them, etc. In addition, a refilling flow path L2 having a refilling pump 14 for refilling the dispersion medium to the sample circulation flow path L1 is connected, and a discharge flow path L3 for discharging the sample via a switching valve 15 is also connected.

[0026] The laser light source 22 emits coherent light, and is a semiconductor laser in this example. The laser light source 22 is capable of adjusting the optical axis and the intensity of the light it emits.

[0027] The photodetectors 23 are arranged discretely on the optical axis of the laser light source 22 and within a predetermined angular range from the optical axis, for example, on the same circumference, with the cell 21 as the center, and detect the intensity at each angle of transmitted light traveling straight on the optical axis and scattered light scattered at various angles by the sample. Each photodetector 23 outputs a light intensity signal corresponding to the intensity of the incident light.

[0028] Structurally, the calculation control unit 3 is a dedicated or general-purpose computer equipped with a CPU, memory, A / D converter, input / output interface, communication interface, etc. This computer causes the CPU and peripheral devices to cooperate in accordance with a predetermined program stored in a predetermined area of ​​the memory, thereby fulfilling functions such as an apparatus main body control unit 31 that controls each part of the apparatus main body 2 and a particle size distribution calculation unit 32 that calculates a particle size distribution based on light intensity signals output from each photodetector 23, as shown in Fig. 2 .

[0029] The device main body control unit 31 controls each part of the device main body 2 to measure particle size distribution. Specifically, the device main body control unit 31 monitors and controls, for example, the laser light source 22, the photodetector 23, the agitator 11, the circulation pump 12, and the ultrasonic oscillator 13.

[0030] The particle size distribution calculation unit 32 receives the light intensity signals output from each photodetector 23 and calculates particle size distribution data representing the particle size distribution from those values ​​according to an algorithm based on MIE scattering theory. The particle size distribution calculation unit 32 can also calculate a representative particle size from the calculated particle size distribution data. The representative particle size refers to a particle size corresponding to a predetermined number of passing fraction accumulation degrees. More specifically, the representative particle size refers to a particle size corresponding to a passing fraction accumulation degree of 10% (hereinafter also referred to as D10 or representative small particle size), a particle size corresponding to a passing fraction accumulation degree of 50% (hereinafter also referred to as median diameter, D50, or representative central particle size), or a particle size corresponding to a passing fraction accumulation degree of 90% (hereinafter also referred to as D90 or representative large particle size).

[0031] Thus, the calculation and control unit 3 of this embodiment is configured to allow a user to recognize particle size measurement results or device states corresponding to various past operations in the particle size distribution measuring device 100. Specifically, the calculation and control unit 3 includes a history data management unit 33 that stores various histories related to the particle size distribution measuring device 100 in a history data storage unit D1 made of memory.

[0032] The history data management unit 33 stores in the history data storage unit D1 an operation history indicating the history of operations performed by the operator on the particle size distribution measuring device 100, a measurement result history indicating the history of particle size measurement results, and an apparatus state history indicating the history of the state of the particle size distribution measuring device 100 in a format that can be displayed as a time series graph.

[0033] Here, the operation history includes at least one of the following: introduction of a particle group into the particle group introduction port 10a, debubbling of the sample in the sample circulation flow path L1, adjustment of the optical axis of the laser light source 22, blank measurement performed with only the dispersion medium placed in the cell 21, main measurement performed with the sample placed in the cell 21, detection of an abnormality such as a communication error, or change of the device state described below.

[0034] The device state also includes at least one of circulation parameters in the sample circulation flow path L1, ultrasonic parameters in the ultrasonic oscillator 13, or stirring parameters in the stirrer 11. The circulation parameters include the water level of the dispersion medium in the mixing bath 10 or the circulation speed of the sample (circulation pump speed). The ultrasonic parameters include the operating time of the ultrasonic oscillator 13 (ultrasonic wave application time), ultrasonic intensity, or whether the ultrasonic oscillator 13 is operating during measurement. The stirring parameters include the stirring speed (stirring intensity) or the operating time of the stirrer 11.

[0035] Specifically, the history data management unit 33 stores the content of each operation in association with the time at which each operation was performed, stores the particle diameter measurement results in association with the measurement time corresponding to each measurement result, and stores each apparatus state in association with the time corresponding to each apparatus state, thereby storing each of these histories in the history data storage unit D1 in a format that can be displayed as a time-series graph.

[0036] Furthermore, the calculation control unit 3 further includes a display control unit 34 that displays a time series graph of the operation history and a time series graph of the measurement result history or a time series graph of the device status history on a display so that they can be compared based on each history data stored in the history data storage unit D1.

[0037] The display control unit 34 displays the time series graph of the operation history and the time series graph of the measurement result history or the time series graph of the device status history with the horizontal or vertical axis scale indicating time aligned. Furthermore, the display control unit 34 displays the time series graph of the operation history and the time series graph of the measurement result history or the time series graph of the device status history in synchronization with each other.

[0038] The display control unit 34 of this embodiment displays a time series graph of the operation history and a time series graph of the measurement result history on the same graph, as shown in Figures 3 and 4, or displays a time series graph of the operation history and a time series graph of the device status history on the same graph, as shown in Figure 5. In other words, the display control unit 34 displays the time series graph of the operation history and the time series graph of the measurement result history in a superimposed manner, and displays the time series graph of the operation history and the time series graph of the device status history in a superimposed manner.

[0039] Specifically, the display control unit 34 displays the measurement results and performs an operation specific display indicating that each operation was performed at the time when each operation was performed on the same graph with the horizontal axis as the time axis, as shown in Figures 3 and 4. Furthermore, the display control unit 34 displays the device status and performs an operation specific display indicating that each operation was performed at the time when each operation was performed on the same graph with the horizontal axis as the time axis, as shown in Figure 5.

[0040] Here, the operation specification display corresponds to, for example, the start and / or end of an operation, and is, for example, a linear or band-like display extending along the vertical axis. Note that other display modes are also acceptable as long as the operation performed can be recognized on the graph. Then, by selecting the operation specification display by pointing a pointing device at it, the specific operation content (e.g., "Ultrasound ON" in FIG. 3 or "Measurement" in FIG. 4) corresponding to the operation specification display is displayed. Furthermore, the representative particle size (e.g., D10, D50, D90) and transmittance (e.g., T%(R), T%(B)) determined from the particle size distribution data are displayed as measurement results.

[0041] Furthermore, as shown in Fig. 5, for example, the liquid level of the dispersion medium, the circulation speed, the ultrasonic intensity, and the agitator operation are displayed as the equipment status. In addition, by selecting the equipment status at a specific time on the graph showing the equipment status by pointing the pointing device at the specific time, the specific details of the equipment status at that specific time (for example, "Ultrasound Intensity 7 (Ultrasound 7)" in Fig. 5) are displayed.

[0042] Furthermore, the display control unit 34 of this embodiment, in addition to the function of displaying a time series graph of each history, can also display a trend information screen W1, which successively updates and displays current trend information in real time, as shown in FIG. 6.

[0043] This trend information screen W1 includes operations performed by the operator on the particle size distribution measurement device 100, as well as particle size measurement results or the status of the particle size distribution measurement device 100. Specifically, the trend information screen W1 includes a display area A1 for the device status, a display area A2 for displaying a time series graph of the measurement results (e.g., representative particle size) and operation details, a display area A3 for displaying the transmittance, a display area A4 for displaying the light intensity signals of each photodetector, and a display area A5 for displaying the particle size distribution. Using the various information displayed on this trend information screen W1, the operator can perform operations such as removing bubbles from the sample in the sample circulation flow path L1, adjusting the optical axis of the laser light source 22, performing a blank measurement with only the dispersion medium in the cell 21, performing a main measurement with the sample in the cell 21, or changing the device status. When each operation is performed, an operation identification indicator (thick dotted line in FIG. 6 ) identifying the operation is displayed on the time series graph in the display area A2.

[0044] Effect of the Present Embodiment The particle size distribution measuring device 100 of the present embodiment configured as described above stores the operation history and the measurement result history or the device status history in a format that can be displayed as a time series graph, and therefore the operation history and the measurement result history or the device status history can be displayed as a time series graph. As a result, the particle size distribution measuring device makes it easy to recognize the various stored operations, the device status, and the instantaneous values ​​of the particle size measurement results in an integrated manner.

[0045] <Other Embodiments> For example, a configuration may be provided with an imaging camera 16 that images the sample circulating through the sample circulation flow path L1. Images captured by this imaging camera 16 can be displayed in the image display area A6 of the trend information screen W1, as shown in Fig. 7. This makes it possible to confirm the dispersion state of particle groups in the sample. The trend information screen W1 shown in Fig. 7 also displays an operation screen area A7 for operating the device main body 2. Various settings for the device main body 2 can be made using this operation screen area A7.

[0046] The present invention may also be applied to a particle size distribution measurement device using nanoparticle tracking analysis (NTA). NTA is a technique in which, for example, scattered light from particles in a dispersion medium irradiated with laser light is captured by a camera to obtain the behavior of each particle, such as Brownian motion, and calculate the particle state from that behavior. In this case, the particle size distribution measurement device measures the particle size distribution of a group of particles contained in a cell by capturing an image of the cell irradiated with laser light.

[0047] The present invention may also be applied to a so-called dynamic light scattering particle size distribution measuring device that detects scattered light generated by irradiating a measurement object with light as secondary light and calculates a particle size distribution based on fluctuations in the light intensity of the scattered light.

[0048] Furthermore, the present invention may be applied to a so-called natural / centrifugal sedimentation type particle size distribution measuring device that irradiates a measurement target with light, detects the transmitted light obtained as secondary light, and calculates a particle size distribution based on changes in the amount of transmitted light.

[0049] As shown in Fig. 8, the display control unit 34 may display the time series graph of the operation history and the time series graph of the measurement result history on separate time series graphs, and may display the time series graph of the operation history and the time series graph of the device status history on separate time series graphs. In this case, these time series graphs may be displayed simultaneously on the same screen, or may be displayed by switching between them on the screen. Even in these cases, it is desirable for the display control unit 34 to display the time axis scales of each time series graph in the same order.

[0050] In addition, various modifications and combinations of the embodiments may be made as long as they do not go against the spirit of the present invention.

[0051] According to the present invention, in a particle size distribution measuring device, it is possible to easily recognize various stored operations, device states, and instantaneous values ​​of particle size measurement results in an integrated manner.

[0052] REFERENCE SIGNS LIST 100: Particle size distribution measuring device 21: Cell 22: Laser light source 23: Photodetector 32: Particle size distribution calculation unit 33: History data management unit D1: History data storage unit 34: Display control unit

Claims

1. A particle size distribution measuring device that irradiates a particle group to be measured with light, detects the secondary light generated by the light, and calculates the particle size distribution of the particle group based on the detection data, comprising a history data management unit that stores in memory an operation history indicating a history of operations performed by an operator on the particle size distribution measuring device, a measurement result history indicating a history of particle size measurement results, or an device status history indicating a history of the status of the particle size distribution measuring device in a format that can be displayed as a time series graph.

2. The particle size distribution measuring device according to claim 1, further comprising a display control unit that displays a time series graph of the operation history and a time series graph of the measurement result history or a time series graph of the device status history on a display so that they can be compared.

3. The particle size distribution measuring device according to claim 2, wherein the display control unit displays a time series graph of the operation history and a time series graph of the measurement result history or a time series graph of the device status history with the horizontal or vertical axis scale indicating time aligned.

4. A particle size distribution measuring device as described in claim 2 or 3, wherein the display control unit displays a time series graph of the operation history and a time series graph of the measurement result history or a time series graph of the device status history on the same graph.

5. A particle size distribution measuring device as described in any one of claims 2 to 4, wherein the display control unit sequentially updates and displays trend information including operations performed by the operator on the particle size distribution measuring device and particle size measurement results or the status of the particle size distribution measuring device in real time.

6. The particle size distribution measuring device according to any one of claims 1 to 5, comprising: a cell for accommodating a sample in which a particle group to be measured is dispersed in a dispersion medium; a laser light source for irradiating laser light onto said cell; a photodetector for detecting diffracted / scattered light generated in said sample; and a particle size distribution calculation unit for calculating a particle size distribution of said particle group based on detection data obtained by said photodetector.

7. A program used in a particle size distribution measuring device that irradiates a particle group to be measured with light, detects the secondary light generated by the light, and calculates the particle size distribution of the particle group based on the detection data, the program providing a computer with a function as a history data management unit that stores in memory an operation history indicating a history of operations performed by an operator on the particle size distribution measuring device, a measurement result history indicating a history of particle size measurement results, or an apparatus status history indicating a history of the status of the particle size distribution measuring device in a format that can be displayed as a time series graph.

8. A particle size distribution measuring method for irradiating a particle group to be measured with light, detecting secondary light resulting from the irradiation, and calculating a particle size distribution of the particle group based on the detection data, wherein an operation history showing a history of operations performed by an operator on the particle size distribution measuring device, a measurement result history showing a history of particle size measurement results, or a device status history showing a history of the status of the particle size distribution measuring device are saved in a format that can be displayed as a time series graph.

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