Apparatus and method for measuring particle size distribution, and program for particle size distribution measuring apparatus

Patent metadata

Field	Value
Publication number	US-11047786-B2
Application number	US-201716461511-A
Country	US
Kind code	B2
Filing date	Oct 30, 2017
Priority date	Nov 16, 2016
Publication date	Jun 29, 2021
Grant date	Jun 29, 2021

Abstract

The particle size distribution measuring apparatus includes a centrifugal sedimentation measuring mechanism and a dynamic light scattering measuring mechanism. The centrifugal sedimentation measuring mechanism causes particles to settle out by rotating a measurement cell accommodating particles dispersed in a dispersion medium and detects transmitted light by irradiating light to the measurement cell to measure a first particle size distribution on a basis of a change of transmitted light intensity of the transmitted light. The dynamic light scattering measuring mechanism detects scattered light occurred upon irradiation of light to particles so as to measure a second particle size distribution based on a change of scattered light intensity of the scattered light occurred due to Brownian motion of particles. After the centrifugal sedimentation measuring mechanism detects the transmitted light, the dynamic light scattering measuring mechanism measures the second particle size distribution by irradiating light onto the measurement cell.

First claim

What is claimed is:

1. A particle size distribution measuring apparatus comprising:
a centrifugal sedimentation type measuring mechanism causing particles to settle out by rotating a measurement cell accommodating particles dispersed in a dispersion medium and measuring a time during which a particle sinks down a predetermined distance by irradiating light to the particles and detecting transmitted light, wherein a first particle size distribution of the particles is measured on a basis of a change of transmitted light intensity of the transmitted light; and
a dynamic light scattering type measuring mechanism detecting scattered light occurred upon irradiation of light to particles to measure a second particle size distribution on a basis of a change of scattered light intensity of the scattered light occurred due to Brownian motion of particles, wherein
after the centrifugal sedimentation type measuring mechanism detects the transmitted light, the dynamic light scattering type measuring mechanism measures the second particle size distribution by irradiating light onto the measurement cell.

2. The particle size distribution measuring apparatus according to claim 1 , further comprising:
a controller configured to control the centrifugal sedimentation type measuring mechanism and the dynamic light scattering type measuring mechanism, wherein
the controller comprises:
a first measurement end determination section determining whether measurement of the first particle size distribution is terminated, on a basis of the transmitted light intensity obtainable by the centrifugal sedimentation type measuring mechanism; and
a second measurement start section transmitting, to the dynamic light scattering type measuring mechanism, a second measurement start signal for starting measurement of the second particle size distribution after the first measurement end determination section makes a determination that the measurement of the first particle size distribution is terminated.

3. The particle size distribution measuring apparatus according to claim 2 , wherein
the centrifugal sedimentation type measuring mechanism comprises a rotation mechanism configured to rotate the measurement cell around a rotation axis, and
the controller causes a rotation of the measurement cell by transmitting a control signal to the rotation mechanism, and
the dynamic light scattering type measuring mechanism measures the second particle size distribution during the rotation of the measurement cell.

4. The particle size distribution measuring apparatus according to claim 3 , wherein
the rotation mechanism is configured to rotate a reference cell accommodating the dispersion medium, and
the dynamic light scattering type measuring mechanism detects background light occurred upon irradiation of light onto the reference cell, and calculates the second particle size distribution on a basis of a change of background light intensity of the background light and a change of the scattered light intensity.

5. The particle size distribution measuring apparatus according to claim 3 , wherein a rotation speed of the measurement cell during measurement of the second particle size distribution is lower than a rotation speed of the measurement cell during measurement of the first particle size distribution.

6. The particle size distribution measuring apparatus according to claim 2 , wherein the first measurement end determination section makes a determination that the measurement of the first particle size distribution is terminated based on the transmitted light intensity or absorbance obtainable on a basis of the transmitted light intensity.

7. The particle size distribution measuring apparatus according to claim 1 , wherein
each of the first particle size distribution and the second particle size distribution is indicated on a graph whose one axis is particle size and whose other axis is a ratio of particles for each particle size relative to a total of particles, and
the particle size distribution measuring apparatus further comprises a distribution composition section to create a composed particle distribution indicated on an identical graph by composing the first particle size distribution and the second particle size distribution.

8. The particle size distribution measuring apparatus according to claim 7 , further comprising:
a particle concentration calculation section configured to calculate a concentration of particles having a particle size indicated on the first particle size distribution on a basis of the transmitted light intensity obtainable by the centrifugal sedimentation type measuring mechanism; and
a distribution conversion section configured to convert, on a basis of the concentration calculated by the particle concentration calculation section, a composed particle size distribution composed by the distribution composition section, from a distribution relatively indicating a number of particles for each particle size to a distribution absolutely indicating the number of particles for the each particle size.

9. The particle size distribution measuring apparatus according to claim 1 , wherein the measurement cell accommodates a plurality of dispersion mediums which are stacked one upon another along a sedimentation direction and have densities different from one another.

10. The particle size distribution measuring apparatus according to claim 1 , wherein the centrifugal sedimentation type measuring mechanism comprises a rotation mechanism with a rotating disk having a holder that receives the measurement cell, and both the first particle size distribution and the second particle size distribution are measured from the measurement cell received in the holder of the rotating disk.

11. A particle size distribution measuring method comprising using:
a centrifugal sedimentation type measuring mechanism designed to cause particles to settle out by rotating a measurement cell accommodating particles dispersed in a dispersion medium and measure a time during which a particle sinks down a predetermined distance by irradiating light to the particles and detecting transmitted light, wherein a first particle size distribution of the particles is measured on a basis of a change of transmitted light intensity of the transmitted light; and
a dynamic light scattering type measuring mechanism detecting scattered light occurred upon irradiation of light to particles to measure a second particle size distribution on a basis of a change of scattered light intensity of the scattered light occurred due to Brownian motion of particles, wherein
the second particle size distribution is measured by detecting the transmitted light with use of the centrifugal sedimentation type measuring mechanism, followed by irradiating light onto the measurement cell with use of the dynamic light scattering type measuring mechanism.

12. A non-transitory program medium storing a program applied to a particle size distribution measuring apparatus, the apparatus comprising:
a centrifugal sedimentation type measuring mechanism causing particles to settle out by rotating a measurement cell accommodating particles dispersed in a dispersion medium and measuring a time during which a particle sinks down a predetermined distance by irradiating light to the particles and detecting transmitted light, wherein a first particle size distribution of the particles is measured on a basis of a change of transmitted light intensity of the transmitted light; and
a dynamic light scattering type measuring mechanism detecting scattered light occurred upon irradiation of light to particles to measure a second particle size distribution on a basis of a change of

Assignees

• Horiba Ltd

Inventors

• Yamaguchi Tetsuji

Classifications

• G01N15/0211 Primary

  Investigating a scatter or diffraction pattern · CPC title

• G01N2015/045

  by optical analysis · CPC title

• G01N2015/0053

  in liquids, e.g. trouble · CPC title

• G01N15/042

  by centrifuging and investigating centrifugates (centrifuges per se B04B) · CPC title

• G01N15/0255

  with mechanical, e.g. inertial, classification, and investigation of sorted collections (with centrifuges G01N15/042) · CPC title