WO2021221044A1 - 測定セル及び当該測定セルを用いた遠心沈降式の粒径分布測定装置 - Google Patents

測定セル及び当該測定セルを用いた遠心沈降式の粒径分布測定装置 Download PDF

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Publication number
WO2021221044A1
WO2021221044A1 PCT/JP2021/016741 JP2021016741W WO2021221044A1 WO 2021221044 A1 WO2021221044 A1 WO 2021221044A1 JP 2021016741 W JP2021016741 W JP 2021016741W WO 2021221044 A1 WO2021221044 A1 WO 2021221044A1
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WO
WIPO (PCT)
Prior art keywords
cell
flow path
measurement
sample
measurement cell
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2021/016741
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English (en)
French (fr)
Japanese (ja)
Inventor
哲司 山口
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Horiba Ltd
Original Assignee
Horiba Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Horiba Ltd filed Critical Horiba Ltd
Priority to JP2022518076A priority Critical patent/JP7601861B2/ja
Priority to US17/997,067 priority patent/US12313645B2/en
Priority to EP21795306.6A priority patent/EP4129488A4/en
Publication of WO2021221044A1 publication Critical patent/WO2021221044A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02Investigating particle size or size distribution
    • G01N15/0205Investigating particle size or size distribution by optical means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • G01N9/30Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by using centrifugal effects
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B1/00Centrifuges with rotary bowls provided with solid jackets for separating predominantly liquid mixtures with or without solid particles
    • B04B1/04Centrifuges with rotary bowls provided with solid jackets for separating predominantly liquid mixtures with or without solid particles with inserted separating walls
    • B04B1/08Centrifuges with rotary bowls provided with solid jackets for separating predominantly liquid mixtures with or without solid particles with inserted separating walls of conical shape
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/04Details of the conveyor system
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1009Characterised by arrangements for controlling the aspiration or dispense of liquids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/04Investigating sedimentation of particle suspensions
    • G01N15/042Investigating sedimentation of particle suspensions by centrifuging and investigating centrifugates
    • G01N2015/045Investigating sedimentation of particle suspensions by centrifuging and investigating centrifugates by optical analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/04Details of the conveyor system
    • G01N2035/0401Sample carriers, cuvettes or reaction vessels
    • G01N2035/0403Sample carriers with closing or sealing means
    • G01N2035/0405Sample carriers with closing or sealing means manipulating closing or opening means, e.g. stoppers, screw caps, lids or covers

Definitions

  • the present invention has been made to solve the above problems, and its main object is to improve the measurement accuracy in the particle size distribution measuring device that measures the particle size distribution by the line start method.
  • the measurement cell according to the present invention is a measurement cell used in the line start method of a centrifugal sedimentation type particle size distribution measuring device, and is a solution in which an opening is formed at one end and a density gradient is formed. It is provided with a cell body that houses the solution and a cell cap that closes the opening of the cell body and has an internal flow path that holds the sample liquid inside. It is characterized in that it is introduced into the density gradient solution from the flow path.
  • the internal flow path further includes an introduction flow path portion that communicates the sample introduction port and the liquid reservoir portion, and the introduction flow path portion is the measurement cell. It is desirable that the main flow path portion is provided along the direction of the rotation axis and is provided along the direction of the centrifugal force applied to the measurement cell. Here, since the main flow path portion is provided along the direction of the centrifugal force, the sample liquid can be made to flow quickly through the main flow path portion.
  • the liquid reservoir has a conical shape or a partial conical shape that tapers toward the bottom.
  • a hole may be drilled in the cell cap using a drill.
  • the surface tension acting near the sample outlet may hinder the spread (dispersion) of the sample liquid introduced into the density gradient solution.
  • the measurement cell 2 is, for example, a hollow rectangular parallelepiped cell having a substantially rectangular parallelepiped shape.
  • the measurement cell 2 contains a density gradient solution WDGS, which is a solution on which a density gradient is formed.
  • This density gradient solution WDGS is formed by using, for example, a plurality of sucrose solutions having different concentrations, and is housed in a multi-layered manner so that the density gradually increases toward the bottom side of the measurement cell 2. .
  • the reference cell 6 is also provided, and the reference cell 6 contains water.
  • the cell rotation mechanism 3 rotates the measurement cell 2 so that a centrifugal force is applied from the smaller density gradient to the larger density gradient.
  • the cell holder 31 has, for example, a disk shape, and the measurement cell 2 and the reference cell 6 are attached so as to sandwich the center of rotation thereof.
  • the measurement cell 2 is attached so that the direction of the density gradient is along the radial direction of the cell holder 31.
  • the cell holding body 31 is formed with a mounting recess 31a corresponding to the cell shape, and is mounted by fitting the cells 2 and 6 into the mounting recess 31a.
  • a guide mechanism (not shown) is provided between the measurement cell 2 and the reference cell 6 and the mounting recess 31a.
  • the guide mechanism is composed of a guide rail provided in one of the mounting recesses 31a or the cells 2 and 6, and a guide groove provided in the other.
  • the cell cap 22 is made of resin, for example, and as shown in FIGS. 3, 4 and 5, the cell cap 22 is inserted into the opening 21H of the cell body 21 to close the opening 21H.
  • the cell cap 22 has an insertion portion 22a inserted into the opening 21H of the cell main body 21 and a rear end portion 22b located outside the cell main body 21.
  • the sample introduction port 2A may be closed by the lid 23.
  • the lid 23 By closing the sample inlet 2A by the lid 23, it prevents the evaporation of the sample liquid W SS, that it can accumulate the air density gradient solution W DGS leaks in internal channel R side internal channel R Can be prevented.
  • the internal flow path R formed in the cell cap 22 holds the sample liquid W SS
  • internal flow sample liquid W SS is by centrifugal force is applied Since it is introduced into the density gradient solution WDGS from the path R, the timing at which centrifugal force is applied to the measurement cell 2 or the timing at which the measurement cell 2 is rotated at a predetermined rotation speed can be set as the measurement start timing of the line start method. It is possible to improve the measurement accuracy.
  • sample liquid W SS since the cell cap 22 is made to hold the sample liquid W SS, it is possible to reduce the distance to the sample liquid W SS and density gradient solution W DGS, sample liquid W SS reaches a density gradient solution W DGS The variation in time until is also small, and this also improves the measurement accuracy. Furthermore, since by holding the sample liquid W SS to the measurement cell 2 which is detachably attached to the apparatus main body, the introduction mechanism for introducing a sample liquid W SS from outside the measuring cell 2 in rotation It can be made unnecessary.
  • the main flow path portion R2 is connected to the upper part of the liquid reservoir portion R1, and the liquid reservoir portion R1 has an inclined surface R1x having an upward slope toward the main flow path portion R2 on the side to which the main flow path portion R2 is connected. Because they have, securely holds the sample liquid W SS to the liquid reservoir portion R1 in the pre-rotation of the measuring cell 2, it is possible to easily flow the sample liquid W SS from the liquid reservoir portion R1 in the main flow channel portion R2 during rotation.
  • the particle size distribution is measured by the line start method, but it can be configured so that not only the line start method but also the particle size distribution measurement by the uniform sedimentation method can be performed.
  • the measurement cell 2 contains a sample dispersion liquid in which particles are dispersed in the medium.
  • the measurement start timing is the rotation start timing of the measurement cell containing the sample dispersion liquid.
  • the measurement cell has a storage space for accommodating the dispersion medium and an internal flow path that communicates with the accommodation space and holds the sample liquid inside, and the sample liquid is inside by applying centrifugal force. It is introduced into the dispersion medium from the flow path.
  • the measurement cell has an opening formed at one end, and a cell cap in which a cell body for accommodating the dispersion medium and an internal flow path for holding the sample liquid are formed while closing the opening of the cell body. It is conceivable that the sample liquid is introduced into the dispersion medium from the internal flow path by applying centrifugal force.
  • the cell body and the cell cap can be made in the same manner as in the above-described embodiment.
  • the internal flow path communicating with the accommodation space holds the sample liquid, and the sample liquid is introduced into the dispersion medium from the internal flow path by applying centrifugal force, so that the sample liquid and the dispersion medium can be reached.
  • the distance can be reduced, and the variation in the time required for the sample solution to reach the dispersion medium can be reduced, which also improves the measurement accuracy.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Optical Measuring Cells (AREA)
PCT/JP2021/016741 2020-04-28 2021-04-27 測定セル及び当該測定セルを用いた遠心沈降式の粒径分布測定装置 Ceased WO2021221044A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2022518076A JP7601861B2 (ja) 2020-04-28 2021-04-27 測定セル及び当該測定セルを用いた遠心沈降式の粒径分布測定装置
US17/997,067 US12313645B2 (en) 2020-04-28 2021-04-27 Measurement cell and centrifugal sedimentation-type particle-size distribution measuring device using said measurement cell
EP21795306.6A EP4129488A4 (en) 2020-04-28 2021-04-27 MEASURING CELL AND CENTRIFUGAL SEDIMENTATION TYPE PARTICLE SIZE DISTRIBUTION MEASURING DEVICE USING SAID MEASURING CELL

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2020079762 2020-04-28
JP2020-079762 2020-04-28

Publications (1)

Publication Number Publication Date
WO2021221044A1 true WO2021221044A1 (ja) 2021-11-04

Family

ID=78331961

Family Applications (1)

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PCT/JP2021/016741 Ceased WO2021221044A1 (ja) 2020-04-28 2021-04-27 測定セル及び当該測定セルを用いた遠心沈降式の粒径分布測定装置

Country Status (4)

Country Link
US (1) US12313645B2 (https=)
EP (1) EP4129488A4 (https=)
JP (1) JP7601861B2 (https=)
WO (1) WO2021221044A1 (https=)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4154793A (en) * 1977-08-18 1979-05-15 Jean Guigan Device for conditioning a sample of liquid for analyzing
US4226531A (en) * 1977-08-29 1980-10-07 Instrumentation Laboratory Inc. Disposable multi-cuvette rotor
JPS62111645U (https=) * 1985-12-31 1987-07-16
JPS62115140U (https=) * 1985-12-03 1987-07-22
JP2003083990A (ja) * 2001-05-30 2003-03-19 Holger Behnk 体液を分析するための装置及び方法
JP2005043158A (ja) * 2003-07-25 2005-02-17 Wyatt Technol Corp 改良された円盤型遠心分離機および分析用超遠心分離機

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US3675846A (en) * 1970-06-15 1972-07-11 Bio Consultants Inc Continuous flow centrifuge head construction
SE8006732L (sv) * 1980-09-26 1982-03-27 Alfa Laval Ab Anordning for att overvaka separerat sediment, som kastas ut genom munstycken hos en centrifugalseparator
JPS61194329A (ja) * 1985-02-23 1986-08-28 Horiba Ltd 遠心沈降式粒度分布測定用試料セル
JPH065610Y2 (ja) * 1986-02-12 1994-02-09 株式会社島津製作所 遠心沈降式粒度分布測定装置
US5786898A (en) * 1996-08-23 1998-07-28 Fitzpatrick; Stephen T. Structure and method for centrifugal sedimentation particle size analysis of particles of lower density than their suspension medium
EP1062044A2 (en) 1998-03-10 2000-12-27 Large Scale Proteomics Corporation Detection and characterization of microorganisms
AU2008314981A1 (en) * 2007-10-24 2009-04-30 Jms Co., Ltd. Separation container, attachment and separation method
ES2602500T3 (es) * 2011-11-25 2017-02-21 Miltenyi Biotec Gmbh Método de separación celular
WO2015172255A1 (en) * 2014-05-16 2015-11-19 Qvella Corporation Apparatus, system and method for performing automated centrifugal separation
CH713443A2 (de) * 2017-02-08 2018-08-15 Roth Felix Medizinalröhrchen.
US11707700B2 (en) * 2017-05-01 2023-07-25 Council Of Scientific & Industrial Research Process for interfacial separation of metal nanoparticles or nanowires using centrifugal separators
WO2020090775A1 (ja) * 2018-10-31 2020-05-07 株式会社堀場製作所 遠心沈降式の粒径分布測定装置
WO2020090776A1 (ja) * 2018-10-31 2020-05-07 株式会社堀場製作所 遠心沈降式の粒径分布測定装置
JP2021194329A (ja) * 2020-06-17 2021-12-27 サミー株式会社 遊技機

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4154793A (en) * 1977-08-18 1979-05-15 Jean Guigan Device for conditioning a sample of liquid for analyzing
US4226531A (en) * 1977-08-29 1980-10-07 Instrumentation Laboratory Inc. Disposable multi-cuvette rotor
JPS62115140U (https=) * 1985-12-03 1987-07-22
JPS62111645U (https=) * 1985-12-31 1987-07-16
JP2003083990A (ja) * 2001-05-30 2003-03-19 Holger Behnk 体液を分析するための装置及び方法
JP2005043158A (ja) * 2003-07-25 2005-02-17 Wyatt Technol Corp 改良された円盤型遠心分離機および分析用超遠心分離機

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
See also references of EP4129488A4
STEPHEN T. FITZPATRICK, MEASUREMENT OF PARTICLE SIZE DISTRIBUTION BY FREQUENCY DEPENDENT CENTRIFUGAL SEDIMENTATION: ADVANTAGES AND DISADVANTAGES, CURRENT SITUATION, AND FUTURE OUTLOOK, 30 May 2018 (2018-05-30), Retrieved from the Internet <URL:https://www.nihon-rufuto.com/myadmin/rufuto_catalog/wp-content/uploads/2017/06/CPS-Polymer-News.pdf>

Also Published As

Publication number Publication date
US20230160801A1 (en) 2023-05-25
EP4129488A1 (en) 2023-02-08
JP7601861B2 (ja) 2024-12-17
JPWO2021221044A1 (https=) 2021-11-04
EP4129488A4 (en) 2024-04-24
US12313645B2 (en) 2025-05-27

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