CN1755347A - Particle size distribution device - Google Patents

Particle size distribution device Download PDF

Info

Publication number
CN1755347A
CN1755347A CN 200510085341 CN200510085341A CN1755347A CN 1755347 A CN1755347 A CN 1755347A CN 200510085341 CN200510085341 CN 200510085341 CN 200510085341 A CN200510085341 A CN 200510085341A CN 1755347 A CN1755347 A CN 1755347A
Authority
CN
China
Prior art keywords
particle
aforementioned
laser light
size distribution
particle size
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.)
Granted
Application number
CN 200510085341
Other languages
Chinese (zh)
Other versions
CN100432652C (en
Inventor
深井秋博
十时慎一郎
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.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
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 Shimadzu Corp filed Critical Shimadzu Corp
Publication of CN1755347A publication Critical patent/CN1755347A/en
Application granted granted Critical
Publication of CN100432652C publication Critical patent/CN100432652C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

To simplify a structure by dispensing with a circulation mechanism and an agitation mechanism for a medium liquid including a specimen under measurement. The lower part of a specimen cell lengthened in its vertical direction is illuminated with laser light to measure particle distribution from the spacial intensity distribution of its scattered light. After once dispersing particles in a measurement cell uniformly, the specimen cell is left at rest to start the measurement of the scattered light. Assuming that measurement time is t seconds and a distance covered by a sedimenting particle D3 in t seconds is X3, the particle diameter of the particle D3 being largest, only distances X2 and X1 smaller than X3 are covered by sedimenting particles D2 and D1 of smaller diameters. Accordingly, particle distribution has no deviation in a laser-illuminated part lower than the distance X3, making it possible to measure accurate particle size distribution on the whole group of particles without being affected by particle sedimentation.

Description

Particle size distribution device
Technical field
The invention relates to a kind of particle size distribution device that is used to measure the Size Distribution of powder particle.Wherein particularly about a kind of powder test portion irradiating laser light to disperseing in the liquid, and mensuration is from the spatial intensity distribution of the diffraction light or the scattered light of this powder particle, and utilize computing by this distribution, calculate the laser diffraction and scattering formula particle size distribution device of the size-grade distribution of determined population based on Fraunhofer diffraction theory or Mie theory.
Background technology
The liquid such as water that form the medium that disperse are different with the common proportion of powder test portion, and the proportion of test portion is great than the ratio of liquid in most mensuration test portion, so as placing after test portion and the liquid mixing, then the powder test portion can be deposited to the bottom of test portion container.Therefore, under the purpose of measuring size-grade distribution, in liquid, disperse, need carry out the stirring of liquid in order to make the powder test portion.Under the situation that is rich in the powder test portion that forms determination object, often employing is a kind of makes in the flow of liquid via flow element that contains the powder test portion by the cycling mechanism that utilizes liquid, and to this flow element irradiating laser light, thereby carry out the method for particle size distribution.Under the situation of using flow element, owing to liquid ceaselessly flows, so the powder test portion is also suitably disperseed in liquid.
And, under situations such as the amount of powder test portion is few, a spot of test portion is got in other test portion container (measuring element), and it is disperseed in liquid, also can carry out the mensuration of size-grade distribution.The relative flow element mode of this method also is known as element mode in batches.In this case, in order to form a kind of powder test portion state that appropriateness is disperseed in liquid, and be provided for rabbling mechanism that the liquid in the measuring element is stirred, and one side makes this rabbling mechanism move one side to carry out the mensuration of size-grade distribution in mensuration.If rabbling mechanism is not set, then the powder test portion can promptly be deposited to the bottom of measuring element, can't precision well size-grade distribution be measured.
The particle size distribution method of component type has illustrated in patent documentation 1 for example in batches.
[patent documentation 1] Japanese Patent Laid Open Publication spy opens flat 5-72106 communique (Fig. 1)
Equipment is used to make liquid to carry out round-robin cycling mechanism and the rabbling mechanism that is used to carry out liquid agitation, makes particle size distribution device complicated, and causes the decline of reliability and the rising of cost.But as do not have these mechanisms also precision well size-grade distribution is measured, that has been the best.
And in component type in batches, some rabbling mechanism must be arranged.For example, sometimes also use a kind of simple paddle-type mixer structure that only disposes in measuring element inside, and the magnetic stirrer passed on by magnetic force from the outside of the power that is used in action, but in this case, also produce the problems such as mensuration that to carry out the magnetic powder.
Summary of the invention
The present invention forms in view of above-mentioned problem, its objective is to make the device easy and seek to improve reliability, and seeks the reduction of installation cost.And, its objective is and do not use magnetic stirrer also can carry out the mensuration of magnetic powder.
In order to solve above-mentioned problem, the present invention is a kind of particle-irradiation laser light to being disperseed in the liquid in measuring element, and mensuration forms the spatial intensity distribution of the scattered light of scattering because of this particle, and calculate the particle size distribution device of the size-grade distribution of this particle, it is characterized in that: the length of the vertical direction of aforementioned measuring element, by the maximum settlement speed of particle with measure the maximum settlement distance of the particle that time of needing derives.
Utilize the particle velocity in the liquid of effect of gravity, with regard to a material, every particle directly is certain, and big more particle precipitation is fast more.The settling velocity of particle that is maximum particle footpath is the fastest, by its speed with measure the needed time and can calculate the maximum settlement distance that the particle in maximum particle footpath in minute carries out sedimentation.As make the length of measuring element on gravity direction than this maximum settlement distance, even then in mensuration, do not stir, also can measure size-grade distribution.
In above-mentioned particle size distribution device, preferably aforementioned laser light is also wanted downward part to the irradiated site of aforementioned measuring element for measure aforementioned maximum settlement distance downwards than the liquid level in aforementioned measuring element.
By this, on the position that laser light is shone, the particle of settling velocity maximum is during the particle of maximum particle diameter also can be present between test period, so can measure all correct size-grade distribution of population.
In addition, in this particle size distribution device, aforementioned measuring element is made of the material that can see through this laser light as the irradiated site that only makes aforementioned laser light, and other part is made of other material, then can make testing material element at an easy rate.
In particle size distribution, need instrumentation weak scattering light, so in the material of the testing material element of the wall that passes through as laser light, need to use the quartz glass that generally is used as optical material usually.When utilizing this quartz glass making element all, because testing material element length of the present invention is long, so the quartz glass that uses is also many, but it is as if above-mentioned like that except the illuminated portion of laser light, all utilizing cheap metal and plastic material, the required expense of making that then can cut down testing material element.
In about the present invention's one particle size distribution device, do not need to form the cycling mechanism and the rabbling mechanism of the liquid that disperses medium, and just utilize an only vertically long testing material element, so constituent apparatus at an easy rate.And, because mechanism is simple,, realize the raising of reliability so can reduce fault.
And in about another particle size distribution device of the present invention, the particle in maximum particle footpath can be measured all correct size-grade distribution of population not than the downward sedimentation in laser radiation position before measuring end.
In addition, in another particle size distribution device about the present invention, can cheap material testing material element, constituent apparatus more at an easy rate.
Description of drawings
Fig. 1 is the summary pie graph of particle size distribution device of the present invention.
Fig. 2 is the key diagram of effect of the present invention.
1: LASER Light Source 2: condenser
3: spatial filter 4: collimator lens
5: testing material element 6: condenser
7: ring detector 8: the sampling of data circuit
9: control device 10: optical axis
D1, D2, D 3: particle footpath
X1, X2, X3: distance
Embodiment
Size-grade distribution device of the present invention is described by summary pie graph shown in Figure 1.By condenser 2, spatial filter 3, collimator lens 4, formation shines on the testing material element 5 after having the parallel-beam of setting the beam dimension diameter from 1 emitted laser light of LASER Light Source.In apparatus of the present invention, the configuration of optical axis 10 approximate horizontal of irradiating laser light.In testing material element 5, be full of liquid such as pure water, and wherein be dispersed with powder test portion as determined test portion.The laser light of being shone on the powder test portion is utilized the effect of scattering or diffraction by the particle of powder test portion, along the direction radiation of leaving from optical axis 10, and this scattered light utilizes condenser 6 to carry out light harvesting to the surface of ring detector 7.
Ring detector 7 can detect the scattered intensity that is produced because of the powder test portion in the testing material element to every scattering angle by being that a plurality of photodetectors that the center disposes ringwise constitute with optical axis 10.The output of ring detector 7 is taken in the control device 9 by sampling of data circuit 8 at every scattering angle.Control device 9 is for containing the device of computing machine, spatial intensity distribution by obtained as described above scattered light, carry out computing, and calculate the size-grade distribution of the powder test portion that in testing material element 5, is disperseed based on Mie theory or Fei Langhefei scattering theory.
Describe again about testing material element 5.Testing material element 5 among the present invention is the container of cube shaped of the upper end atmosphere opening of vertical direction, is used as batch-wise element and uses.This just puts into the liquid that is formed for making the medium that the powder test portion disperses, is not to resemble the flow-type element with other circulating device etc. to be communicated with.And the irradiated site of irradiating laser light is that quartz glass etc. constitutes by material transparent at least, powder test portion irradiating laser light that can be in testing material element, and the scattered light that is caused because of the powder test portion is emitted to the testing material element outside.
It is long that this testing material element is characterised in that the length of vertical direction is configured, and be set with the irradiated site of laser light at the lower position of this testing material element.By utilizing such element, can not use stirring apparatus, and obtain correct size-grade distribution as the powder particle group of determined object.
Utilize Fig. 2 that the action and the effect of this sample element are described.Can will before measuring scattered intensity, stir the liquid in the testing material element in advance test portion irradiating laser light.The stirring of this moment utilizes stirring rod etc. to stir simply by operating personnel and gets final product.After well stirring, leave standstill degree and when calming down, form a kind of particle homodisperse state in liquid of all sizes with convection current.In order to oversimplify, suppose a kind of 3 particles footpaths D1, D2, D3 (state of the particle of D1<D2<D3), and form state shown in Fig. 2 (a) that exists.
Then, the particle of each size carries out sedimentation respectively, be certain speed but one one particle carries out the speed of sedimentation, and this speed is different because of the size of particle.That is, the settling velocity of particle is according to Stokes' law, so carry out sedimentation with the speed Vt shown in the Stokes formula of following formula.
V t=(ρ PW)D 2g/18μ ...(1)
Here, ρ P: Particle Density, ρ W: the density of matchmaker's liquid, D: the diameter of particle, g: acceleration of gravity, μ: the viscosity of matchmaker's liquid.This formula represents that the big particle in particle footpath promptly carries out sedimentation.According to the condition in particle footpath, the settling velocity of particle is according to Alan's law and Newton's law, but no matter for any also be that the big particle in particle footpath promptly carries out sedimentation.
In Fig. 2, establishing maximum particle D3 is deposited to the upper end of laser irradiating part from liquid level time is t second, and then the state from Fig. 2 (a) after second, forms the state of Fig. 2 (b) through t.As the distance of establishing 3 sedimentations of particle D is X3, and then the settling height of particle D2 is X2, and the settling height of particle D1 is X1.And magnitude relationship separately forms X1<X2<X3.
The settling velocity of each particle that the particle footpath is identical is identical value each other, and do not change in time and be certain value, in addition because laser irradiating part is in downside apart from the position of liquid level X3, so the concentration of each particle in the laser irradiating part did not change during this t second.That is, can during this t second, there be the skew of the size-grade distribution that causes because of sedimentation, and size-grade distribution is measured.Here said size-grade distribution skew for example is meant after the time of second, not have particle D3 at laser irradiating part greater than t in process that so the particle that exists is D1 and D2 only, the size-grade distribution of being observed seems the situation to the displacement of small-particle side.
State about Fig. 2 (b) describes again.Since from the liquid level to the distance X between 1 the particle of all sizes carry out sedimentation, so do not have particle in this zone.From forming the zone that only has particle D1 the distance X 1 to X2.There are particle D1 and particle D2 from the distance X 2 to X3, do not have particle D3.And, on the part big, have all particle D1, D2, D3 than distance X 3, and concentration separately the state with initial is identical respectively.Therefore, by as described above, make laser irradiating part be configured in downside with the position of liquid level distance X 3, the time of mensuration, can be measured as all correct size-grade distribution of population in second at t.
This situation in general, as estimate that the maximum particle of determination object carries out the speed of sedimentation, and by this value with measure the required time and estimate the maximum settlement distance that maximum particle carries out sedimentation in minute, then, can carry out correct particle size distribution by utilizing the length testing material element big than this distance.More exactly, as make distance big, then do not have the skew of the size-grade distribution that causes because of sedimentation, can carry out correct particle size distribution than the maximum settlement distance from the liquid level of matchmaker's liquid to the irradiated site of laser light.
About the size of particle and the size of testing material element, as an example with some concrete numerals.For example, make beaded glass as the particle test portion and in water, disperse, and to make maximum particle directly be 100 μ m.As with particle density: 2500kg/m 3, matchmaker's liquid density: 1000kg/m 3, matchmaker's liquid viscosity: 0.001Pas, weight acceleration: 9.8m/s 2Be applied to calculate in the above-mentioned formula (1), then settling velocity is 8.2mm/s.
The length of known employed common element is about 100mm, and the distance of the upper end from the liquid level to the laser irradiating part is about 50mm.This moment, the particle of maximum diameter 100 μ m arrived the upper end of laser irradiating part, as utilized above-mentioned settling velocity 8.2mm/s to calculate, be about 6 seconds after.
Here, as if the present invention is such, make testing material element vertically extend to for example 300mm, then the distance of upper end is 250mm from the liquid level to the laser irradiating part.At this moment, after the upper end of the particle of maximum diameter 100 μ m arrival laser irradiating part is about 30 seconds as calculated.Under 6 seconds the situation when using known element,, just measure 1 time and so on, and be difficult to usually measure even skilled operating personnel promptly measure.But, as if the present invention prolongs testing material element like this, then can form 30 seconds time, can measure by any people, and can measure repeatedly.
Employed testing material element also can all be made by quartz glass and the such transparent material of transparent plastic in apparatus of the present invention.And, because container need be the transparent just irradiated site of laser light, thus also can make this part utilize transparent materials such as glass, and other part is utilized metal and opaque plastics, and the member more than 2 is combined to form container.Because transparent part can be the optical axis part that laser light is passed through, thus also can make near the part of 2 involutory formation optical axises of transparent panel, and other part utilizes other shape and material to make.
And, in above-mentioned example, testing material element be shaped as the open Nogata body in upper end, but also can be other shape, for example columniform shape.And the upper end opening is not necessary to element, as dreams up a kind ofly in the method that the powder test portion is disperseed, even the testing material element to utilizing lid to seal then, the present invention also is effective.The for example also hand-holdable testing material element that has lid vibrates, and then testing material element is installed on the locating of setting.

Claims (5)

1. particle size distribution device, to the particle-irradiation laser light of being disperseed in the liquid in measuring element, and mensuration forms the spatial intensity distribution of the scattered light of scattering because of this particle, and calculate the size-grade distribution of this particle, it is characterized in that: the length of the vertical direction of aforementioned measuring element, by the maximum settlement speed of particle with measure the maximum settlement distance of the particle that time of needing derives.
2. particle size distribution device according to claim 1 is characterized in that: aforementioned laser light is to the irradiated site of aforementioned measuring element, for the aforementioned maximum settlement distance of measuring downwards than the liquid level in aforementioned measuring element is also wanted downward part.
3. particle size distribution device according to claim 2 is characterized in that: aforementioned measuring element has only the irradiated site of aforementioned laser light to be made of the material that can see through this laser light, and other part is made of other material.
4. particle size distribution device according to claim 3 is characterized in that: the aforementioned material that sees through this laser light is a quartz glass.
5. particle size distribution device according to claim 3 is characterized in that: aforementioned other material is metal or plastic material.
CNB2005100853414A 2004-09-29 2005-07-22 Particle size distribution device Expired - Fee Related CN100432652C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2004-284615 2004-09-29
JP2004284615A JP4507799B2 (en) 2004-09-29 2004-09-29 Particle size distribution measuring device
JP2004284615 2004-09-29

Publications (2)

Publication Number Publication Date
CN1755347A true CN1755347A (en) 2006-04-05
CN100432652C CN100432652C (en) 2008-11-12

Family

ID=36238178

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2005100853414A Expired - Fee Related CN100432652C (en) 2004-09-29 2005-07-22 Particle size distribution device

Country Status (2)

Country Link
JP (1) JP4507799B2 (en)
CN (1) CN100432652C (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104380078A (en) * 2012-06-06 2015-02-25 株式会社岛津制作所 Fine particle classification measurement device, sample creation device with uniform particle concentration, and nanoparticle film forming device
CN104483165A (en) * 2014-11-21 2015-04-01 江苏博迁新材料有限公司 Sampling method of large-particle-diameter powder in ultrafine magnetic powder
JP2016099279A (en) * 2014-11-25 2016-05-30 株式会社島津製作所 Particle analyzer and particle analysis method
CN104458512B (en) * 2014-12-01 2016-09-07 华中科技大学 A kind of method measuring particle swarm fractal dimension
CN106290087A (en) * 2016-09-21 2017-01-04 迈安德集团有限公司 Micro-size fraction material automatic grading experimental system

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101881719B (en) * 2010-06-28 2012-01-04 中国科学院西安光学精密机械研究所 Test method of gel particles in polyacrylonitrile polymer solution
KR101458320B1 (en) * 2013-08-29 2014-11-04 전북대학교산학협력단 Viscometer using Terminal setting velocity and Method of measuring viscosity
JP6864908B2 (en) * 2016-03-28 2021-04-28 国立研究開発法人 海上・港湾・航空技術研究所 Ore wear evaluation method and ore wear measuring device
JP6872558B2 (en) * 2016-11-16 2021-05-19 株式会社堀場製作所 Particle size distribution measuring device, particle size distribution measuring method, and program for particle size distribution measuring device

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58160842A (en) * 1982-03-18 1983-09-24 Horiba Ltd Light transmitting type measuring method of particle size distribution
US4457624A (en) * 1982-05-10 1984-07-03 The United States Of America As Represented By The Secretary Of The Interior Suspended sediment sensor
AT393169B (en) * 1985-06-05 1991-08-26 Staudinger Gernot METHOD AND DEVICE FOR GRANE SIZE ANALYSIS
US4696571A (en) * 1985-10-25 1987-09-29 The United States Of America As Represented By The Secretary Of The Interior Suspended sediment sensor
CN2041041U (en) * 1987-11-19 1989-07-12 河海大学 Detecting device for wide-range particle size analyzer
JPH02212742A (en) * 1989-02-13 1990-08-23 Kowa Co Measuring apparatus for fine particle in liquid
JPH0438442A (en) * 1990-06-04 1992-02-07 Sumitomo Chem Co Ltd Automatic particle size distribution measuring device
JPH0572106A (en) * 1991-09-17 1993-03-23 Shimadzu Corp Particle size distribution measuring device
JPH10213534A (en) * 1997-01-29 1998-08-11 Shimadzu Corp Particle size distribution measuring device
JP2002062248A (en) * 2000-07-01 2002-02-28 Malvern Instruments Ltd Device and method for specifying particle size distribution
CN1202412C (en) * 2003-07-01 2005-05-18 武汉理工大学 Settling type laser reflection image point granularity measuring method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104380078A (en) * 2012-06-06 2015-02-25 株式会社岛津制作所 Fine particle classification measurement device, sample creation device with uniform particle concentration, and nanoparticle film forming device
CN104483165A (en) * 2014-11-21 2015-04-01 江苏博迁新材料有限公司 Sampling method of large-particle-diameter powder in ultrafine magnetic powder
CN104483165B (en) * 2014-11-21 2017-07-28 江苏博迁新材料股份有限公司 The sampling method of big particle diameter powder in a kind of ultra-fine magnetic powder
JP2016099279A (en) * 2014-11-25 2016-05-30 株式会社島津製作所 Particle analyzer and particle analysis method
CN104458512B (en) * 2014-12-01 2016-09-07 华中科技大学 A kind of method measuring particle swarm fractal dimension
CN106290087A (en) * 2016-09-21 2017-01-04 迈安德集团有限公司 Micro-size fraction material automatic grading experimental system

Also Published As

Publication number Publication date
JP4507799B2 (en) 2010-07-21
JP2006098212A (en) 2006-04-13
CN100432652C (en) 2008-11-12

Similar Documents

Publication Publication Date Title
CN100432652C (en) Particle size distribution device
Gee et al. 2.4 Particle‐size analysis
US9310286B2 (en) Patient sample classification based upon low angle light scattering
US20050248765A1 (en) Small container fluid dynamics to produce optimized inspection conditions
Zarraga et al. The characterization of the total stress of concentrated suspensions of noncolloidal spheres in Newtonian fluids
US5272092A (en) Method for analyzing a reaction solution
Marrington et al. Validation of new microvolume Couette flow linear dichroism cells
US9019493B2 (en) Method and device for the characterization of multiple samples of one or various dispersions
CN1346970A (en) Balance with weighing chamber
JP2585740B2 (en) Automatic analyzers and reaction vessels
Norton et al. The measurement of particle sizes in clays
EP1808687A3 (en) Absolute measurement centrifuge
JP3283078B2 (en) Immunological measurement device
McFadyen et al. High-resolution particle size analysis from nanometres to microns
KR101458320B1 (en) Viscometer using Terminal setting velocity and Method of measuring viscosity
EP3382370A1 (en) Probe arrangement and method for rheometric measurements with a disposable probe and remote readability
Börger et al. Development of a new digital camera setup for the online recording of Schlieren optical pictures in a modified Beckman Optima XL analytical ultracentrifuge
EP0021236A1 (en) Method for optically assaying liquid samples
Ghorbanian Farah Abadi The role of rheology in the flow and mixing of complex fluids
Ahmed et al. A designed setup of low-priced in-house goniometer/tensiometer
RU118746U1 (en) PHOTOSEDITEMETER
Colfen et al. A Modified Experimental Setup for Sedimentation Equilibrium Experiments with Gels: Part 2: Technical Developments
CN216309714U (en) Device for measuring content of ultra-large particles in particle material
Chambino et al. New optical method for water treatment control
RU2310185C1 (en) Method of determining sizes of nonmagnetic dispersion particles using magnetic fluid

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20081112

Termination date: 20180722

CF01 Termination of patent right due to non-payment of annual fee