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WO1994020833A1 - Procede et appareil de manipulation, de positionnement et d'analyse de particules en suspension - Google Patents

Procede et appareil de manipulation, de positionnement et d'analyse de particules en suspension Download PDF

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Publication number
WO1994020833A1
WO1994020833A1 PCT/GB1994/000431 GB9400431W WO9420833A1 WO 1994020833 A1 WO1994020833 A1 WO 1994020833A1 GB 9400431 W GB9400431 W GB 9400431W WO 9420833 A1 WO9420833 A1 WO 9420833A1
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WIPO (PCT)
Prior art keywords
particles
fluid
radiation
suspension
characteristic
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/GB1994/000431
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English (en)
Inventor
Ian Leslie John Holwill
Gareth Bowen Davies
Nigel John Titchener-Hooker
Michael Hoare
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University College London
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University College London
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Application filed by University College London filed Critical University College London
Publication of WO1994020833A1 publication Critical patent/WO1994020833A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/28—Mechanical auxiliary equipment for acceleration of sedimentation, e.g. by vibrators or the like
    • B01D21/283—Settling tanks provided with vibrators
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D43/00—Separating particles from liquids, or liquids from solids, otherwise than by sedimentation or filtration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography

Definitions

  • This invention relates to methods of manipulation and analysis of the positions of particles suspended in a fluid and finds particular application in the in situ optical monitoring of suspensions of particles of differing sizes.
  • bands or “banding” is used to describe the formation of striations of particles in suspension by ultrasound.
  • internodal light scattering is used to describe the formation of striations of particles in suspension by ultrasound.
  • IMS is used to describe the coupling of optical analyses with such ultrasonic pre-preparation of the sample.
  • Photon correlation spectroscopy is a technique for measuring particle diffusion coefficients in suspension. It has been applied to many biological systems in the past as it is a fast, accurate and noninvasive measure which can be used for inferring particle size or velocity distribution. The technique may be applied to the problem of analysis of complex process streams on-line in a biochemical pilot plant. This is a useful technique for monitoring and control applications using information such as size distribution and concentration to optimise yield in a multi-stage purification process. Here a wide distribution of particle size is encountered.
  • One of the problems faced is the fast and non-invasive sample preparation needed to remove unwanted particulates from the suspension prior to measurement.
  • a method of particle handling in which a source of acoustic oscillations is applied to a conduit through which a particulate fluid suspension may be caused to pass to create acoustic standing waves in said suspension, thereby to create local inhomogeneities in the positional distribution of particles in said suspension.
  • apparatus for conditioning samples of particulates suspended in a fluid comprising a flow cell having input and output ports for the ingress and egress of fluid and primary and secondary sources of acoustic radiation to direct radiation at said flow cell to create acoustic radiation nodes and anti-nodes therein.
  • These local inhomogeneities may be used for purposes of measurement or particle removal and separation.
  • Figure 1 is a graph showing correlogram data for different particle sizes
  • Figure 2 is a schematic diagram illustrating the principles of the internodal light scattering technique
  • Figures 3a to 3d show the migration of suspended particles under the influence of acoustic radiation
  • Figure 4 is a schematic diagram of one specific embodiment of the invention
  • Figure 5 shows a practical cell design for use with the apparatus of Figure 4;
  • Figures 6 to 9 are results of measurements made on suspensions of different sized particles.
  • FIGS 10a to 13 are diagrams illustrating specific embodiments of the invention.
  • Photon correlation spectroscopy measures intensity fluctuations from a suspension of particles undergoing Brownian motion and from these fluctuations a diffusion coefficient is calculated which can be related to particle size.
  • the relation for the relaxation rate of the fluctuations and diffusion coefficient are shown below.
  • the problem of inverting such data into the required distribution is an ill-posed question, that is to say, for one set of data many solutions can be fitted to within the noise of the experiment.
  • the correlation function can be represented as below.
  • the experimental procedure of photon correlation results in a correlation function which in the case of a range of particle size measurement is a sum of many exponential decays.
  • a priori information about the size distribution may also be included to aid the deconvolution programs. However, improvement of the data quality must be the first step to a reliable measurement of the system.
  • T is the experiment duration. This shows that a determining factor for noise on the correlogram is the largest particle size present (all other things being equal).
  • the only other way to improve the ratio is to increase gamma. This can be done by using larger angles. If the maximum particle size is reduced however this will increase gamma as there is an inverse relation between the two.
  • Multiple sample time correlators are used so that a wide range of particle size distribution can be covered. Better resolution is possible however with a narrower size range and a correspondingly narrower spacing of sample times. Keeping T as low as possible is important in on-line applications.
  • Dust particles are always a problem in light scattering experiments. In particular it makes the noise level of measurement difficult to assess and this information is necessary in some data processing techniques. In most photon correlation instruments dust detection systems operate to shut down the data collection when dust is in the laser beam. This operates using estimates of dust size and the dimensions of the scattering volume. In biochemical engineering applications, smaller particles in the suspension are often those of most interest i.e. they are the product and the larger particles unwanted (although they provide useful information for process optimisation considerations). Examples are virus-Uke particles or hepatitis-B virus surface antigen vaccine particles both of which can be expressed in carrier cells such as yeast.
  • Yeast homogenate covers a wide range of particle size from whole cell ghosts of about 5 ⁇ m down to the 200nm region.
  • the upper size limit is about 3 microns and the presence of particles larger than this compromise the result substantially.
  • filtration or centrifugation is required to remove the larger contaminants although their size and quantity are still an important measure in the present situation. More recently a two aqueous phase operation has been used to separate the smaller contaminants.
  • a miniaturised centrifuge may be used to remove unwanted components rapidly and for small sample volumes.
  • Inline filters are also used to remove dust particles from the samples. We have found that the presence of these large particles tends to distort the resulting size distribution or indeed hide the smaller particles altogether so that sample preparation is essential prior to measurement.
  • the errors in the baseline can do more than simply shift the distribution.
  • the larger particles can contribute an almost constant offset to the baseline when their size is such that it is out of range of the correlator.
  • Acoustic standing waves cause migration of fine particles in suspension to the nodes of the sound field which are spaced at half-wavelength distances.
  • the main driving force for migration is the radiation pressure exerted on each particle in suspension. Equation 3 describes the radiation pressure exerted on a spherical particle in a plane stationary wave.
  • FIG 2 is a schematic of the internodal light scattering 0 technique (ILS).
  • Particles 21 migrate towards nodes 23 in the standing wave field where the pressure is minimum.
  • the force on the particles is size dependent hence larger particles may be fractionated from the smaller and with appropriate choice of ultrasonic frequency the distance between the nodes allows a 5 focused laser beam 25 to pass through for light scattering analysis.
  • the distance between the nodes is of the order of hundreds of microns and the diameter of the laser beam is of the order of tens of microns.
  • Figures 3a-3d show the migration of particles at four stages from initial application of a standing wave field.
  • FIG 4 is a schematic diagram of the ILS apparatus.
  • An RF signal generator and amplifier 41 feed a transducer 42 connected to the light scattering cell 46 by way of a waveguide 44 and reservoir 42.
  • the laser 45 and detector 47 part of the Malvern 4700 photon correlation spectrometer, are set up to perform light scattering analysis on the internodal spaces.
  • the oscilloscope 49 is used to monitor the voltage fed to the ultrasonic transducers.
  • any particles over a chosen size can be immobilised or "banded" at the nodal plane of the stationary wave leaving the smaller particles free (unhanded) in the inter-nodal spaces.
  • Appropriate choice of ultrasonic frequency and laser beam dimensions allows the particles in the inter-nodal spaces to be analysed by photon correlation spectroscopy. It is possible to do this rapidly and in situ so that a sample can be put into the apparatus without filtration or centrifugation steps and their associated problems. In the present application this may in some cases enhance and in other cases make possible measurement of soluble or insoluble products further up the unit operations chain.
  • the technique of coupling laser analysis with ultrasonic standing wave clarification has been termed internodal light scattering (ILS).
  • Ultrasonic frequencies in the region of 1MHz were chosen due to relatively large distance between the nodal planes of the generated sound field and because of the efficient separation that occurs with sound of this frequency.
  • An Audley Scientific Stabilised Frequency Signal Generator and Dual Ultrasonic Amplifier were used to drive the PC4 ceramic transducer (Morgan Matroc Ltd) producing the sound field.
  • the initial work was carried out with a Malvern 4700 photon correlation instrument with a 633nm HeNe 30mW laser and an IBM PS2 for data processing. This technique is capable of particle sizing in the range 3 ⁇ m down to about 3nm.
  • the ultrasonic sample cell was set up in the index matching bath of the Malvern 4700 which reduces unwanted light reflections at the sample cell wall and fine vertical adjustment was facilitated by means of a Melles Griot optical component fine positioner. Thus the light beam could be passed through any part of the sample cell required.
  • Polystyrene latex particles were chosen for use in this investigation as the aim of the work was to remove large particles from mixtures containing sub icron particles. Initial experiments were conducted using mixed mono odal distributions of very small latex particles (39nm) and larger (4.000 to 15.000nm) particles. The difference in average size between the two component distributions in suspension was then reduced to assess the lower size limit for the effective removal of the larger particles from the inter-nodal spaces.
  • yeast homogenate diluted 1: 10 with filtered phosphate buffer was investigated with ILS analysis.
  • the transducer voltage used was in the region of 25 volts peak-to-peak for the experiments using polystyrene latex particles and considerably higher (50 volts p-p) for the yeast homogenate experiments. The higher power levels were required due to the lower values of F associated with such biological particles.
  • the water reduces flare and reflections where the laser beam hits the outer walls of the tube.
  • Glass windows 54,55 are present in both the straight through position for transmission measurements and at 90 degrees for light scattering measurements.
  • 0-rings 56 prevent the sample and index-matching water from mixing.
  • the approximate dimensions of the device are 130mm from top to bottom and 50mm across and deep.
  • the results obtained for a mixture of polystyrene latex spheres are shown in Figure 6. Particle size analysis of a mixture of 4 ⁇ m and 39nm latex spheres.
  • the solid line shows the analysis without banding.
  • the two dotted traces are the internodal analysis and an analysis of 39nm spheres alone for comparison.
  • the internodal analysis gives rise to a slightly broadened distribution probably due to scattering at the nodal planes.
  • the distribution means for the lower two traces are 42.2nm for the onodisperse and 53.5nm for the internodally analysed mixture.
  • a bimodal distribution is not shown for the normal analysis of the mixture as the software method used here was the cumulants method which is strictly for unimodal distributions but indicates the presence of the larger particles in the suspension by returning a higher distribution mean of 496.6nm.
  • Results from an analysis performed on the concentrated bands of particles accumulated at the nodes of the standing wave field show a mean of 18,500nm, about nine times the actual size of the 2,000nm particles. This result may be attributed to a number of phenomena, such as may be caused by the high concentration of the particles in this region resulting in particle interaction effects such as particles aggregating to form floes of particles; or an effect of the ultrasonic field hindering the normal diffusion of the particles.
  • multiple scattering of the light from the sample may occur which invalidates the analysis technique used by the instrument as it is based on singly scattered light.
  • multiple scattered light when interpolated in a dynamic light scattering experiment, will give rise to a lower than expected particle size rather than a very much greater one, hence one of the aforementioned causes is likely to be the reason for the large particle size returned by the analyser.
  • the dotted line represents a normal analysis (without ultrasound) of the mixture and shows a bimodal distribution indicating the presence of 85nm particles.
  • the very broad peak from 5,000nm upwards reveals the presence of contaminants and as well as the 15,000 nm particles in the mixture.
  • the ILS analysis shows a dramatic increase in the 85nm peak indicating the removal of the 15,000nm particles from the inter-nodal space.
  • the remaining signal at 200-1,200 nm represents the contaminating particles in the suspension whose distribution has now been resolved by the removal of the 15,000 nm particles by the standing wave field.
  • Figure 9 a chart which shows internodal analysis of a suspension of 1.4 ⁇ m and 85nm latex spheres.
  • the original distribution (not shown) is very similar and shows that, for this experimental set-up, the banding limit for latex spheres is about 1.4 ⁇ m. It will be possible to extend banding to lower particle sizes by appropriate modification to the design of the ultrasonic cell.
  • results of the ILS measurements returned a mean particle size of 636 ⁇ 215nm with a polydispersity of 0.438 ⁇ 0.051 for the yeast homogenate.
  • Normal analysis (without ultrasound) of the homogenate gave a mean size of 1003 ⁇ 328.2nm and a polydispersity of 0.535 ⁇ 0.186 (The polydispersity is a measure of the deviation of the particle distribution from a perfect onodisperse distribution).
  • the 90° scattered light from the normal and inter-nodal samples was 129.9xl0 3 ⁇ 14.4xl0 3 and 79.8xl0 3 ⁇ 14.5xl0 3 (counts per second) respectively indicating that particles contributing to nearly half of the scatter intensity had been shifted to the nodes of the standing wave field.
  • Applications of this device for on-line sampling in biochemical pilot plant operations are wide.
  • VLP monitoring after homogenisation requires removal of a substantial fraction of the large yeast debris particles and it has been shown that yeast homogenate bands readily in the standing wave field.
  • Dust particles especially for forward light scattering applications may be held away from the beam. This will be particularly useful in quality assurance and control experiments.
  • one ultrasonic transducer and a reflector or two transducers acting in opposition are operated across a sample chamber as shown in Figure 5.
  • a standing wave field is created resulting in a periodic variation of pressure through the sample.
  • the particles in suspension migrate to where the pressure gradient is minimum which is at the vibration nodes of the standing wave. These are spaced at half-wavelength intervals through the sample.
  • the speed of sound in water is approximately 1500ms "1 and the frequency of sound used is typically from 500Hz up to 10MHz.
  • a 1MHz standing wave in water therefore has an inter-nodal spacing of 750mm.
  • Ultrasonic standing waves maybe used to segregate particle suspensions in terms of size forming striations of particles in the sample of alternately large and small particle sizes as described above. The width of these striations is of the order of the acoustic wavelength, typically several hundred microns.
  • the acoustic forces acting on the particles are strongly dependent on size and the energy density of the acoustic field may be varied to choose a particular size cut-off above which particles will move into striations leaving the smaller species to diffuse freely between these "bands".
  • the smaller particles or other components may then be examined by light scattered from a focused laser beam which may be aimed into the suspension between the striations of large particles.
  • the diameter of a focused beam at visible wavelengths may be easily designed to be of the order of lOOnm.
  • the distance between the centres of the striations is ⁇ /2 where ⁇ is the acoustic wavelength in the medium. For a 2MHz frequency wave in water this is 375mm.
  • the scattered light may be detected with a complementary optical set-up and hence a light scattering experiment carried out.
  • sample delivery and extraction are very simply effected with a stopped flow system. No membrane changes are required and no moving parts for sample delivery or extraction and the set-up can be simply operated in a contained fashion which may be important when dealing with volatile, corrosive or toxic samples.
  • the sample to sample separation characteristics are also fixed by the energy density of the acoustic field. Acoustic streaming forces which are generated due to non-uniform radiation pressure across the sample due to a non-uniform radiation from the driving transducer may cause flow effects throughout the sample similar to thermal convection currents and such flows may affect the particle size measurement. In practice we have found that reducing the area over which banding occurs will aid reduction of such disturbances however a larger area allows a greater energy density in the acoustic field and hence better separation.
  • a priori information about the size distribution may also be included to aid the deconvolution programs, however improvement of the data quality must be the first step towards the realisation of a reliable measurement of the system.
  • the measurement can often provide more information if the range of particle size to be measured is reduced. Also the presence of particles above the upper size threshold at which the sizing technique operates decreases the signal to noise ratio at the detector by scattering spurious light. The removal of such particles can therefore provide better data from which to calculate the size distribution of the sample. The free diffusion of the smallest particles is unaffected by the ultrasonic forces.
  • the measurement of optical density is prevalent in many areas in order to determine concentrations of solutions or suspensions.
  • the Beer-Lambert law is usually used to describe the reduction in transmitted light intensity due to scattering and absorption in dilute systems. When the sample is more concentrated multiple scattering occurs and the Beer-Lambert law breaks down. In such cases alternative theories must be used or a calibration made.
  • the ILS method may be useful here.
  • the first concerns the measurement of solutions or small particulates in the presence of large and the second the measurement of low concentrations of particles which may be enhanced by concentrating them with the ultrasound into the measurement volume.
  • the former reflects a similar situation to that found in DLS in that the presence of larger particles in the suspension cause the detected signal to be dominated by light scattered from such particles and further information may be available if these particles are removed.
  • the latter situation may be useful where a low concentration of particles open to manipulation by ultrasound may only be detected by increasing their local concentration thus rending a higher OD or scattered signal .
  • FIG. 11 The geometry of this set-up depends upon the method of refractive index measurement but one possible method is shown in Figure 11.
  • a sample cell 111 is mounted on a glass block 113 of refractive index N. Acoustic waves are generated by a transducer 115. Incident optical I- j radiation is focused by a lens 117. The emergent radiation I t is measured by a diode array 119.
  • Another possible application is infra-red spectroscopy. The detection method for this is the absorption of infra-red radiation due to the optical resonances of chemical bonds. With knowledge of components present and precalibration, multi-component mixtures may be quantified. Again for complex suspensions where soluble components are of interest, the larger particulates often hinder the accuracy of the detected signal.
  • Low angle and multiple angle laser light scattering may be used to determine molecular weight and elucidate particle shape, as shown in Figure 13, which shows a sample 131 held in a cylindrical cell 133.
  • Light from a laser beam is scattered through an angle ⁇ by the particles.
  • a direct analogy of the case of dynamic light scattering may be drawn here when attempting to measure small components in a complex mixture. In particular for low angle measurements where scattering from large particles is greatest it will be most useful in removing unwanted scatterers.
  • the technique is not restricted to clearing suspensions for dynamic light scattering experiments alone. Static light scattering would also be possible in the simplest case for optical density measurements. The technique should find applications in other areas as well.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

Dans ce procédé de manipulation des particules, une source d'oscillations acoustiques est appliquée à un conduit à travers lequel passe un fluide contenant des particules en suspension. Cette source crée des ondes acoustiques stationnaires dans la suspension, provoquant ainsi localement une absence d'homogénéité dans la distribution des particules, ce qui peut être utilisé pour améliorer le rapport signal/bruit d'un faisceau optique d'interrogation.
PCT/GB1994/000431 1993-03-05 1994-03-07 Procede et appareil de manipulation, de positionnement et d'analyse de particules en suspension Ceased WO1994020833A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9304545.8 1993-03-05
GB939304545A GB9304545D0 (en) 1993-03-05 1993-03-05 Method and apparatus for positional manipulation of suspended particles

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WO1994020833A1 true WO1994020833A1 (fr) 1994-09-15

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2867279A1 (fr) * 2004-03-05 2005-09-09 Nanotec Solution Procede et dispositif pour mesurer et caracteriser une biomasse, application a une mesure en ligne de donnees de biomasse dans un processus de fermentation, et procede de pilotage associe
WO2006002452A1 (fr) * 2004-07-05 2006-01-12 Austria Wirtschaftsservice Gesellschaft mit beschränkter Haftung Procede et dispositif de spectroscopie raman
US7568251B2 (en) 2006-12-28 2009-08-04 Kimberly-Clark Worldwide, Inc. Process for dyeing a textile web
WO2011006525A1 (fr) * 2009-07-13 2011-01-20 Foss Analytical A/S Analyse d'un liquide séparé par voie acoustique
US8858892B2 (en) 2007-12-21 2014-10-14 Kimberly-Clark Worldwide, Inc. Liquid treatment system
US9239036B2 (en) 2006-09-08 2016-01-19 Kimberly-Clark Worldwide, Inc. Ultrasonic liquid treatment and delivery system and process
US9283188B2 (en) 2006-09-08 2016-03-15 Kimberly-Clark Worldwide, Inc. Delivery systems for delivering functional compounds to substrates and processes of using the same
US9421504B2 (en) 2007-12-28 2016-08-23 Kimberly-Clark Worldwide, Inc. Ultrasonic treatment chamber for preparing emulsions
EP3220131A1 (fr) 2016-03-17 2017-09-20 Commissariat À L'Énergie Atomique Et Aux Énergies Alternatives Procédé de caractérisation d'un échantillon liquide comportant des particules
US10245821B2 (en) 2015-12-04 2019-04-02 At&T Intellectual Property I, L.P. Reusable networked 3-D printing

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EP0147032A1 (fr) * 1983-10-31 1985-07-03 National Research Development Corporation Manipulation de particules
JPS6166150A (ja) * 1984-09-08 1986-04-04 Olympus Optical Co Ltd 免疫反応測定方法
US4877516A (en) * 1986-05-27 1989-10-31 National Research Development Corporation Manipulating particulate matter
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005085412A3 (fr) * 2004-03-05 2006-01-19 Nanotec Solution Procede et dispositif pour mesurer et caracteriser une biomasse, application a une mesure en ligne de donnees de biomasse dans un processus de fermentation et procede de pilotage associe
FR2867279A1 (fr) * 2004-03-05 2005-09-09 Nanotec Solution Procede et dispositif pour mesurer et caracteriser une biomasse, application a une mesure en ligne de donnees de biomasse dans un processus de fermentation, et procede de pilotage associe
WO2006002452A1 (fr) * 2004-07-05 2006-01-12 Austria Wirtschaftsservice Gesellschaft mit beschränkter Haftung Procede et dispositif de spectroscopie raman
US9239036B2 (en) 2006-09-08 2016-01-19 Kimberly-Clark Worldwide, Inc. Ultrasonic liquid treatment and delivery system and process
US9283188B2 (en) 2006-09-08 2016-03-15 Kimberly-Clark Worldwide, Inc. Delivery systems for delivering functional compounds to substrates and processes of using the same
US7568251B2 (en) 2006-12-28 2009-08-04 Kimberly-Clark Worldwide, Inc. Process for dyeing a textile web
US8858892B2 (en) 2007-12-21 2014-10-14 Kimberly-Clark Worldwide, Inc. Liquid treatment system
US9421504B2 (en) 2007-12-28 2016-08-23 Kimberly-Clark Worldwide, Inc. Ultrasonic treatment chamber for preparing emulsions
WO2011006525A1 (fr) * 2009-07-13 2011-01-20 Foss Analytical A/S Analyse d'un liquide séparé par voie acoustique
US10245821B2 (en) 2015-12-04 2019-04-02 At&T Intellectual Property I, L.P. Reusable networked 3-D printing
US10647106B2 (en) 2015-12-04 2020-05-12 At&T Intellectual Property I, L.P. Reusable networked 3-D printing
EP3220131A1 (fr) 2016-03-17 2017-09-20 Commissariat À L'Énergie Atomique Et Aux Énergies Alternatives Procédé de caractérisation d'un échantillon liquide comportant des particules
FR3049062A1 (fr) * 2016-03-17 2017-09-22 Commissariat Energie Atomique Procede de caracterisation d’un echantillon liquide comportant des particules
US9921147B2 (en) 2016-03-17 2018-03-20 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for characterizing a liquid sample containing particles

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