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WO2013091118A1 - Procédé et dispositif d'analyse d'échantillons contenant de petites particules - Google Patents

Procédé et dispositif d'analyse d'échantillons contenant de petites particules Download PDF

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Publication number
WO2013091118A1
WO2013091118A1 PCT/CH2012/000274 CH2012000274W WO2013091118A1 WO 2013091118 A1 WO2013091118 A1 WO 2013091118A1 CH 2012000274 W CH2012000274 W CH 2012000274W WO 2013091118 A1 WO2013091118 A1 WO 2013091118A1
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WO
WIPO (PCT)
Prior art keywords
sample liquid
particles
nozzle
characteristic
channel
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/CH2012/000274
Other languages
English (en)
Inventor
Markus Michler
David Bischof
André Bernard
Andres HELDSTAB
Ruedi OBERHOLZER
Klaus Dietrich
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.)
NANOTION AG
Original Assignee
NANOTION AG
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 NANOTION AG filed Critical NANOTION AG
Publication of WO2013091118A1 publication Critical patent/WO2013091118A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1404—Handling flow, e.g. hydrodynamic focusing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • 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
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1456—Optical investigation techniques, e.g. flow cytometry without spatial resolution of the texture or inner structure of the particle, e.g. processing of pulse signals
    • G01N15/1459—Optical investigation techniques, e.g. flow cytometry without spatial resolution of the texture or inner structure of the particle, e.g. processing of pulse signals the analysis being performed on a sample stream
    • 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
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N2015/1486—Counting the particles
    • 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
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N2015/1493—Particle size
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/718—Laser microanalysis, i.e. with formation of sample plasma

Definitions

  • the invention relates to the analysis of liquids containing small particles, more particularly to the detection of small particles in liquids by laser-induced breakdown detection (LIBD). It relates more specifically to the determination of sizes and/or concentrations of nanoparticles in solutions.
  • LIBD laser-induced breakdown detection
  • the invention relates to methods and apparatuses according to the opening clauses of the claims. Such methods and apparatuses find application, e.g., in potable water analysis and in contamination detection.
  • WO 00/106993 Al From WO 00/106993 Al is known a method for determining the size of particles in a solution.
  • the method is based on the principle of laser-induced breakdown detection (LIBD) and allows to determine particle sizes. This is achieved by generating plasma emissions and detecting the plasma emissions in a spatially resolved manner and representing the plasma emissions in a location-frequency diagram which is a function of particle size, and comparing the location-frequency diagram with location-frequency diagrams of solutions containing particles of known size. From this, particles sizes can be determined.
  • LIBD laser-induced breakdown detection
  • US 7,679,743 Al an apparatus and method for measuring the size of nanoparticles present in an aqueous solution based on laser-induced breakdown is presented. Using calibration curves, the size of the nanoparticles can be determined.
  • EP 1 918 694 Al relates to the detection of changes in a population of particles in a solution, based on laser-induced breakdown detection.
  • laser-induced breakdown spectroscopy is applied to the determination of FeO(OH) in water.
  • plasma light is detected in a direction perpendicular to the direction of incidence of an exciting laser beam, and the sample solution is provided in an open jet, a sheath of gas surrounding this open jet.
  • DLS dynamic light scattering
  • LIBS spectroscopy
  • One object of the invention is to create an improved way of providing a sample liquid to be examined. Even more specifically, an improved way of creating an open jet suitable for use in a method for determining a characteristic of a sample liquid comprising particles shall be provided, and in second aspect of the invention, an improved way of creating an air curtain (or more generally a gas sheath) shall be provided.
  • a nozzle and a nozzle device and an arrangement shall be provided, as well as a method for manufacturing a nozzle.
  • Futhermore shall be provided a method for determining a characteristic of a sample liquid comprising particles and an apparatus for determining a characteristic of a sample liquid comprising particles and a use of a nozzle.
  • a method for determining a characteristic of a sample liquid comprising particles and an apparatus for determining a characteristic of a sample liquid comprising particles and an arrangement for use in such an apparatus or method shall be provided.
  • Another object of the invention is to create an improved way of carrying out LIBD and more particularly to create an improved way of providing a sample liquid to be examined by means of LIBD.
  • Another object of the invention is to create an improved way of carrying out LIBS and more particularly to create an improved way of providing a sample liquid to be examined by means of LIBS.
  • Another object of the invention is to create an improved way of carrying out DLS and more particularly to create an improved way of providing a sample liquid to be examined by means of DLS.
  • Another object of the invention is to provide a way of producing a well-defined open jet.
  • Another object of the invention is to provide a way of producing a particularly small open jet.
  • Another object of the invention is to provide a way of producing a particularly stable open jet.
  • Another object of the invention is to provide a nozzle being well manufacturable.
  • Another object of the invention is to provide a nozzle manufacturable with excellent reproducibility.
  • Another object of the invention is to provide a way of carrying out with high precision a method for determining a characteristic of a sample liquid comprising particles, in particular dynamic light scattering (DLS) or laser-induced breakdown detection (LIBD), or more particularly laser-induced breakdown spectroscopy (LIBS).
  • Another object of the invention is to provide a way of carrying out with high sensitivity for the detection small particles a method for determining a characteristic of a sample liquid comprising particles, in particular DLS or LIBD, or more particularly LIBS.
  • Another object of the invention is to provide a way of carrying out a method for determining a characteristic of a sample liquid comprising particles, in particular DLS or LIBD, or more particularly LIBS, in such a way that it requires little maintenance.
  • Another object of the invention is to provide a way of simply and/or quickly adjusting an apparatus for determining a characteristic of a sample liquid comprising particles, in particular an DLS or LIBD or, more specifically an LIBS apparatus, to different kinds of sample liquid.
  • Another object of the invention is to provide a way of simply and/or quickly exchanging a nozzle for producing an open jet of a sample liquid.
  • the method for determining a characteristic of a sample liquid comprising particles comprises the steps of a) producing an open jet of said sample liquid; wherein step a) is carried out using a nozzle according to the invention.
  • the method can comprise the steps of c) irradiating said sample liquid in said open jet by means of a pulsed light beam focused into said open jet; and d) obtaining a signal by detecting a breakdown of at least one of said particles; wherein said characteristic is obtainable from said signal.
  • the nozzle is a nozzle suitable for use in a method or an apparatus for determining a characteristic of a sample liquid comprising particles, and the nozzle comprises
  • said method or apparatus is a method or apparatus for determining a characteristic of a sample liquid comprising particles by irradiating sample liquid in an open jet of said sample liquid by l o means of a pulsed light beam focused into said open jet and obtaining a signal by
  • Said characteristic usually is a characteristic relating to said particles. More particularly, said characteristic comprises at least one of a size of said particles and a concentration 15 of said particles; e.g., a mean size of the particles; a concentration of said particles; a size distribution of said particles; and/or a concentration of those of said particles having a size in a pre-determined size range.
  • Said sample liquid usually either is a specimen to be examined or is a liquid containing specimen to be examined, e.g., a solution of specimen to be examined, e.g., based on 20 water or on another solvent.
  • Said particles are usually nanoparticles.
  • this designates particles having a volume of at most 1 ⁇ , and in particular of at least 1 nm . More specifically, nanoparticles are particles having a maximum linear extension of at most 1 ⁇ , and in particular at least 1 nm.
  • Another way of interpreting the term nanoparticles is to let it 5 designate particles measuring in at least one dimension at most 100 nm, and more
  • said light is laser light.
  • Laser light can readily provide energy densities large 5 enough for creating a breakdown of nanoparticles. The breakdown generates a plasma.
  • the plasma can be detected, e.g., photosensitively, acoustically or otherwise.
  • the plasma is detected by detecting the absorption of light of a light pulse of said pulsed light beam. Therein, the absorption takes place because inducing a plasma absorbs energy.
  • a detector e.g., a i o pyroelectrical detector, can be used which is positioned for the detection of radiation propagating in the direction of the light pulses.
  • an apparatus is set-up in such a way that the center of the focus of the pulsed light beam is inside the open jet.
  • the method comprises the step of b) producing a sheath of a gas surrounding said open jet.
  • step b) can in particular comprise the step of bl) guiding said gas along a gas path to a gas outlet at which said sheath of said gas emerges, wherein an area of a cross-section experienced by said gas flowing along said gas path reduces along said gas path.
  • a sheath of gas can protect equipment close to the location where the breakdown takes place (and the plasma is formed) from contamination.
  • a lens for focusing the pulsed light beam into the open jet and/or a lens for collecting radiation propagating from the open jet can be protected from spillings caused by the plasma.
  • a gas sheath can contribute to avoiding or minimizing contamination of sample fluid in the open jet and to stabilizing the open jet.
  • the described particular way of generating the sheath of gas can make possible to create a particularly homogeneous and a particularly stable sheath of gas.
  • said gas can flow along said gas path along which it enters a first section having a first cross- sectional area and, subsequently thereto, enters a second section having a second cross- sectional area, wherein said first cross-sectional area is larger than said second cross- i o sectional area.
  • said gas outlet describes, in cross-section, a closed shape, e.g., a ring shape, wherein elliptic or rectangular shapes or also other shapes are generally possible, too.
  • an extension of said channel in a direction parallel to a propagation direction of said pulsed light beam is, at said open end, at most 3 mm, more particularly at most 1 mm, even more particularly at most 500 ⁇ , but it can even be provided that said extension of said channel in a direction parallel to a propagation direction of said pulsed light beam is, at said open end, at most 200 ⁇ , more
  • a lower limit for said extension of said channel in a direction parallel to a propagation direction of said pulsed light beam is 1 ⁇ .
  • an extension of said channel in a direction parallel to a propagation direction of said pulsed light beam is, at said open end, at most two times, more particularly at most 1.2 times a confocal parameter b of said focused pulsed light - Si -
  • an extension of said channel in a direction parallel to a propagation direction of said pulsed light beam is, at said open end, at least 0.05 times, more particularly at least 0.2 times a confocal parameter b of said focused pulsed light beam.
  • an extension of said channel at said open end is, in a direction perpendicular to a propagation direction of said pulsed light beam and perpendicular to a direction of flow of said sample liquid in said open jet, at most 3 mm, l o more particularly at most 1 mm, even more particularly at most 500 ⁇ , but it can even be provided that an extension of said channel at said open end is, in a direction perpendicular to a propagation direction of said pulsed light beam and perpendicular to a direction of flow of said sample liquid in said open jet, at most 200 ⁇ , more particularly at most 100 ⁇ , even more particularly at most 50 ⁇ . Vibrations and
  • an extension of said channel at said open end along said first direction is between 0.5 times and 2 times, more particularly between 0.7 and 1.5 times an extension of said channel at said open end along said second direction.
  • step d) is replaced by the step of
  • said channel comprises a trench in said first member. It is optionally also possible to provide a trench in said second member contributing to said channel.
  • the i o latter way of forming the channel requires a precise alignment of the first and second members in order to obtain a properly shaped channel.
  • a way of precisely and reproduceably manufacturing said trench is to make use of etching, in particular using a lithographic process.
  • said first member - at least in the region where said trench is formed - is made of a crystalline semiconductor material, this can allow to
  • said channel is of substantially rectangular cross-section, at least in the region of said open end.
  • elliptic, circular, triangular or other cross- 20 sectional shapes are possible.
  • the method for manufacturing a nozzle can be a method for manufacturing a nozzle suitable for use in an apparatus for determining a characteristic of a sample liquid comprising particles and in particular is a method for manufacturing a nozzle according to the invention.
  • the method comprises the steps of
  • said method can, more specifically be a method for manufacturing a nozzle suitable for use in an apparatus for determining a characteristic of a sample liquid comprising particles by irradiating a sample liquid in an open jet of said sample liquid by means of a pulsed light beam focused into said open jet and obtaining a signal by detecting a breakdown of at least one of said particles.
  • the fixing addressed in step D) can be accomplished, e.g., using a bonding technique, e.g., gluing.
  • the first and second members are usually substantially plate-shaped, e.g., wafers, wherein wafer materials are not limited to semiconductor materials, e.g., also glass materials and other materials are possible.
  • step C) is replaced by the step of C) forming a multitude of trenches in said first member; and step D) is replaced by the step of
  • step E) separating said stack into at least two parts and thereby separating each of said multitude of channels into two separate channels. and/or the step of F) separating said stack into a multitude of nozzles each comprising one channel; in particular, and if step E) is carried out, each comprising one of said channels obtained in step E).
  • nozzles can be produced in high quality in large numbers.
  • 5 step E it can be possible to obtain high-precision nozzles, more precisely nozzles having well-defined open ends.
  • step E) and/or step F) may be accomplished, e.g., by laser cutting or using a wafer saw or otherwise.
  • the nozzle device according to the invention comprises a nozzle according to the i o invention and at least one plug part attached to said nozzle, in particular a first and a second plug part, said first plug part attached to said first member and said second plug part attached to said second member.
  • the nozzle device can form a plug, in particular a plug-in connector. This can facilitate replacing nozzles. Adjusting an apparatus such as an LIBD, DLS or LIBS apparatus to sample liquids of different properties such as 15 different viscosity, is thus greatly facilitated.
  • the nozzle device describes, in a plane parallel to said interface between said first and second members, a silhouette describing a waist. This can contribute to producing a sheath of gas of particularly good quality.
  • a width of a portion of said silhouette adjacent to said waist and located 20 between said waist and the location of said open end is smaller than a width of another portion of said silhouette adjacent to said waist and located on a side of said waist opposite to that side where said open end is located. This way, a stable and
  • the arrangement according to the invention comprises a nozzle according to the 25 invention and a top portion and a base portion, said top portion and said base portion being fixed with respect to each other in a distance from each other.
  • said top portion forms a socket for accepting a nozzle device according to the invention.
  • sample liquid having passed the region where the irradiation with light pulses takes place can be drawn off and, if a gas sheath is provided, also gas of a sheath of gas can be drawn off there.
  • the nozzle In the top part, the nozzle can be held in a well- defined position. And in an open space between top and bottom part, sample liquid in the open jet can be irradiated by the pulsed light beam. All required inlets and outlets 5 can be provided by the arrangement.
  • it can furthermore comprise i o — a light source unit for irradiating a sample liquid in an open jet of said sample liquid emerging from said open end of said nozzle by means of a pulsed light beam focused into said open jet; and
  • a detecting unit for detecting a breakdown of at least one of said particles.
  • the apparatus comprises
  • the light source unit usually comprises a light source, e.g., a laser operable in pulsed mode. And in addition, it usually also comprises at least one lens for focusing a light beam produced by said light source. Futhermore, it usually comprises means of
  • the apparatus comprises an evaluation unit for obtaining said characteristic from said signal produced by said detecting unit.
  • Said detecting unit can 25 be or comprise, e.g., a pyroelectric detector or a photosensitive detector such as, e.g., a photo diode, a photo element, a photomultiplier tube, an amplified photomultiplier tube. If breakdowns are detected by detection of light emitted as a result of the breakdown, the detected light usually is of a wavelength range not including a wavelength range of said pulsed light beam.
  • Fig. 1 a schematic illustration of an LIBD apparatus
  • Fig. 2 a schematic illustration of a detail of an LIBD apparatus
  • FIG. 3 a schematized cross-section through a nozzle
  • Fig. 4 a schematized cross-section through a nozzle
  • Fig. 5 a semi-transparent perspective view a nozzle with attached sample inlet
  • Fig. 6 an illustration of a top view onto a channel
  • Fig. 7 a schematic illustration of top view onto a wafer for manufacturing nozzles
  • Fig. 8 a side view a constituent of a nozzle device
  • Fig. 9 a side view two constituents of a nozzle device
  • Fig. 10 a schematic cross-section through a nozzle device
  • Fig. 11 a schematic cross-section through a nozzle device
  • Fig. 12 a front view of an arrangement
  • Fig. 13 a side view of a cross-section through an arrangement
  • Fig. 14 a perspective view of a cross-section through an arrangement.
  • Fig. 1 shows schematic illustration of an LIBD apparatus.
  • LIBD stands for laser- induced breakdown detection.
  • a breakdown of a small particle, usually a nanoparticle is detected, and this is usually carried out for a multitude of particles in a liquid sample.
  • LIBS light emitted because of the breakdown of a particle is spectrometrically analyzed.
  • Such methods are referred to as LIBS.
  • the LIBD apparatus illustrated in Fig. 1 comprises a light source LQ capable of producing light pulses (the produced light being referenced as 5), typically a pulsed laser, and two lenses LI, L2 each of which, of course, may comprises more than one lens elements, and a detector D.
  • One or more of various possible detection principles 5 known in the art can be implemented in detector D.
  • An evaluation unit 8 is
  • Sample liquid may contain a specimen to be investigated, e.g., in an 1 o aqueous solution.
  • an open jet J also referred to as "free jet" of sample liquid S is produced which furthermore is surrounded by a sheath V of a gas G.
  • the light beam produced in light source LQ is focused by lens LI into open jet J.
  • a sufficiently high energy density provided by the light pulses is present in sample liquid S in open jet J
  • particles in sample liquid S can be subject to breakdown and thus convert into a plasma and, accordingly emit light and also sound waves. If the breakdown shall be detected by detecting the light or the sound waves originating from the plasma, detector D would usually not have to be arranged in the light path described 20 by the light emitted by light source LQ. But another way of detecting a breakdown of a particle in an arrangement as illustrated in Fig. 1 is to detect a drop in intensity of light produced in light source LQ and having passed open jet J.
  • a light pulse having induced a breakdown of a particle in open jet J will comprise less energy than a light pulse having traversed open jet J without doing so.
  • This way of detecting breakdowns of 25 particles does not require the presence of a spatially resolving detector such as an array (image) detector.
  • Detector D will, accordingly, be positioned in the light path of the light 5 emitted by light source LQ having traversed lens L2, as illustrated in Fig. 1.
  • Fig. 2 is a schematic illustration of a detail of an LIBD apparatus. Like in Fig. 1 and in other Figures of the present patent application, a coordinate system is sketched for showing the orientation of the respective Figure.
  • the pulses of light 5 propagate in the direction of the (positive) x axis, and the sample liquid S in open jet J flows in the
  • the beam of light 5 has its focus.
  • a region in which the energy density of light 5 is sufficiently high for inducing a breakdown of nanoparticles in open jet J is referenced 5 and known as effective focus volume E.
  • the length of the effective focus volume E is referenced F.
  • zR is the Rayleigh range.
  • length F is not necessarily larger than depth of focus b.
  • the energy density required for inducing a breakdown in a smaller particle (having a smaller volume) is, at least usually, larger than the energy density required for inducing a breakdown in a larger
  • effective focus volumes E are preferably defined for particles of a certain size or volume.
  • the effective volume E (and the corresponding length F thereof) for a smaller particle therefore is smaller than for a larger particle.
  • said thickness of the open jet in x-direction is at least 0.2 times or rather 0.4 times the confocal parameter b.
  • Fig. 3 shows a cross-section through a nozzle N which can be used for creating open jets in LIBD apparatuses, e.g., like described in conjunction with Figs. 1 and 2.
  • the nozzle N comprises or even substantially consists of two members Ml, M2 which form an interface 4 at which a channel C is present.
  • Members Ml , M2 are, e.g., of plate shape, and are usually, at least at their surfaces contributing to interface 4, substantially flat.
  • a trench T contributes to channel C, trench T being formed in member Ml .
  • Channel C can be, as illustrated in Fig. 3, of rectangular cross-section with a depth t (usually in x-direction) and width B (usually in y-direction). Other cross-sectional shapes are possible. Depths t are typically below 200 ⁇ , more particularly at most 5 100 ⁇ and in many cases at most 50 ⁇ or even below at most 30 ⁇ . Such small dimensions in the direction of the propagation of the exciting light 5 can result in a particulary high sensitivity to particularly small particles.
  • Fig. 4 shows, in the same manner as Fig. 3, a cross-section through another nozzle N which can be used for creating open jets in LIBD apparatuses, e.g., like described in l o conjunction with Figs. 1 and 2.
  • This is to illustrate another possible cross-sectional shape (elliptic, which could also be round) and to show that it is possible to provide that a trench Tl in member Ml and, in addition, a trench T2 in member M2 can contribute to channel C.
  • a polymer material or a semiconductor material can be used for each member Ml , M2, e.g., glass.
  • a semiconductor material or glass can be particularly suitable, whereas for a member in which no trench 20 contributing to channel C shall be present, glass can be a particularly good choice.
  • Fig. 5 is a semi-transparent perspective view a nozzle N with attached sample inlet 1 1.
  • Channel C can be formed, e.g., like illustrated in Fig. 3 and has open end El at which a fine (thin) open jet can emerge when sample liquid is injected at sample inlet 1 1 at a closed end E2.
  • a through-hole can be 25 provided in member M2 which allows sample liquid to traverse member M2 and enter channel C.
  • Open end El is located at an edge face of nozzle N. Open end El is located at a side face of first member M 1 and, at least possibly, at a side face of second member M2.
  • sample liquid in an open jet avoids problems that may occur when sample liquid is present in a container, e.g., plasmas emerging at container walls, contamination of container walls and the like.
  • Using an open jet can make it possible to carry out LIBD in-line measurements in an elegant and stable, reproduceable way, e.g., for in-line 5 quality control.
  • Fig. 6 illustrates a top view onto a channel C, the small insert in Fig. 6 illustrating a cross-section through channel C at line A-A.
  • a through- hole in one member typically the one not having a trench contributing to channel C
  • the cross-sectional i o area of channel C reduces.
  • the cross-sectional area of channel C remains at least substantially constant.
  • the depth of the trench T can remain constant, such that a variation of the cross-sectional area of channel C can be accomplished by varying the width B of channel C.
  • Fig. 7 is a schematic illustration of top view onto a wafer or member Ml ' for
  • nozzles e.g., nozzles of the above-described kind.
  • several members Ml like described above may be manufactured using one semiconductor wafer, e.g., a silicon wafer or a glass wafer.
  • Trenches T for a plurality of nozzles can be etched into member ⁇ , e.g., using processes such as lithographic processes well- known in semiconductor industry.
  • Separating member M 1 ' into a plurality of members 20 Ml each comprising one trench can take place along the directions indicated by the dashed arrows, e.g., using a wafer saw or by laser cutting. At El ', the locations where open ends El will be located are indicated.
  • Figs. 8 and 9 show in a side view constituents of a nozzle device.
  • the drawings are to scale.
  • the nozzle device comprises a nozzle, in particular a nozzle of the above-described kind.
  • a nozzle can be provided, e.g., by gluing parts PI , P2 onto the outer sides of the nozzle.
  • Such a nozzle device can function as a plug facilitating changing nozzles in an apparatus for LIBD. And, in addition, it can contribute to producing a gas sheath around the open jet, e.g., an air curtain.
  • the gas can be air, in particular ambient air.
  • the nozzle device has sections si , s2, s3 which, in case of the prevailingly rotationally symmetric geometry, have different diameters dl , d2, d3.
  • a plug-like nozzle device can be inserted (plugged) into a top portion 1 of a arrangement shown in Figs. 12 to 14, that top portion 1 functioning a socket for the nozzle device 10.
  • Figs. 10 and 1 1 show a schematic cross-section through a nozzle device 10 at least similar to the one illustrated in Figs. 8 and 9.
  • Figs. 12 to 14 illustrate an arrangement for use in an LIBD apparatus, e.g., like described above, with inserted nozzle member 10.
  • Fig. 12 is a front view
  • Fig. 13 a side view of a cross-section
  • Fig. 14 a perspective view of a cross-section.
  • the drawings are to scale.
  • Nozzle device 10 comprising nozzle N is plugged into top portion 1 having an inner diameter d4 (cf. Figs 10, 11) substantially identical to and possibly smaller (by play) than outer diameter d3 (cf. Fig. 9) of nozzle device 10 in section s3 (cf. Fig. 8).
  • Diameter d2 is smaller than d3, and diameter dl is even smaller than d2, thus presenting 5 for gas injected into gas inlet 14 (cf. Fig. 13), cross-sectional areas along the path along nozzle device 10 to a gas outlet 15 which reduce, as is also visible from Figs. 10 and 1 1.
  • nozzle device 10 forms a waist, and farther down in the gas path, at section s2, the cross-section through which the gas flows is smaller than at the waist. A consequence of this is that the distribution of gas in the gas sheath over the
  • diameters in sections si and s2 are at least substantially identical and to design the inner diameters of top portion 1 accordingly, forming a reducing cross-section before gas outlet 15.
  • other cross-sectional shapes of the gas path i.e. not ring-shaped ones are generally possible, e.g., elliptic shapes, triangular shapes, rectangular shapes, possibly with rounded corners
  • Sample liquid S is injected in sample liquid inlet 11 , enters channel C through a
  • the gas of the gas sheath enters base portion 2 of the arrangement (cf. Figs. 12 to 14), usually together with sample liquid having passed the region E' where the effective focus volume is when in operation.
  • Gas G and/or sample liquid S can alternatively or additionally leave through a bottom opening 16 in base portion 2.
  • Top portion 1 and base portion 2 are distanced from each other, e.g., by a mechanical connection 3 like shown in Figs. 12 to 14, so as to provide space in which the focused light beam can interact with the sample liquid S.

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  • 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)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

L'invention concerne une buse pouvant être utilisée dans un dispositif permettant de déterminer une caractéristique d'un échantillon liquide comprenant des particules par irradiation de l'échantillon liquide dans un jet libre dudit échantillon liquide au moyen d'un faisceau lumineux pulsé concentré sur ledit jet libre et d'obtenir un signal par détection d'une rupture d'au moins l'une desdites particules, ladite caractéristique pouvant être obtenue par ledit signal. La buse comprend un premier élément et un second élément, lesdits premier et second éléments étant fixés l'un à l'autre, et un canal étant formé à une interface entre les premier et second éléments. Le canal possède une extrémité d'ouverture pour laisser émerger ledit jet libre. L'agencement comprend une partie supérieure dans laquelle la buse est introduite et une partie de base. Une enveloppe gazeuse entoure le jet libre.
PCT/CH2012/000274 2011-12-22 2012-12-17 Procédé et dispositif d'analyse d'échantillons contenant de petites particules Ceased WO2013091118A1 (fr)

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CH20362011 2011-12-22
CH2036/11 2011-12-22

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CZ305788B6 (cs) * 2014-07-22 2016-03-16 Vysoké Učení Technické V Brně Způsob analýzy kapalin, zejména kapalných suspenzí pomocí spektroskopie laserem indukovaného plazmatu a zařízení pro jeho provádění
JP2016165708A (ja) * 2015-03-03 2016-09-15 水ｉｎｇ株式会社 被処理水の膜閉塞性の評価方法、膜処理装置およびその運転方法
WO2016158443A1 (fr) * 2015-03-27 2016-10-06 東京エレクトロン株式会社 Dispositif de mesure de particules
EP3415896A4 (fr) * 2016-02-12 2019-09-25 Femto Deployments Inc. Dispositif de génération de film liquide et cartouche de film liquide utilisée dans celui-ci

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Cited By (6)

* Cited by examiner, † Cited by third party
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CZ305788B6 (cs) * 2014-07-22 2016-03-16 Vysoké Učení Technické V Brně Způsob analýzy kapalin, zejména kapalných suspenzí pomocí spektroskopie laserem indukovaného plazmatu a zařízení pro jeho provádění
JP2016165708A (ja) * 2015-03-03 2016-09-15 水ｉｎｇ株式会社 被処理水の膜閉塞性の評価方法、膜処理装置およびその運転方法
WO2016158443A1 (fr) * 2015-03-27 2016-10-06 東京エレクトロン株式会社 Dispositif de mesure de particules
JPWO2016158443A1 (ja) * 2015-03-27 2018-01-18 東京エレクトロン株式会社 微粒子計測装置
EP3415896A4 (fr) * 2016-02-12 2019-09-25 Femto Deployments Inc. Dispositif de génération de film liquide et cartouche de film liquide utilisée dans celui-ci
US10724941B2 (en) 2016-02-12 2020-07-28 FEMTO Deployments, Inc. Liquid membrane forming device and liquid membrane cartridge used therein

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