WO2004099757A1 - Cuves a circulation faisant intervenir des techniques photometriques - Google Patents

Cuves a circulation faisant intervenir des techniques photometriques Download PDF

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Publication number
WO2004099757A1
WO2004099757A1 PCT/US2003/011281 US0311281W WO2004099757A1 WO 2004099757 A1 WO2004099757 A1 WO 2004099757A1 US 0311281 W US0311281 W US 0311281W WO 2004099757 A1 WO2004099757 A1 WO 2004099757A1
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WO
WIPO (PCT)
Prior art keywords
radiant energy
flow cell
tube
layer
fluid
Prior art date
Application number
PCT/US2003/011281
Other languages
English (en)
Inventor
Yuri Gerner
Carl Sims
Thomas J. Thielen
Original Assignee
Systec, Inc.
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 Systec, Inc. filed Critical Systec, Inc.
Priority to EP03723993A priority Critical patent/EP1616166A4/fr
Priority to PCT/US2003/011281 priority patent/WO2004099757A1/fr
Priority to AU2003230887A priority patent/AU2003230887A1/en
Priority to JP2004571629A priority patent/JP2006515421A/ja
Publication of WO2004099757A1 publication Critical patent/WO2004099757A1/fr

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    • 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
    • B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/0303—Optical path conditioning in cuvettes, e.g. windows; adapted optical elements or systems; path modifying or adjustment
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/05—Flow-through cuvettes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/02—Adapting objects or devices to another
    • B01L2200/026—Fluid interfacing between devices or objects, e.g. connectors, inlet details
    • B01L2200/027—Fluid interfacing between devices or objects, e.g. connectors, inlet details for microfluidic devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0832—Geometry, shape and general structure cylindrical, tube shaped
    • B01L2300/0838—Capillaries
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0861—Configuration of multiple channels and/or chambers in a single devices
    • B01L2300/0877—Flow chambers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/16—Surface properties and coatings
    • B01L2300/168—Specific optical properties, e.g. reflective coatings
    • 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
    • B01L3/56—Labware specially adapted for transferring fluids
    • B01L3/565—Seals
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N2021/0346—Capillary cells; Microcells
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/05—Flow-through cuvettes
    • G01N2021/052—Tubular type; cavity type; multireflective
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/0317—High pressure cuvettes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/06—Illumination; Optics
    • G01N2201/064—Stray light conditioning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/06—Illumination; Optics
    • G01N2201/064—Stray light conditioning
    • G01N2201/0642—Light traps; baffles
    • 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
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors

Definitions

  • the present invention relates to flow cells generally, and more particularly to radiant energy flow cells for use in various analytical chemistry applications, such as spectrophotometry .
  • This invention also relates to methods for fabricating such flow cells.
  • Flow cells have typically been utilized to transport liquid samples, but other flowable sample types have also been implemented.
  • flow cells have been implemented to transport sample solutions through a volume disposed between a radiant energy source and an energy detector, which detector measures the relevant energy absorption or transmission through the sample solution.
  • An example of such a detector is a spectrophotometer .
  • Various analytical instruments then interpret the resultant energy "fingerprints" or transmitted vs. absorbed wavelengths to decipher sample constituents.
  • the flow cell walls typically use focusing optics such that energy impact upon the flow cell walls is minimized.
  • focusing optics Without such focusing optics, previous flow cell configurations called for the sample solvating fluid to have a higher index of refraction than materials commonly used in the flow cell walls.
  • organic fluids were typically utilized as solvents in flow cell applications prior to the incorporation of focusing optics.
  • aqueous fluid carriers have been sought as a preferred alternative to such organic fluids.
  • a material having an index of refraction less than that of water is needed for the respective flow cells.
  • One such material is a perflourinated copolymer developed by DuPont of
  • analytical flow cells preferably include a layer of Teflon AF ⁇ or other low index of refraction material to allow efficient radiant energy propagation in spectrophotometry and photometry applications.
  • stray light is light which is perceived by the photometric detector without first passing through the sample being analyzed. Such stray light is most often a result of light transmitting directly through transparent or translucent flow cell material without passing through the sample path.
  • flow cell systems are specifically designed to maximize internal reflection of photometric radiation through the flow cell to the detector. Such systems simultaneously attempt to minimize source light from entering directly into an end of the flow cell wall to correspondingly minimize stray light reaching the detector.
  • mechanical photomasking devices have been implemented to block at least incoming light from entering an end of the flow cell wall. As flow cell systems become ever smaller, however, such mechanical photomasking devices become extremely difficult to effectively block stray light while allowing sample radiant energy transmission to pass therethrough into the core of the flow cell.
  • an improved flow cell is contemplated for use in transporting sample fluids in radiant energy fields.
  • Such a flow cell introduces a structure for improved fluid sealing and fluid flow characteristics.
  • One embodiment of the flow cell of the present invention preferably includes a cell structure having a first elongated tube disposed therein which forms a continuous passageway through the cell structure.
  • the tube includes a radiant energy-blocking portion integral therewith for minimizing passage of stray light through the tube.
  • Attached to the flow cell is at least one end cap that is sealingly engagable with the cell structure.
  • the end cap preferably includes a substantially conical frustum portion extending outwardly therefrom. When assembled, the conical frustum portion preferably extends at least partially into the first open channel.
  • a first open channel within the first tube is preferably clad with one or more layers forming concentric tubes.
  • the innermost tube is a low index of refraction material such as perfluorinated copolymer.
  • a second tube preferably comprising PEEK substantially concentrically surrounds the first tube.
  • a third tube comprising FEP substantially concentrically surrounds the PEEK tube, and is in intimate contact with an outer wall of the first open channel.
  • the conical frustum portion of the end caps preferably displace a portion of the FEP tube against the first open channel wall, thereby forming a fluid-tight seal between the FEP tube and the conical frustum portions .
  • the end caps include one or more open channels for transporting the sample fluid and the radiant energy.
  • the radiant energy channels are in substantial alignment with the first open channel within the cell structure.
  • the radiant energy channels and the fluid channels preferably merge such that the radiant energy may pass through the sample fluid.
  • At least one end of the innermost tube is preferably flared outwardly to more efficiently transport the radiant energy and sample fluid.
  • the flared portion of the innermost tube is calibrated so that an internal dimension of the innermost tube may be reduced without significant radiant energy losses, and further enables a reduction in fluid flow turbulence. Such reduced flow turbulence increases the reliability of photometric sample analysis.
  • a gap volume is provided between the first open channel within the cell structure and fluid channels within respective end caps.
  • the gap volume is preferably and adjustably calibrated to define an appropriate volume such that radiant energy losses among various fluids having distinct indexes of refraction may be standardized.
  • the present invention also contemplates a method for determining sample composition through radiant energy interaction with the sample fluid utilizing the structural elements described above.
  • FIG. 1 is a partially exploded cross-sectional view of a flow cell of the present invention.
  • FIG. 2 is a cross-sectional view of the flow cell shown in FIG. 1.
  • FIG. 3 is an enlarged cross-sectional view of the flow cell shown in FIG. 2.
  • FIG. 4 is a cross-sectional view of tubing including a radiant energy-blocking portion disposed along a length thereof.
  • FIG. 5 is a cross-sectional view of tubing having radiant energy-blocking portions disposed at respective end surfaces of the tubing.
  • FIGURE 1 a partially exploded cross-sectional view of a flow cell 10 of the present invention is shown.
  • Flow cell 10 includes cell body 12, and first and second end caps 14, 16 respectively.
  • Cell body 12 preferably includes a first open channel 18 extending therethrough to form a continuous passageway through a length of the cell body.
  • One or more distinct material layers preferably surround open channel 18.
  • Such layers preferably concentrically surround open channel 18, so as to form concentric tubes, an inside diameter of the innermost tube thereby defining open channel 18.
  • the concentricity of respective layers is preferably tightly controlled.
  • a first layer 20 of relatively low index of refraction material concentrically surrounds open channel 18.
  • a low refractive index material is desired for use in the first layer 20 so that radiant energy passing through sample fluids in channel 18 is able to propagate over relatively long distances with little deterioration.
  • Flow cell applications employing spectrophotometers or other instruments to analyze fluid composition require that the tube walls within which the fluid and radiant energy pass preferably possess an index of refraction less than that of the fluid to allow efficient propagation of the radiant energy (by a phenomenon known as full internal reflection) .
  • the internal wall material preferably has an index of refraction less than that of water.
  • first layer 20 preferably comprises a perfluorinated copolymer.
  • an inner surface of such first layer 20 is relatively free of imperfections, and any imperfections present are preferably smaller than the radiant energy wavelength.
  • first layer 20 is sufficiently thick to prevent radiant energy losses caused by radiant energy penetration through the first layer.
  • first open channel 18 of cell body 12 the radiant energy penetrates first layer 20 as an evanescent wave, the intensity of which decays exponentially with the depth of first layer 20.
  • the thickness "T" of first layer 20 should be larger than the penetration depth 'T" of the radiant energy incident thereon.
  • n ⁇ is the refractive index of first layer 20
  • ni is the refractive index of the sample fluid
  • Q is the wavelength of the incident radiant energy
  • i is the radiant energy angle of incidence into channel 18.
  • first layer 20 has a thickness of at least two wavelengths of the respective radiant energy passing through open channel 18. Most preferably, first layer 20 is at least 15 Thx thick.
  • first layer 20 is tubular in form, and preferably forms the boundary defining a course of travel for fluid and radiant energy through cell body 12.
  • second and third layers 22, 24, respectively are disposed concentrically around first layer 20.
  • Second and third layers 22, 24 are preferably polymeric materials, and are preferably tubular in form.
  • second layer 22 is PEEK
  • third layer 24 is FEP.
  • second layer 22 is interposed between first layer 20 and third layer 24, and may be in intimate contact with both first layer 20 and third layer 24.
  • clearance between first, second, and third layers, respectively, is maintained at no greater than 2% of an inner dimension of channel 18.
  • third layer 24 is substantially concentrically surrounded by the remainder of cell body 12, which is preferably a rigid, non-corrodable material such as stainless steel. Other materials, however, may be used in place of the exemplary stainless steel.
  • First and second end caps 14, 16 preferably include at least one open channel extending therethrough.
  • Second open channel 26 is preferably disposed in first end cap 14, and is preferably in alignment with first open channel 18.
  • a third open channel 30 is disposed in end cap 16, and is in alignment with channel 18.
  • second and third open channels 26 and 30 preferably extend through an entire length of end caps 14 and 16 respectively.
  • channels 26, 30 are utilized for transporting radiant energy through flow cell 10, and are desirably disposed in a single plane to eliminate measurement errors which could result from various angled reflection characteristics.
  • channels 26, 30 are fabricated from a material efficient in transporting radiant energy, such as, for example, fiber optic material.
  • a particularly preferred material for use in channels 26, 30 is a quartz fiber optic.
  • channels 26, 30 are in a direct, straight-line alignment with channel 18.
  • first, second, and third layers 20, 22, 24, respectively, are substantially in concentric alignment with channels 26, 30, and have an offset of no greater than 5% of an inner dimension of channel 18.
  • photomasking is utilized to minimize or block stray light passing through flow cell 10 without passing through the sample fluid.
  • radiant energy is directed through open channels 30, 18, and 26, respectively.
  • open channel 18 is preferably mechanically aligned with channels 30 and 26 such that radiant energy may pass directly through the channel without scattering beyond respective boundaries thereof, a portion of the emitted radiation may undesirably pass through one or more of layers 20, 22, and 24 without passing through the sample fluid within channel 18. Most typically, however, any such stray light not passing through the sample fluid between channels 30 and 26 passes through layer 20.
  • layer 20 is preferably manufactured from a perfluorinated copolymer such as Teflon AF for particular index of refraction characteristics. To overcome the difficulties associated with mechanically masking relatively small flow cell applications, layer 20 is preferably impregnated or coated with light blocking material.
  • a preferred embodiment of the present invention includes an opaque portion 72 disposed in layer 20.
  • Light blocking portion 72 may preferably be disposed along an entire length of layer 20, as shown in FIGURE 4. In other embodiments, however, light blocking portion 72 may be disposed at only portions of layer 20 as deemed necessary per particular applications .
  • light blocking portion 72 is preferably spaced from an inner surface 19 of layer 20, such that a non-opaque layer 74 is formed between inner surface 19 and light blocking portion 72.
  • a non-opaque layer 74 is preferably incorporated into flow cell 10 so that radiant energy incident upon inner surface 19 of layer 20 may be received and efficiently reflected or refracted therefrom without significant energy losses. Since radiant energy typically penetrates materials a small degree prior to being reflected or refracted, a non-opaque portion such as layer 74 is preferably provided to minimize absorption of radiant energy incident upon inner surface 19. The depth of penetration of incident radiant energy is dependent upon the material utilized in layer 20.
  • non-opaque layer 74 has a thickness of at least about two wavelengths of the respective radiant energy passing through open channel 18.
  • the thickness of layer 74 is preferably determined by the relationship defined above.
  • Layer 74 is preferably integral with light blocking portion 72, though layer 74 and portion 72 may alternatively be distinct layers disposed immediately adjacent to one another, wherein such adjacent layers may preferably be chemically bonded to one another. In other embodiments, however, such adjacent layers may be juxtaposed adjacent one another without having chemical bonding therebetween.
  • light blocking portion 72 includes a colorant such as carbon black.
  • a variety of light blocking colorants may be incorporated into portion 72, although carbon has been found to be particularly advantageous when used in combination with perfluorinated copolymer materials in first layer 20.
  • Another light-blocking colorant useful in the present invention is titaniumdioxide (Ti0 2 ) .
  • the carbon is preferably suspended or dispersed into a perfluorinated copolymer solution at a concentration of between about 0.01-2% by weight carbon. More preferably, the carbon loading is between about 0.1-1% by weight in the perfluorinated copolymer solution.
  • a particular carbon material preferred for use in the present invention is manufactured by Cabot® under the trade name Elftex 12.
  • light blocking portion 72 is formed from a polymeric solution including the desired colorant material.
  • perfluorinated copolymer such as Teflon AF may be dissolved in a commercially available solvent such as AusimontTM HT-55 or 3M® FC-75. Powdered carbon may then be suspended or dispersed directly into the perfluorinated copolymer solution to form a light blocking polymeric material.
  • One method for forming layer 20 of the present invention provides for extruding the light blocking solution over a preformed tube defined by layer 74.
  • the perfluorinated copolymer in light blocking layer 72 preferably chemically bonds to the perfluorinated copolymer of non- opaque layer 74 to form a continuous first layer 20.
  • An alternative method for forming layer 20 includes dipping a preformed tube defined by layer 74 into the carbon-loaded perfluorinated copolymer solution such that layer 72 is formed in surrounding relationship to layer 74.
  • Layer 72 preferably chemically bonds to layer 74 to form an integral layer 20 having a light-blocking portion 72.
  • the initial tube 74 may be formed by dipping surface-modified fiber optic tubing into a solution of perfluorinated copolymer, and subsequently removing the fiber optic tubing from within the now-formed perfluorinated copolymer tube 74.
  • Such surface modification may include coating the fiber optic tubing with a stable, non-binding compound such as a poly-imide material .
  • a preferred method for forming layer 20 having a light-blocking portion 72 integral therewith is through a single-step extrusion process.
  • a polymeric solution such as perfluorinated copolymer in an appropriate solvent, having between about 0.01 and about 2% by weight carbon suspended or dispersed therein may be extruded over a pin to form a tube of desired dimensions. It has been determined that such a single-step extrusion process extruding a carbon-loaded polymeric material such as perfluorinated copolymer preferably forms an inner portion 74 substantially free of the carbon or other light-blocking material. In such a manner, a single extruded tube having a light-blocking portion 72 in substantially surrounding relationship with a colorant- free portion 74 may be efficiently manufactured through such a single-step extrusion process.
  • a particular example of this method includes direct mixing in a screw-type extruder.
  • the perfluorinated copolymer is dry-mixed with an appropriate amount of carbon or other opaquing material, and subsequently fed into the extruder.
  • the carbon is coated with the perfluorinated copolymer, thus forming a layer during the tubing extrusion process.
  • the extruded tubing includes a layer of a few wavelengths or more of pure perfluorinated copolymer.
  • Light blocking portion 72 may also be incorporated into second layer 22 and third layer 24 as desired. Similar methods for impregnating the respective layers with light blocking colorant may be utilized.
  • pigment-loaded solution as described above may be coated onto end surfaces 21 of first layer 20 to minimize stray light from passing therethrough.
  • Light blocking material 82 may therefore be "painted” on surfaces which may be exposed to radiant energy.
  • Material 82 preferably acts as a block to incoming radiant energy, whereby incident radiant energy is directed through open channel 18.
  • Light blocking material 82 is preferably the same as that used in light blocking portion 72, and may be applied to layers other than, or in addition to first layer 20 as desired.
  • Light blocking layer 82 is preferably sufficiently thick to inhibit incident radiant energy from passing therethrough.
  • a fluid channel 28 is disposed in end cap 14, and extends from said second channel 26 to an exterior surface of end cap 14. As shown in FIGURE 1, fluid channel 28 preferably extends through an entire dimension of end cap 14 such that fluid may flow between an exterior surface of end cap 14 and open channel 18 through fluid channel 28. Walls defining fluid channel 28 may be the same material as end cap 14, or may be lined or coated with a different material that may be desired for particular applications .
  • end cap 16 is preferably similar to end cap 14.
  • End cap 16 preferably includes a third open channel 30 extending therethrough in a plane coincident with a plane associated with open channel 18.
  • end cap 16 preferably includes a fluid channel 32 extending from such third open channel 30 to an exterior surface of end cap 16, thereby providing a flow duct for fluid to pass between open channel 18 and the exterior of end cap 16.
  • a preferred feature of the embodiment depicted in FIGURE 1 is the protrusion 40 extending from the respective end caps 14, 16. Protrusions 40 are adapted to be received in cell body 12 such that a fluid seal is formed at an interface between the cell body and the respective end caps 14, 16.
  • Second and third open channels 26, 30, respectively, preferably extend through protrusions 40 such that respective openings to the second and third open channels are disposed in respective outer surfaces of the protrusions 40.
  • protrusions 40 substantially form conical frustum portions extending from respective end caps 14, 16.
  • second and third open channels 26, 30 preferably extend through the frustum portions of said protrusions 40.
  • first layer 20 is flared outwardly.
  • the flared section of first layer 20 is preferably formed by inserting a highly polished heated conical structure into channel 18 defined by first layer 20.
  • first layer 20 comprises Teflon AF ⁇
  • the conical structure is heated to a temperature near a Teflon AF ⁇ glass transition point (240°C) , but under the melting point for Teflon F ⁇ .
  • the heated conical structure therefore forms a portion of first layer 20 to an exterior surface shape of the conical structure.
  • first layer 20 is flared to alter an inner dimension of open channel 18 such that fluid may pass to and from open channel 18 more efficiently.
  • the flared section of first layer 20 reduces fluid flow turbulence in channel 18, thereby providing a higher degree of laminar flow. Since fluid flow turbulence causes dispersion in radiant energy passing through the fluid, a reduction in flow turbulence desirably reduces "scattering noise" in photometric analyses of radiant energy transmission, and therefore results in increased spectrophotometric accuracy.
  • an end section 50 of first layer 20 is flared outwardly such that an inner dimension of open channel 18 at end section 50 is substantially equal to a respective inner dimension of open channel 26.
  • an inner dimension of open channel 18 may be correspondingly reduced.
  • Such reduction in the internal dimension of open channel 18 correspondingly reduces an inner dimension of first layer 20, which allows a smaller internal volume of open channel 18, thereby reducing sample band spreading in the channel without significant reduction in radiant energy transmission through open channel 18.
  • flared section 50 of first layer 20 enables the reduction of an internal dimension of first layer 20 to less than that of open channel 26 without significant radiant energy losses, due to the angle of inflection between open channel 26 and flared section 50 of channel 18.
  • Such minimum radiant energy loss is possible so long as the flared portion angle combined with the radiant energy angle of incidence is smaller than a radiant energy acceptance angle T.
  • Such an acceptance angle T may be determined by the following relationship, where NA is the numerical aperture of channel 18, n f is the refractive index of the sample fluid, and n f i is the refractive index of the first layer.
  • Outwardly flared section 50 of first layer 20 is preferably sealingly in intimate contact with a chamfered portion 52 of second layer 22.
  • protrusion 40 preferably outwardly displaces a portion of third layer 24 against cell body 12. Such outward displacement creates a latent expansion force in compressed portion 54 of third layer 24. This expansion force preferably assists in securing protrusion 40 in place, and acts to form a fluid seal between protrusion 40 and third layer 24.
  • Protrusions 40 are illustrated in FIGURE 3 as having a generally conical frustum shape, and extending substantially perpendicularly from respective end caps 14, 16. Such a conical frustum shape is preferred for providing desired alignment and sealing characteristics.
  • Conical frustum portions 42 of respective protrusions 40 preferably firmly seat against first layer 20 and displace a portion of the third layer when the respective end caps 14, 16 are assembled to cell body 12 to form flow cell 10. Such displacement provides a relatively high-pressure fluid seal between third layer 24 and protrusion 40.
  • Such a high-pressure seal preferably withstands fluid pressure of up to 2000-3000 pounds per square inch.
  • the engagement of frustum portions 42 in cell body 12 provides a high-pressure fluid seal at an interface between layers 22 and 24.
  • Frustum portions 42 are preferably arranged to linearly align open channel 18 with respective second and third open channels 26, 30.
  • the flow cell of FIGURES 1-3 is preferably formed by providing the end caps as described above and a cell body having an open bore extending therethrough.
  • a section of Teflon AF tubing is selected for use as the first layer within the open bore.
  • the Teflon AF tube may be formed through an extrusion process or any other process that effectively creates such tubing.
  • the Teflon AF tube section is then preferably positioned within a section of PEEK tubing, which PEEK tubing forms the second layer within the open bore.
  • the PEEK tube section is in intimate contact with the Teflon AF tube.
  • An inner surface of at least one end portion of the PEEK tube section is preferably chamfered outwardly to form a generally conical end portion.
  • a heated cone is subsequently inserted a desired distance into a corresponding portion of the Teflon AF tube to flare such Teflon AF tube section outwardly against the chamfered portion of the outwardly-disposed PEEK tube.
  • the combination PEEK/Teflon AF (PT) tube section is then cut to a precision length in such a manner so as to form a clean cut edge having little or no edge distortions or burrs .
  • a section of FEP tubing is cut to a length which is longer than the PT tube section, and the PT tube section is inserted therein, thereby forming a multiple-layered tube section.
  • the multi-layered tube section is then inserted into the open bore in the cell body.
  • the FEP tube section is heated to a point at which the material is somewhat pliable.
  • the heated tube section is then stretched and thinned, and pulled through the open bore of the cell body, and subsequently cut to a desired length.
  • the PT tube section is inserted into the FEP tube section to thereby form a multi-layered tube assembly within the cell body.
  • the PT tube section is friction fit within the FEP tube section.
  • the respective end caps are engaged to the cell body such that the protrusions extend at least partially into the open bore.
  • the protrusions 40 displace a portion of the FEP layer against the cell body, thereby forming a fluid- tight seal between respective protrusions 40 and the FEP layer 24, and between PEEK layer 22 and FEP layer 24.
  • the multi-layered tube assembly is effectively secured between respective end caps 14, 16, and within cell body 40.
  • open channel 18, defined by an inner dimension of the Teflon AF is in alignment with respective second and third open channels 26, 30 to allow efficient fluid and radiant energy flow through flow cell 10.
  • a gap 60 is preferably left between conical frustum portion 42 of end cap 14 and a respective end of channel 18.
  • sample fluid fills gap 60, thereby resulting in calculatable radiant energy losses as the radiant energy passes through the fluid-filled gap which is absent the efficient radiant energy transmitting first layer 20.
  • radiant energy entering gap 60 is allowed to disperse throughout the volume defined by gap 60, causing partial diffusion or loss of the radiant energy. Fluids having relatively higher refractive indexes result in greater degree of radiant energy loss as compared to fluids having relatively lower refractive indexes.
  • Such radiant energy losses may be calculated by the following relationship:
  • E is the radiant energy loss
  • a is the distance between conical frustum portion 42 of end cap 14 and channel 18, defined as gap 60
  • NA is the numerical aperture of channel 18
  • D is an internal dimension of channel 18
  • nf is the refractive index of the respective sample fluid.
  • a typical range for gap 60/channel 18 inner dimension ratio (a/D) is between about 0.1 and about 1.0.

Abstract

Cette invention concerne une cuve à circulation (10) assurant le transport d'un liquide dans un champ d'énergie rayonnante, qui comprend un corps de cuve (12) traversé par un tube (20),auquel est intégré une partie de blocage de l'énergie. Dans un mode de réalisation particulier, le corps de cuve (12) comprend un ou plusieurs chapeaux d'extrémité (14, 16) présentant une partie saillante (40) qui peut s'insérer dans le tube (20) et créent un joint d'étanchéité pour le liquide. Ces chapeaux comportent des canaux ouverts par où passent le liquide (28, 32) et l'énergie radiante (26, 30). Le tube (20) du corps de cuve (12) comporte une chemise assurant une transmission efficace de l'énergie rayonnante. Cette chemise, qui se trouve à l'écart des parties saillantes de couvercle (40), forment un volume intercalaire dans le canal ouvert (18) de la cuve de circulation, lequel volume peut être étalonné pour que les pertes d'énergie rayonnante puisent être normalisées dans des cuves de circulation qui transportent des liquides aux indices de réfraction différents.
PCT/US2003/011281 2003-04-07 2003-04-07 Cuves a circulation faisant intervenir des techniques photometriques WO2004099757A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP03723993A EP1616166A4 (fr) 2003-04-07 2003-04-07 Cuves a circulation faisant intervenir des techniques photometriques
PCT/US2003/011281 WO2004099757A1 (fr) 2003-04-07 2003-04-07 Cuves a circulation faisant intervenir des techniques photometriques
AU2003230887A AU2003230887A1 (en) 2003-04-07 2003-04-07 Flow cells utilizing photometric techniques
JP2004571629A JP2006515421A (ja) 2003-04-07 2003-04-07 測光技術を使用するフローセル

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2003/011281 WO2004099757A1 (fr) 2003-04-07 2003-04-07 Cuves a circulation faisant intervenir des techniques photometriques

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JP (1) JP2006515421A (fr)
AU (1) AU2003230887A1 (fr)
WO (1) WO2004099757A1 (fr)

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CN110940669A (zh) * 2019-11-21 2020-03-31 安徽益佳通电池有限公司 一种锂电池极片端面毛刺测试装置及方法
WO2021056445A1 (fr) * 2019-09-27 2021-04-01 深圳华大智造科技有限公司 Cuve à circulation et dispositif à réaction pour substance biochimique utilisant la cuve à circulation

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JP7180760B2 (ja) * 2019-04-24 2022-11-30 株式会社島津製作所 クロマトグラフィ検出器用フローセルおよびクロマトグラフィ検出器

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JP2006515421A (ja) 2006-05-25
AU2003230887A1 (en) 2004-11-26
EP1616166A4 (fr) 2008-07-09
EP1616166A1 (fr) 2006-01-18

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