EP0643989B1 - Procédé et système pour mélanger des liquides - Google Patents

Procédé et système pour mélanger des liquides Download PDF

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Publication number
EP0643989B1
EP0643989B1 EP94114512A EP94114512A EP0643989B1 EP 0643989 B1 EP0643989 B1 EP 0643989B1 EP 94114512 A EP94114512 A EP 94114512A EP 94114512 A EP94114512 A EP 94114512A EP 0643989 B1 EP0643989 B1 EP 0643989B1
Authority
EP
European Patent Office
Prior art keywords
mixing element
liquid
mixing
vessel
gas
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.)
Expired - Lifetime
Application number
EP94114512A
Other languages
German (de)
English (en)
Other versions
EP0643989A1 (fr
Inventor
Hans Dr. Schels
Karl-Heinz Mann
Horst Menzler
Leonhard Geissler
Georg Kuffer
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.)
Roche Diagnostics GmbH
Original Assignee
Roche Diagnostics GmbH
Boehringer Mannheim GmbH
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 Roche Diagnostics GmbH, Boehringer Mannheim GmbH filed Critical Roche Diagnostics GmbH
Publication of EP0643989A1 publication Critical patent/EP0643989A1/fr
Application granted granted Critical
Publication of EP0643989B1 publication Critical patent/EP0643989B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/40—Mixers using gas or liquid agitation, e.g. with air supply tubes
    • B01F33/407—Mixers using gas or liquid agitation, e.g. with air supply tubes by blowing gas on the material from above
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/21—Measuring
    • B01F35/211—Measuring of the operational parameters
    • B01F35/2112—Level of material in a container or the position or shape of the upper surface of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/22—Control or regulation
    • B01F35/2201—Control or regulation characterised by the type of control technique used
    • B01F35/2209—Controlling the mixing process as a whole, i.e. involving a complete monitoring and controlling of the mixing process during the whole mixing cycle
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/23—Mixing of laboratory samples e.g. in preparation of analysing or testing properties of materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/11—Automated chemical analysis
    • Y10T436/119163—Automated chemical analysis with aspirator of claimed structure
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
    • Y10T436/25625—Dilution

Definitions

  • the invention relates to a method for mixing a Liquid with another liquid or solid by blowing air onto the surface of the liquid, and a system for performing the method.
  • Chemical and medical analyzes are often performed using equipment carried out a quick, targeted and consistent Allow treatment of a variety of samples. in the This not only makes comparison to manual procedures a cost reduction but also an improved reliability and accuracy of the analyzes achieved.
  • Discrete analyzers where every single analysis in one separate reaction vessel is carried out.
  • the vessels are through the analytical equipment transported, substances are added or removed, the contents of the vessel are mixed and the contents of the vessel become a measuring method, for example photometry or potentiometry subjected.
  • the analysis vessel is attached to a Ultrasound source coupled and the contents of the vessel through Ultrasound mixed. Mix this way often does not run completely and also has the disadvantage that many substances, especially larger organic ones Molecules that can be destroyed.
  • Patent application WO-A-85 03571 describes a mixing process described in which the liquid in an analysis vessel is mixed by inflating air.
  • Figure 10 of this Registration shows that a nozzle is located above the edge of the vessel becomes. A liquid is ejected through the Air jet is prevented by a defined fluid level is set. This method has the Disadvantage that precautions have to be taken in order to to ensure defined liquid level.
  • the invention was based on the object, a method and a To propose a system for mixing a liquid, which works without procrastination and is fast, effective and enables reliable mixing of the liquid.
  • Another object of the invention is a method to provide with the regardless of fluid volume and Vessel shape ensures extensive mixing can be.
  • the invention also relates to a system for Mixing a liquid with at least one other Liquid or with at least one solid that is a vessel with the substances to be mixed, a mixing element, a Detection device, a device for moving the Mixing element and a control unit.
  • a method according to the invention relates above all not exclusively on mixes in clinical Analysis equipment.
  • the liquid to be mixed is located in the analysis apparatus usually in cylindrical Vessels with a round or square cross-section, the are open to the top.
  • a liquid with at least another liquid or with at least one solid be mixed.
  • Liquids in this sense can for example analysis samples or reagent solutions, as well Be washing and auxiliary solutions.
  • sample solutions Liquids, such as water samples, urine, blood, Understood saliva etc.
  • mixing liquids does not necessarily have to have a phase boundary. Mixing may also be desirable when mixable liquids successive pipetting into a common Vessel were put together, as a rule by the Combining does not result in complete mixing.
  • mixing a liquid with a solid usually the purpose is that the solid in the liquid dissolves.
  • a mixing element from which a gas jet emerges onto the surface of the liquid moved in the analysis vessel.
  • gas from the mixing element during the movement process is generally used as the gas for cost reasons.
  • gases for example inert gases, can also be used.
  • a detection takes place during the movement of the mixing element, whether contact of the mixing element with the liquid surface is reached.
  • the detection can for example through an optical system from outside the reaction vessel respectively.
  • Particularly advantageous can the mixing element mechanically with a detection device be coupled. Detection of the liquid surface is commonly referred to as "liquid level detection”.
  • the invention uses the different liquid levels detection "known method to ensure thorough mixing Inflation of air to open up another area of application and improve their functioning. According to the invention this is done by coupling a mixing element with a detection device.
  • the mixing element is removed from the liquid removed as soon as contact with the liquid is detected has been.
  • Detection device and mixing element are mechanical connected with each other, but offset in height, so can over the Height offset of the distance of the mixing device from the Liquid surface to be regulated. In this case it is not necessarily an additional movement of the mixing element necessary from the surface.
  • the vessels are preferably not completely filled with liquid filled so that a margin of several millimeters to a few Withstands centimeters. If a mixing element is brought into the vessel, so this results in a narrowing of the vessel, what when the gas flow is switched on to a congestion effect and thus to reduce the risk of splashing of the liquid leads.
  • the or the gas jets emerging from the mixing element can surface in different ways Liquid. Possible types of targeting are exemplified below for a single gas jet described.
  • the gas jet can be radial to the vessel axis offset at a point between the vessel axis and the vessel wall hit the liquid surface, taking it not immediately must be directed towards the surface of the liquid, but also aimed at the vessel wall at a flat angle can be and from there indirectly to the area close to the wall strikes the liquid surface.
  • the gas jet can also be aligned so that the escaping gas Performs rotational movement around the axis of the vessel. By this arrangement will be near-surface areas of the liquid also set in a circulating movement, whereby deeper layers of liquid are almost instantaneous be moved and thus a quick mixing is achieved becomes.
  • a non-contact measurement of the distance between the surface of the liquid and mixing element takes place on optical way.
  • Most of the analysis vessels are out optically permeable material, as a rule optical measurements are made in the analysis solutions.
  • optical sensors for example map an optical array.
  • the mixing element After the foam layer has been displaced, the mixing element continue to approach the liquid surface and the true liquid surface is detected.
  • the mixing element is removed from the surface by a predetermined amount and gas preferably inflated from additional nozzles.
  • the described methods can be carried out using a method for Combination detection can be combined. It is for Example possible to irradiate the liquid and the Constancy of a measured value, e.g. B. the light absorption as To use the criterion of thorough mixing.
  • a system according to the invention can also be equipped with a device for dispensing liquids, e.g. B. a pipetting device, be coupled.
  • a device for dispensing liquids e.g. B. a pipetting device
  • a particularly favorable combination results when a pipetting device is in a Mixing element is integrated.
  • a vessel in the context of the invention has at least one Opening.
  • a mixing element in the sense of the invention has at least an outlet opening for a gas jet.
  • Preferably owns the mixing element also has further outlet openings, also called nozzles. It is not necessarily under the nozzle a conically narrowing outlet opening means but also such openings that have a constant diameter have.
  • cylindrical analysis vessels has an inventive Mixing element itself also essentially cylindrical shape with a diameter smaller than that of the analysis vessel.
  • the nozzles of the mixing element are preferably located on the side facing the liquid of the mixing element. The nozzles can move against the axis of the Mixing element be inclined and / or tangential components to the axis of the mixing element. Are an advantage several nozzles, preferably 3, which are at a height of Mixing element are.
  • nozzles are attached to a wreath that is farther from the surface than the first sentence Nozzles.
  • This arrangement ensures that the gas flow is stowed in the analysis vessel, which is a detachment of Suppresses droplets from the liquid.
  • the Also part of the mixing element facing the analysis vessel be rotatable.
  • a particularly preferred arrangement results when a nozzle is firmly under a tangential An angle of 45 ° is arranged and above this nozzle Wreath of 8, also at 45 ° axially attached nozzles is available.
  • Preferred diameters of the nozzles are included 0.3 to 0.7 mm, with 0.4 to 0.6 mm being particularly preferred are.
  • Preferred volume flows are 4-11 liters per Minute.
  • Moving the mixing element towards the liquid surface can with devices known in the prior art, for example a spindle drive.
  • FIG. 1 schematically shows a system (1) according to the invention for mixing liquids.
  • the system (1) is a capacitive measuring principle.
  • the mixing element (2) provides one pole of the measuring arrangement, while the second pole (3) located outside on the wall of the vessel (4).
  • a Touching the tip (5) of the mixing element (2) with the Liquid surface leads to a change in capacity between the mixing element (2) and the second pole (3) by the Evaluation and control device (6) is processed.
  • the Evaluation and control device (6) controls both Motor (7) and a pump (8).
  • the motor (7) moves over a rack the mixing element (2) relative to the surface the liquid (9).
  • Air is pumped in with the pump (8)
  • the air passes through a nozzle (11) which is about 40 ° against the Liquid surface is inclined from the mixing element out.
  • the mixing element (2) is initially in a starting position above the liquid.
  • the evaluation and Control device sets the pump (8) in motion so that a weak air flow is promoted.
  • the mixing element (2) is by driving the motor (7) slowly on the Liquid surface moved and this movement stopped, as soon as a Touching the tip (5) of the mixing element with the Liquid surface is detected.
  • the mixing element (2) is moved 2 mm away from the liquid surface and the Pump (8) controlled so that a volume flow of 5 l / min through the nozzle (11).
  • FIG. 2A shows a longitudinal section through a mixing element (20).
  • the metal body (21) of the mixing element (20) an inner tube (22), the opening of which is perpendicular to the longitudinal axis the mixing element is arranged.
  • This inner tube (22) is suitable to blow foam away.
  • the mixing element (20) has a feed pipe (23) which opens into a nozzle (24).
  • the Nozzle (24) forms one with the longitudinal axis of the mixing element 45 ° angle. With air emerging from the nozzle (24) liquids can be mixed.
  • Figure 2B shows the cross section of a mixing element (30) tangentially arranged nozzles.
  • a longitudinal tube (31) to blow foam away can.
  • This longitudinal tube (31) has three nozzles each surround two heights of the longitudinal axis.
  • Tangential nozzles (32) of the first set have an inclination against the longitudinal axis of the Mixing element, d. that is, emerging from the tangential nozzles (32) Gas hits at an angle to that Surface normal to the liquid surface.
  • the Set of vertical nozzles (33) is further from the Tip of the mixing element removed. From these nozzles escaping gas forms a back pressure in the mixing vessel, which a splash of liquid when mixing suppressed.
  • FIG 3 is the time course of mixing shown.
  • a cylindrical analysis vessel (diameter 1 cm, height 4 cm) 10 ul of ink were added and 1000 ul Water layered.
  • the mixing was carried out with a Mixing element that has 3 tangential holes (diameter 0.5 mm) is at a distance of 6 mm from the liquid surface and a volume flow of 8.4 l / min. 9 mm above the bottom of the vessel was with a photodiode and a receiver performed a color measurement.
  • Figure 3 is plotted on the abscissa the time that the Mixing element was operated and the resulting on the ordinate Color the solution. From the graphic it can be seen that complete mixing is achieved after approx. 2.5 s is.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Mixers With Rotating Receptacles And Mixers With Vibration Mechanisms (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Claims (9)

  1. Procédé pour mélanger un liquide avec au moins un liquide de plus ou bien avec au moins un solide dans un récipient accessible par une ouverture constitué de matière optiquement transparente avec au moins un jet gazeux sortant d'un élément mélangeur, qui comprend les étapes consistant:
    (a) à déplacer l'élément mélangeur en direction de la surface du liquide,
    (b) à mesurer la distance entre l'élément mélangeur et la surface du liquide,
    (c) à terminer le déplacement de l'élément mélangeur lorsqu'une distance prédéterminée entre l'élément mélangeur et la surface du liquide est atteinte,
    (d) à insuffler un gaz provenant de l'élément mélangeur sur la surface du liquide, de manière à mettre le liquide en mouvement;
    caractérisé en ce que la mesure de la distance s'effectue de manière optique à partir de l'extérieur du récipient au moyen d'un dispositif.
  2. Procédé selon la revendication 1, dans lequel l'élément mélangeur contient des dispositifs qui servent à introduire des liquides dans le récipient.
  3. Procédé selon la revendication 1, dans lequel la distance prédéterminée entre l'élément mélangeur et la surface du liquide vaut de 3 à 6,5 mm.
  4. Procédé selon la revendication 1, dans lequel un gaz est insufflé à partir d'un élément mélangeur en direction de la surface du liquide, pour déplacer de la mousse ou des substances se trouvant sur le liquide.
  5. Procédé selon la revendication 1, dans lequel l'insufflation du gaz n'est pas interrompue entre-temps.
  6. Procédé selon la revendication 1, avec une étape qui comporte une détection d'un mélange.
  7. Appareillage pour mélanger un liquide avec au moins un liquide de plus ou avec au moins un solide, qui comporte les éléments suivants:
    (a) un récipient constitué de matière optiquement transparente, qui contient les substances à mélanger et qui possède au moins une ouverture,
    (b) un élément mélangeur, qui possède au moins une buse par laquelle un jet gazeux peut sortir,
    (c) un dispositif pour mesurer la distance entre la surface de liquide et l'élément mélangeur,
    (d) un dispositif pour déplacer l'élément mélangeur en direction de la frontière des phases et pour l'éloigner de celle-ci,
    (e) un dispositif d'analyse et de commande, avec lequel le positionnement de l'élément mélangeur et la sortie du gaz de l'élément mélangeur sont commandés en se basant sur les signaux du dispositif de détection et en tenant compte d'un plan de déroulement de programme,
    caractérisé en ce qu'un dispositif se trouve à l'extérieur du récipient pour mesurer optiquement la distance.
  8. Appareillage selon la revendication 7, dans lequel l'élément mélangeur possède une buse avec une ouverture perpendiculaire à l'axe longitudinal de l'élément mélangeur et au moins une buse de plus, dont l'ouverture est inclinée par rapport à l'axe longitudinal de l'élément mélangeur.
  9. Appareillage selon la revendication 7, dans lequel l'élément mélangeur possède un jeu de buses, dont les ouvertures sont orientées pour l'essentiel perpendiculairement à l'axe longitudinal de l'élément mélangeur et qui sont plus éloignées de la pointe de l'élément mélangeur que les buses déjà citées.
EP94114512A 1993-09-21 1994-09-15 Procédé et système pour mélanger des liquides Expired - Lifetime EP0643989B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4331997A DE4331997A1 (de) 1993-09-21 1993-09-21 Verfahren und System zur Mischung von Flüssigkeiten
DE4331997 1993-09-21

Publications (2)

Publication Number Publication Date
EP0643989A1 EP0643989A1 (fr) 1995-03-22
EP0643989B1 true EP0643989B1 (fr) 1998-12-09

Family

ID=6498170

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94114512A Expired - Lifetime EP0643989B1 (fr) 1993-09-21 1994-09-15 Procédé et système pour mélanger des liquides

Country Status (5)

Country Link
US (1) US5780306A (fr)
EP (1) EP0643989B1 (fr)
JP (1) JP2883819B2 (fr)
DE (2) DE4331997A1 (fr)
ES (1) ES2125387T3 (fr)

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CN103575659B (zh) * 2013-11-01 2016-01-13 合肥金星机电科技发展有限公司 一种用于对烟道中烟气进行检测的装置
WO2020257963A1 (fr) * 2019-06-24 2020-12-30 深圳迈瑞生物医疗电子股份有限公司 Dispositif d'étalement et procédé de coloration d'échantillons

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Also Published As

Publication number Publication date
EP0643989A1 (fr) 1995-03-22
JP2883819B2 (ja) 1999-04-19
DE59407433D1 (de) 1999-01-21
DE4331997A1 (de) 1995-03-23
ES2125387T3 (es) 1999-03-01
US5780306A (en) 1998-07-14
JPH07155581A (ja) 1995-06-20

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