EP0589363A1 - Procédé et dispositif de mélange automatique sans contact d'un mélange de réaction dans un dispositif d'analyse - Google Patents
Procédé et dispositif de mélange automatique sans contact d'un mélange de réaction dans un dispositif d'analyse Download PDFInfo
- Publication number
- EP0589363A1 EP0589363A1 EP93114983A EP93114983A EP0589363A1 EP 0589363 A1 EP0589363 A1 EP 0589363A1 EP 93114983 A EP93114983 A EP 93114983A EP 93114983 A EP93114983 A EP 93114983A EP 0589363 A1 EP0589363 A1 EP 0589363A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- vessel
- gas jet
- mixing element
- gas
- liquid surface
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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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
Definitions
- the invention relates to a method for the contactless automatic mixing of a liquid reaction mixture in an analysis device and a device for carrying out the method.
- the present invention is particularly suitable for so-called discrete analyzers, in which each individual analysis is carried out in a separate reaction vessel, which is in the Usually has a round (usually circular) cross-section, is transported in a vertical position through various processing stations of the device and is open at the top.
- the reaction vessel is fed computer-controlled with sample liquids and liquid reagents, the resulting reaction mixture is homogenized with the aid of a mixing device and after a predetermined reaction time, in many cases also after a multi-stage reaction in which several reagents are added in succession, one of the reactions of sample and Reagents resulting physically detectable measurable characteristic for the analysis determined.
- This measured variable can be, for example, a photometrically determinable extinction, a fluorescence signal or an electrochemical measured variable (voltage or current flow).
- the present invention is directed, regardless of the details of the method and the measured variable used for the detection, to automated analyzers of the most varied types, as long as they require the mixing of a reaction mixture in an elongated vessel with a vertical longitudinal central axis accessible from above through an opening.
- the discrete automatic analyzers mentioned largely mimic the processing steps known from manual analyzes with the aid of mechanical, hydraulic and electronic means. It is therefore not surprising that machines of this type were among the first devices for automatic analysis. Although numerous other types of automatic analyzers, such as centrifugal analyzers and continuous flow analyzers, were subsequently developed, the discrete analyzers have not lost their importance in the long term. Rather, from today's perspective, they are by far the most important Group of automated analyzers. This success is essentially due to the fact that discrete automatic analyzers enable a completely selective, sample-oriented mode of operation, ie an individual program of different analytes can be determined in succession for each sample.
- reaction vessel In order to avoid this so-called “carryover”, proposals have long been made to mix the reaction mixture in a reaction vessel without touching the reaction liquid (non-invasively). For example, cylindrical reaction vessels with mixing elements fixed to their base were used, which were quickly rotated back and forth in the mixing device. In another known device, the reaction vessel is sonicated with ultrasound in a liquid bath in order to achieve the required homogenization.
- the invention is based on the object of proposing a method and a device for automatically mixing a liquid reaction vessel in an analysis device which works without contact (non-invasively) and nevertheless enables the liquid to be mixed quickly, effectively and reliably.
- the object is achieved in a method in which the reaction mixture is located in a vessel accessible from above through an opening, with the aid of a gas jet emerging from an outlet opening of a mixing element, in which the mixing element is lowered in the direction of the liquid surface at the beginning of the mixing process and the lowering movement in a lower end position, in which the mixing element protrudes into the vessel,
- the liquid surface is not touched, stopped, the gas jet is switched on during the lowering of the mixing element, the gas jet is oriented in such a way that it causes an unsymmetrical lowering of a part of the liquid surface in the vicinity of the vessel wall and the gas jet has a tangential component of motion so that the lowered part of the liquid surface is set in rotation around the axis of the vessel.
- Air is expediently used as the mixed gas for cost reasons.
- the invention further relates to a device for carrying out the method, in which at least one and at most three gas jet outlet openings are provided in the vicinity of the lower end of the mixing element and are connected to a mixed gas source via a mixed gas line of the mixing element.
- the reaction mixture is rapidly mixed without the mixing element or the surroundings of the vessel being contaminated by the liquid.
- the lower end position in which the mixing element is stopped is selected so that the outlet opening of the gas jet is below the edge of the opening of the reaction vessel, but on the other hand the lower end of the mixing element does not touch the liquid surface.
- the gas jet should be offset radially with respect to the axis of the vessel, i.e. it should hit the liquid surface at a point between the axis of the vessel and the wall of the vessel, although it does not have to be directed directly at the surface of the liquid, but can also be directed at a flat angle to the vessel wall and from there strikes the area of the liquid surface close to the wall.
- the jet of the mixed gas is dimensioned in its strength and spatial extent so that it causes an asymmetrical lowering of part of the liquid surface. The “strength" of the jet depends on the speed of the gas molecules and their flow rate.
- the movement of the molecules of the gas jet has a rotational movement component, that is to say a movement component circulating around the longitudinal central axis of the vessel.
- the liquid is rapidly set into a circulating movement, with liquid layers lying below the asymmetrical lowering of the liquid surface being set into a substantially horizontally circulating movement with almost no delay.
- the lower liquid areas in the central area of the circulation rise in a spiral up and mix very quickly with the upper liquid areas.
- the beam is preferably directed in such a way that the radial distance of the deepest point of the asymmetrical depression from the wall is less than 10% of the largest vessel diameter.
- the rotational movement component of the gas jet can be achieved in that the mixing element rotates with the outlet opening of the gas jet in the lower end position (about an axis coaxial to the central axis of the vessel). According to an alternative preferred embodiment, however, it can also be generated by appropriate alignment of the end section determining the jet direction of the mixed gas line leading to the outlet opening.
- This end section is referred to below as the nozzle.
- this expression should not be understood to mean that the end section of the line must have a nozzle-shaped, tapering shape. Rather, it can be cylindrical in shape with a constant cross section.
- the mixing element 1 shown in FIG. 1 protrudes with its lower end 2 into a circular-cylindrical reaction vessel 4 accessible from above through an opening 3, the vertical longitudinal axis of which is designated by A. There is a liquid 6 to be mixed in the vessel 4.
- the mixing element 1 consists essentially of two coaxial tubes, namely an outer tube 8 and an inner tube 9.
- the walls of the outer tube 8 converge conically at the lower end 2 of the mixing element 1, so that the mixing element downwards (apart from in the wall 8a of the outer tube 8 existing holes, which serve as nozzles 12 and 13) is closed.
- the lower end of the inner tube 9 is sealed at the annular line of contact 10 to the inside of the wall 8a of the outer tube 9, so that the interior of the tube 9 is separated from the annular space between the tube 9 and the tube 8.
- the inner tube 9 serves as a mixed gas line 14, through which air is supplied from a mixed gas source 15 at a controllable pressure and, after passing through the nozzle 12, exits through an outlet opening 16.
- the annular space between the tubes 8 and 9 forms a line 18 which is separate from the mixed gas line 14 and which is connected to a gas source 19 in order to supply an additional gas stream which emerges from the outlet openings 20 through the bores 13 and - as will be explained in more detail below - serves as a protective gas.
- the gas sources 15, 19 and the connecting lines 15a, 19a to the mixing element 1 are only indicated symbolically. Suitable connection techniques, also in the case of a mixing element rotating about the vertical axis A, are known to the person skilled in the art.
- the mixing element 1 In order to homogenize the liquid 6 in the vessel 4, the mixing element 1 is moved vertically downward in accordance with the arrow 21 and lowered into the upper part of the vessel 4, so that at least the lower end 2 projects into the vessel.
- the lowering movement is stopped in a defined lower end position, which is selected such that the outlet openings 16 and 20 are located below the edge 3a of the opening 3 and the mixing element 1 does not touch the surface of the liquid 6.
- mixed gas is already supplied through line 14 and preferably also protective gas through line 18 and exits through outlet openings 16 and 20, respectively.
- this lowered shape of the liquid surface 22 is shown as a solid line, while the rest position of the liquid surface is shown as a dashed line 23.
- the gas jet emerging from the outlet opening 16 has a rotational component with respect to the longitudinal central axis A of the vessel 4, in the preferred case of a round vessel cross section, that is, a component tangential to the wall 5 of the vessel 4.
- the Nozzle 12 from which the mixed gas jet emerges runs radially (that is, without a directional component tangential to the vessel wall).
- FIG. 2 Such an embodiment is shown in FIG. 2.
- the tangential component of the gas jet movement is brought about by rotation of the mixing element 1 about the axis A.
- the rotation frequency should preferably be between 10 and 80 revolutions per minute, preferably between 20 and 30 revolutions per minute.
- the last section of the line of the mixed gas which determines the direction of the gas jet has a directional component tangential to a circle around the longitudinal central axis A of the vessel.
- Such an embodiment is shown in FIG. 3.
- FIGS. 2 and 3 also differ to the extent that only one outlet opening 16 is provided for the gas jet in FIG. 2, while FIG. 3 has three nozzles 12 ′ running obliquely with a tangential direction component with outlet openings 16 ′.
- the number of gas jet outlet openings is preferably between 1 and 3 regardless of the orientation of the nozzles.
- the mixing action occurs without the mixing element 1 being rotated, but of course both measures can also be combined, i.e. a mixing element with gas outlet openings according to FIG. 3 can also be set in rotation.
- the movement of the liquid 6 during the mixing process is characterized in that on the one hand the liquid surface 22 is lowered relatively asymmetrically and that on the other hand this lowering of the liquid surface is set into a rotational movement.
- the difference d between the highest point of the liquid surface and the lowest point of its lowered part is preferably at least 25%, particularly preferably at least 50% of the diameter of the liquid surface (in the case of a non-circular cross section of its largest diameter).
- the reduction naturally depends on the flow of the gas jet, the gas pressure in the line 14 and the diameter of the at least one gas jet outlet opening.
- the gas flow is preferably between 10 ml / S and 70 ml / S, particularly preferably between 20 ml / S and 60 ml / S.
- the diameter of the gas jet outlet openings 16 should preferably be between 0.1 and 0.8 mm, particularly preferably between 0.5 and 0.7 mm.
- the gas pressure is preferably between 1.2 bar and 1.7 bar.
- the nozzles are preferably oriented at an angle ⁇ between approximately 30 ° and approximately 60 ° to the axis A, an angle of approximately 45 ° having proven particularly useful.
- the additional outlet openings 20 are provided above the outlet openings 16, through which a second gas stream is supplied as a protective gas.
- the mixing element preferably has at least four such outlet openings 20, which form a ring which is uniformly distributed over the circumference of the mixing element 1.
- the shape of the lower end 2 is also essential for a good mixing action and for reducing the risk that the mixing element 1 is contaminated by splashes of the liquid 6 during the mixing process of the mixing element 1 in relation to the cross section of the vessel 4 (in its upper region 4a, into which the mixing element 1 projects).
- the largest horizontal cross-sectional area of the part of the mixing element 1 projecting into the vessel 4 in the lower end position should be at least 30% of the corresponding horizontal cross-sectional area of the vessel (measured at the same vertical height). It should be taken into account that the cross-sectional area to which this statement relates is square to the linear dimensions of the components.
- a ratio of the diameter of the mixing element 1 and the vessel 4 of 0.6: 1 corresponds to a cross section ratio of 0.36: 1.
- the cross section of the mixing element 1 should fill the vessel 4 relatively largely at least in a partial area of its height, so that only a considerably reduced cross section for the backflow of gas according to the arrows 25 past the mixing element 1 is available. As a result, the gas is stowed to a certain extent below the mixing element 1.
- the lower boundary surface 26 slopes outwards and upwards from a deepest point 26a as shown.
- the lower boundary surface is to be understood as the surface closing the mixing element 1 downwards, i.e. the surface of the mixing element 1 below its largest cross-section immersed in the vessel 4.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
- Automatic Analysis And Handling Materials Therefor (AREA)
- Mixers With Rotating Receptacles And Mixers With Vibration Mechanisms (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4232096A DE4232096A1 (de) | 1992-09-25 | 1992-09-25 | Verfahren und Vorrichtung zum berührungslosen automatischen Mischen eines Reaktionsgemisches in einem Analysegerät |
| DE4232096 | 1992-09-25 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0589363A1 true EP0589363A1 (fr) | 1994-03-30 |
| EP0589363B1 EP0589363B1 (fr) | 1996-03-27 |
Family
ID=6468788
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP93114983A Expired - Lifetime EP0589363B1 (fr) | 1992-09-25 | 1993-09-17 | Procédé et dispositif de mélange automatique sans contact d'un mélange de réaction dans un dispositif d'analyse |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US5362147A (fr) |
| EP (1) | EP0589363B1 (fr) |
| JP (1) | JP2524474B2 (fr) |
| DE (2) | DE4232096A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0643989A1 (fr) * | 1993-09-21 | 1995-03-22 | Roche Diagnostics GmbH | Procédé et système pour mélanger des liquides |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE29502594U1 (de) * | 1995-02-17 | 1995-04-06 | Arthur Eugster AG, Romanshorn | Mehrzweck-Aufschäumhilfe, insbesondere für Espressomaschinen |
| JP3567187B2 (ja) * | 1995-02-23 | 2004-09-22 | アークレイ株式会社 | 試料液等の撹拌装置 |
| TW529456U (en) * | 2002-06-27 | 2003-04-21 | Nanya Technology Corp | Pipeline for mixing |
| US8323984B2 (en) * | 2002-12-19 | 2012-12-04 | Beckman Coulter, Inc. | Method and apparatus for mixing blood samples for cell analysis |
| DE102004028303A1 (de) * | 2004-06-11 | 2005-12-29 | Roche Diagnostics Gmbh | Verfahren und Vorrichtung zum Nachweis von Analyten |
| WO2007063929A1 (fr) * | 2005-12-02 | 2007-06-07 | Wako Pure Chemical Industries, Ltd. | Appareil d’agitation de liquide et procede |
| IT1392463B1 (it) * | 2008-12-18 | 2012-03-09 | Nuova Simonelli S P A | Lancia eroga-vapore per macchine da caffe' elettriche. |
| JP5831857B2 (ja) * | 2012-01-24 | 2015-12-09 | 株式会社サンギ | 粉体分散装置、微粉体生成方法 |
| EP2838650B1 (fr) | 2012-04-18 | 2019-09-25 | Life Technologies Corporation | Procédés et appareil pour transfert de masse entre un flux de gaz et un liquide |
| JP7292195B2 (ja) * | 2019-12-06 | 2023-06-16 | 株式会社日立ハイテク | 自動分析装置 |
| CN113588350B (zh) * | 2021-09-28 | 2021-12-17 | 哈焊所华通（常州）焊业股份有限公司 | 蓄水池快速取样装置 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3398935A (en) | 1964-03-25 | 1968-08-27 | Bausch & Lomb | Mixing means |
| JPS5858471A (ja) * | 1981-10-02 | 1983-04-07 | Toshiba Corp | 自動生化学分析装置における撹拌装置 |
| JPS58137758A (ja) * | 1982-02-10 | 1983-08-16 | Omron Tateisi Electronics Co | 血液撹拌装置 |
| WO1985003571A1 (fr) | 1984-02-01 | 1985-08-15 | Hulette William C | Systemes et procedes d'analyse clinique |
| EP0176014A2 (fr) * | 1984-09-22 | 1986-04-02 | Eppendorf-Netheler-Hinz Gmbh | Procédé et dispositif pour mélanger un échantillon d'un liquide à analyser |
| WO1987006618A1 (fr) * | 1986-04-30 | 1987-11-05 | Baxter Travenol Laboratories, Inc. | Systemes et procedes d'analyse clinique ameliores |
| EP0281958A2 (fr) * | 1987-03-07 | 1988-09-14 | Hoechst Aktiengesellschaft | Dispositif de régulation de température et de mélange du contenu d'une plaque de micro titration |
| JPS63229134A (ja) * | 1987-03-18 | 1988-09-26 | Toshiba Corp | 検体検査装置における液体撹拌装置 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3531093A (en) * | 1968-03-26 | 1970-09-29 | Susanna Mikhailovna Karpacheva | Device for pulsating mixing of liquid reagents and liquid-and-solid reagents |
| US4390284A (en) * | 1980-01-25 | 1983-06-28 | Neptune Microfloc, Inc. | Method and apparatus for wetting powder |
| US4498819A (en) * | 1982-11-08 | 1985-02-12 | Conoco Inc. | Multipoint slurry injection junction |
-
1992
- 1992-09-25 DE DE4232096A patent/DE4232096A1/de not_active Withdrawn
-
1993
- 1993-09-17 DE DE59302034T patent/DE59302034D1/de not_active Expired - Fee Related
- 1993-09-17 EP EP93114983A patent/EP0589363B1/fr not_active Expired - Lifetime
- 1993-09-21 US US08/123,994 patent/US5362147A/en not_active Expired - Lifetime
- 1993-09-24 JP JP5238500A patent/JP2524474B2/ja not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3398935A (en) | 1964-03-25 | 1968-08-27 | Bausch & Lomb | Mixing means |
| JPS5858471A (ja) * | 1981-10-02 | 1983-04-07 | Toshiba Corp | 自動生化学分析装置における撹拌装置 |
| JPS58137758A (ja) * | 1982-02-10 | 1983-08-16 | Omron Tateisi Electronics Co | 血液撹拌装置 |
| WO1985003571A1 (fr) | 1984-02-01 | 1985-08-15 | Hulette William C | Systemes et procedes d'analyse clinique |
| EP0176014A2 (fr) * | 1984-09-22 | 1986-04-02 | Eppendorf-Netheler-Hinz Gmbh | Procédé et dispositif pour mélanger un échantillon d'un liquide à analyser |
| WO1987006618A1 (fr) * | 1986-04-30 | 1987-11-05 | Baxter Travenol Laboratories, Inc. | Systemes et procedes d'analyse clinique ameliores |
| EP0281958A2 (fr) * | 1987-03-07 | 1988-09-14 | Hoechst Aktiengesellschaft | Dispositif de régulation de température et de mélange du contenu d'une plaque de micro titration |
| JPS63229134A (ja) * | 1987-03-18 | 1988-09-26 | Toshiba Corp | 検体検査装置における液体撹拌装置 |
Non-Patent Citations (3)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN vol. 13, no. 24 (C - 561)<3372> 19 January 1989 (1989-01-19) * |
| PATENT ABSTRACTS OF JAPAN vol. 7, no. 146 (P - 206)<1291> 25 June 1983 (1983-06-25) * |
| PATENT ABSTRACTS OF JAPAN vol. 7, no. 253 (P - 235)<1398> 10 November 1983 (1983-11-10) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0643989A1 (fr) * | 1993-09-21 | 1995-03-22 | Roche Diagnostics GmbH | Procédé et système pour mélanger des liquides |
Also Published As
| Publication number | Publication date |
|---|---|
| US5362147A (en) | 1994-11-08 |
| JPH06194371A (ja) | 1994-07-15 |
| JP2524474B2 (ja) | 1996-08-14 |
| EP0589363B1 (fr) | 1996-03-27 |
| DE4232096A1 (de) | 1994-03-31 |
| DE59302034D1 (de) | 1996-05-02 |
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