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WO2000047976A1 - Procédé de chauffage pour évaporateurs - Google Patents

Procédé de chauffage pour évaporateurs Download PDF

Info

Publication number
WO2000047976A1
WO2000047976A1 PCT/GB2000/000279 GB0000279W WO0047976A1 WO 2000047976 A1 WO2000047976 A1 WO 2000047976A1 GB 0000279 W GB0000279 W GB 0000279W WO 0047976 A1 WO0047976 A1 WO 0047976A1
Authority
WO
WIPO (PCT)
Prior art keywords
fluid
particles
containers
evaporator
pseudo
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/GB2000/000279
Other languages
English (en)
Inventor
Michael Cole
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.)
Genevac Ltd
Original Assignee
Genevac Ltd
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
Priority claimed from GBGB9902746.8A external-priority patent/GB9902746D0/en
Priority claimed from GBGB9918831.0A external-priority patent/GB9918831D0/en
Priority claimed from GBGB9926569.6A external-priority patent/GB9926569D0/en
Application filed by Genevac Ltd filed Critical Genevac Ltd
Publication of WO2000047976A1 publication Critical patent/WO2000047976A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L7/00—Heating or cooling apparatus; Heat insulating devices

Definitions

  • This invention concerns stationary and rotational evaporators, such as centrifugal and vortex evaporators.
  • sample holders such as glass tubes containing liquid are spun around in a vacuum chamber.
  • the centrifugal force acting on the liquid samples not only retains the latter in the tube which typically is pivoted so that they occupy a non-vertical attitude during rotation.
  • the centrifugal force can also assist in preventing unwanted boiling and spitting as the liquids evaporate under the reducing pressure.
  • a vortex evaporator typically consists of a vacuum chamber in which liquid samples, generally containing dissolved solids, are held in containers such as glass tubes, which in turn are frequently held in racks in heated aluminium blocks and subjected to orbital motion. This motion causes the liquid in the tubes to spin round inside the tubes and form a vortex. This motion increases the surface area of contact between the liquid and the wall of the container thereby increasing the amount of heat transferred to the liquid and increasing evaporation rate when the samples are subjected to vacuum by evacuation of the chamber.
  • An example of such a device is shown in Figure 1.
  • the vacuum pressure has to be carefully controlled (usually manually) so that it is low enough to promote rapid evaporation but not too low to cause bumping or spitting of the liquids.
  • the sample tubes themselves are held in an array, for example, in a rack or holder, such as that illustrated in Figure 2, they cannot be mounted intimately in heat exchange blocks of aluminium or other suitable material, which will transfer heat efficiently and uniformly to all the tubes in the array so as to procure evaporation of the samples at a uniform rate.
  • the array can be surrounded by a heat exchanger, heat will tend to be preferentially transferred to the outer tubes in the array while those in the middle of the array will receive much less heat.
  • samples can be dissolved in a wide range of mixtures of water and acetonitrile. In this case water evaporates much more slowly than acetonitrile and samples dissolved in acetonitrile-rich mixtures dry more quickly than those in water-rich mixtures.
  • heat is conveyed to the latter by conduction from a surrounding heat source through a non-volatile heat conducting fluid which completely surrounds the containers.
  • vacuum is applied to the plurality of containers in that they are placed in a vacuum chamber.
  • the fluid may be a non-volatile liquid such as a silicone, a pseudo-fluid comprised of a mass of small particles of an inert solid such as aluminium, polypropylene or polytetrafluoethylene, or a slurry which is a mixture of solids and liquids.
  • a non-volatile liquid such as a silicone
  • a pseudo-fluid comprised of a mass of small particles of an inert solid such as aluminium, polypropylene or polytetrafluoethylene
  • a slurry which is a mixture of solids and liquids.
  • the particles should be shaped to be free flowing and of a size which will allow them to flow between the stacked tubes yet be subjected to vacuum without risk of being sucked into the vacuum pump.
  • the fluid is typically heated to a temperature below the maximum permissible sample temperature, and is caused to flow around and to make contact with the sample containers, to which it imparts heat, but the temperature of the samples will not exceed the temperature of the fluid.
  • the evaporative cooling effect reduces and eventually ceases, and they quickly reach the fluid temperature, but thereafter do not absorb any more heat, so remain at that temperature.
  • Samples containing evaporating liquid will continue to absorb heat and will therefore continue to evaporate.
  • the pseudo-fluid particles are made of a good thermal conductor such as aluminium or silver, which will reliably conduct heat with minimal loss into the centre of the rack, and from one sample to another, even without significant particle movement.
  • the particles are preferably packed around and in between the containers so that there are continuous lines of touching particles throughout the matrix and the temperature limiting feature of the arrangement is still obtained if the particles are of a good heat conducting material such as aluminium or silver, so that temperature gradients in the matrix are kept to the minimum.
  • vacuum may alternatively be applied individually to each container in an array by means of sealing caps and tubes connected by a manifold to a source of vacuum.
  • An example of an array of such sample containers is illustrated in Figure 3.
  • the conducting fluid may be a liquid, gas or vapour.
  • the fluids may be heated and then forced past the containers.
  • the sample array is mounted in a gas-tight enclosure so that the fluid can be recirculated through heating means. Good performance can be achieved by choosing a vapour which condenses at the temperature to which the containers need to be heated.
  • the pressure may be varied in the enclosure to adjust the condensing temperature of the vapour.
  • solid particles are used in the heat conducting pseudo-fluid, they may be made more effective either by being fluidised by blowing gas through them in the case in which vacuum is applied individually to the containers, or by vibration, if the particles are in a vacuum chamber.
  • the invention also extends to a method of heating in an evaporator wherein, in order to heat a liquid sample contained in a tube, the tube is immersed in a heat conducting nonvolatile fluid.
  • Figure 4 is a section in elevation of the main part of the vortex evaporator shown in Figure 1;
  • Figure 5 is a perspective view corresponding to Figure 4.
  • Figure 6 shows diagrammatically how the evaporator part is rotated.
  • a rectangular array of say 36 sample tubes one of which is indicated at 10, are mounted in appropriate tightly fitting holes in upper and lower plastic tray holders 12, 14.
  • the base of the tubes rest on a plastic mat 16 supported within a cylindrical container 18, akin to a cake tin.
  • gauze 22 Resting firmly against the top of the tubes 10 is a gauze 22 which is stretched over the upper edges of the walls of the container and is secured thereto by suitable fixings, one of which is indicated at 24.
  • the lower parts of the tubes are surrounded by a mass of pseudo-fluid particles 26 which extend up to about the level of the lower tray holder 14.
  • the particles are of about 1 to 2 mm diameter in size, not necessarily round, and are made of aluminium or aluminium oxide which is a good heat conductor.
  • the container 18 Normally in a vortex evaporator the container 18 is horizontally disposed, as shown. However, in order for the particles to move relative to the tubes, the container is given a slow backwards and forwards tilting motion about a single axis, in addition to the normal rapid orbital rotation which causes the liquid sample in each tube to form a vortex. Typically, a tilting action occurs within the range 1 to 60 times per minute, while the orbital rotation takes place at 100 to 1000 rpm.
  • the container is mounted on a spindle 28, which is driven about an eccentric path 30 so that it sweeps out the shape of a cone.
  • the container 18 remains inclined, rotating from one extreme position 18 to the opposite extreme position 18' (shown chain-dotted).
  • the particles 26 migrate or slush around the circular wall of the container in a kind of vortex motion, similar to that of the liquid samples as shown in Figure 1.
  • the panicles are heated, by known means, the heat is transferred to the tubes and in turn to the liquid sample therein.
  • the whole device is situated within a vacuum chamber (not shown), and the apertures in the gauze 22 are large enough to enable evaporated vapour 32 from the tubes 10 to escape, but small enough to prevent the particles 26 from passing through.
  • the density of the particles 26 is sufficiently high to tend to cause the tubes 10 io float upwards, particularly when the outer tubes are subjected to a higher level of the particles at each rotation of the container 18. It is therefore important that the gauze 22 is sufficiently strong to hold down the tubes at all times.
  • evaporation is achieved or at least promoted by placing a suction tube inside each sample tube 10 so that the inserted end of the suction tube is positioned just above the top surface of the liquid in the sample tube. Evaporating vapour is thus withdrawn through the suction tube, while allowing ambient gas to flow into the sample tube to replace the volume of vapour extracted by the suction process.
  • An example of such a suction tube arrangement is described in co-pending UK Application No. 9918914.4 (ref: C1094/C), the entire disclosure of which is hereby incorporated by reference into the present specification.
  • the whole sample tube arrangement may again be placed within a vacuum chamber, as in Figure 1 , or alternatively may be held at atmospheric pressure or at any other desired pressure.

Landscapes

  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Dans un évaporateur du type rotatif ou à tourbillon pourvu de contenants étroitement espacés à partie supérieure ouverte qui contiennent des échantillons liquides soumis à des conditions de vide, la chaleur est transportée vers les contenants par l'intermédiaire d'un fluide non volatil qui entoure complètement les contenants. Le fluide peut être un liquide ou un pseudo-liquide non volatil tel que des particules d'aluminium, d'oxyde d'aluminium ou de polypropylène.
PCT/GB2000/000279 1999-02-09 2000-01-31 Procédé de chauffage pour évaporateurs Ceased WO2000047976A1 (fr)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
GB9902746.8 1999-02-09
GBGB9902746.8A GB9902746D0 (en) 1999-02-09 1999-02-09 Improved heating method for vortex evaporator
GB9903470.4 1999-02-17
GBGB9903470.4A GB9903470D0 (en) 1999-02-09 1999-02-17 Improved heating method for evaporators
GBGB9918831.0A GB9918831D0 (en) 1999-02-09 1999-08-11 Improved heating method for evaporators
GB9918831.0 1999-08-11
GB9926569.6 1999-11-11
GBGB9926569.6A GB9926569D0 (en) 1999-02-09 1999-11-11 Improved heating method for evaporators

Publications (1)

Publication Number Publication Date
WO2000047976A1 true WO2000047976A1 (fr) 2000-08-17

Family

ID=27451870

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB2000/000279 Ceased WO2000047976A1 (fr) 1999-02-09 2000-01-31 Procédé de chauffage pour évaporateurs

Country Status (2)

Country Link
GB (1) GB2349588A (fr)
WO (1) WO2000047976A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE202008015964U1 (de) * 2008-12-03 2010-05-06 Vacuubrand Gmbh + Co Kg Verdampfer, insbesondere für einen Vakuumpumpstand
CN106179555A (zh) * 2016-09-12 2016-12-07 贵州大学 一种高度可调的恒温水箱
WO2022269068A1 (fr) * 2021-06-24 2022-12-29 Andreas Hettich Gmbh & Co. Kg Dispositif pour le traitement d'échantillons dans des récipients d'échantillons sous vide

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115382498A (zh) * 2022-08-05 2022-11-25 上海组波智能仪器科技有限公司 一种原位化学合成及后处理工作站及其使用方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4003713A (en) * 1975-08-14 1977-01-18 Bowser Everett N Multiple test tube evaporator
EP0592354A2 (fr) * 1992-10-07 1994-04-13 Firma Andreas Hettich Centrifugeuse à vide
US5569357A (en) * 1994-04-28 1996-10-29 Labconco Corporation Vortex evaporator

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2653214A (en) * 1951-02-16 1953-09-22 A A Morgan Electric test bottle bath
FR2298354A1 (fr) * 1975-01-23 1976-08-20 Fisons Lab Sa Appareillage pour la concentration d'extraction de tissus animaux et vegetaux
JPH0622689B2 (ja) * 1986-02-24 1994-03-30 中央化工機株式会社 恒温装置
FR2644356B1 (fr) * 1989-03-20 1992-11-20 Jouan Procede de concentration d'echantillons par evaporation du solvant et evaporateur-concentrateur centrifuge pour la mise en oeuvre de ce procede
DE29622848U1 (de) * 1996-07-02 1997-07-03 Barkey, Volker, 33619 Bielefeld Vorrichtung zum Temperieren von Probengefäßen
CH688987A5 (de) * 1996-11-13 1998-07-15 Doebelin Werner Reaktionskammer fuer die chemische Synthese oder verwandte Anwendungen.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4003713A (en) * 1975-08-14 1977-01-18 Bowser Everett N Multiple test tube evaporator
EP0592354A2 (fr) * 1992-10-07 1994-04-13 Firma Andreas Hettich Centrifugeuse à vide
US5569357A (en) * 1994-04-28 1996-10-29 Labconco Corporation Vortex evaporator

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE202008015964U1 (de) * 2008-12-03 2010-05-06 Vacuubrand Gmbh + Co Kg Verdampfer, insbesondere für einen Vakuumpumpstand
CN106179555A (zh) * 2016-09-12 2016-12-07 贵州大学 一种高度可调的恒温水箱
WO2022269068A1 (fr) * 2021-06-24 2022-12-29 Andreas Hettich Gmbh & Co. Kg Dispositif pour le traitement d'échantillons dans des récipients d'échantillons sous vide

Also Published As

Publication number Publication date
GB2349588A (en) 2000-11-08
GB0001976D0 (en) 2000-03-22

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