WO2001040763A1 - Ameliorations de, ou se rapportant a l'evaporation sous vide - Google Patents

Ameliorations de, ou se rapportant a l'evaporation sous vide Download PDF

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Publication number
WO2001040763A1
WO2001040763A1 PCT/GB2000/004276 GB0004276W WO0140763A1 WO 2001040763 A1 WO2001040763 A1 WO 2001040763A1 GB 0004276 W GB0004276 W GB 0004276W WO 0140763 A1 WO0140763 A1 WO 0140763A1
Authority
WO
WIPO (PCT)
Prior art keywords
spitting
warning signal
samples
detecting
vessel
Prior art date
Application number
PCT/GB2000/004276
Other languages
English (en)
Inventor
Michael Cole
Original Assignee
Genevac Limited
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 Genevac Limited filed Critical Genevac Limited
Publication of WO2001040763A1 publication Critical patent/WO2001040763A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04B—CENTRIFUGES
    • B04B7/00—Elements of centrifuges
    • B04B7/02—Casings; Lids
    • B04B7/06—Safety devices ; Regulating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample

Definitions

  • This invention relates to drying of samples comprising a volatile liquid and non-volatile sample material by vacuum evaporation, in particular to a method of, and apparatus for, detecting spitting of liquid from the sample caused by excessively vigorous boiling of said liquid during drying by vacuum evaporation.
  • samples are subjected to centrifugal force as in a centrifugal evaporator, such that the liquid is constrained to remain in the sample containers by the centrifugal force.
  • samples can be subjected to an orbital motion as in a vortex evaporator and the pressure controlled to a range in which spitting should not occur.
  • These methods are effective for the majority of samples but there are some combinations of sample material and volatile liquids including mixtures of volatile liquids which are not constrained to remain in their containers unless a greater vacuum vessel pressure and/or centrifugal force than normal are/is applied.
  • An object of the present invention is therefore to provide a method of, and apparatus for, detecting when spitting is occurring during vacuum evaporation.
  • a method of detecting spitting of liquid from samples during drying by vacuum evaporation within a vessel wherein the vessel pressure, which is normally held constant or constrained to change only downwards and slowly, is monitored for any momentary increases in pressure and a warning signal is generated in response thereto.
  • the warning signal may also serve as a feedback signal to a control system to increase the speed of rotation of the samples (to assist in retaining ejected material within the sample containers) or to increase the pressure in the vacuum vessel (to reduce the tendency for spitting to occur).
  • the warning signal may be audible and/or visible.
  • apparatus for detecting spitting of liquid from samples during drying by vacuum evaporation comprising a vacuum vessel, a vacuum pump, transducer means in said vessel, a computing means for detecting momentary increases in signals derived from the transducer means, a signal conveying means e.g. wire or transmitter and receiver whereby pressure information from the transducer means is communicated to the computing means, and a warning signal generating means which is under the control of the computing means.
  • the transducer means has a response time of the order of 0.1 seconds to 1 second.
  • the computing means may include a differentiator, so as to respond to, and provide a signal indicative of, the rate of change of the transducer means signal.
  • the invention also lies in a centrifugal evaporator including apparatus for detecting spitting of material from samples during drying by vacuum evaporation, as aforesaid.
  • the invention also lies in a vortex evaporator including apparatus for detecting spitting of material from samples during drying by vacuum evaporation, as aforesaid.
  • Figure 1 shows a known form of centrifugal evaporator, wherein sample containers 10 containing sample material 12 are pivotally suspended from rotor arms 14 and the rotor arms are attached to a shaft 16 that is capable of rotation in a bearing 18 about a vertical axis.
  • the shaft 16 is driven for rotation by a motor (not shown), which rotation causes the sample containers 10 to lift upwards and outwards and thus to restrain the sample material 12 in the sample containers through the centrifugal force resulting therefrom.
  • the sample containers, sample material, rotor arms and shaft are enclosed by a vacuum vessel 20 which has an opening 22 leading to a vacuum pump (not shown).
  • a pressure transducer 24 linked by wires with a computing means produces an electrical output signal proportional to the pressure inside the vacuum vessel 20.
  • the computing means is operable to detect increases in the pressure inside the vacuum vessel, which pressure is normally constrained to remain constant or to change slowly downwards during evaporation. On detecting such an increase the computing means activates a warning signal generating means (not shown) which may be audible or visible.
  • Figuie 2 shows a vortex evaporator, wherein sample containers 26 are supported in an aluminium block 28.
  • the aluminium block 28 is clamped upon a baseplate 30 by clamps 32.
  • the baseplate 30 is mounted upon an eccentric section of a shaft 34.
  • the shaft 34 is driven for rotation about a vertical axis in a bearing 36 by a motor (not shown), which rotation causes the baseplate 30, aluminium block 28 clamped thereto, sample containers 26 and sample material 38 therein to describe an orbital path in a plane perpendicular to the axis of rotation of the shaft 34.
  • the orbital rotation agitates the sample material and tends to cause vortices in the material, which tend to reduce any tendency for spitting.
  • the sample containers 26, sample material 38, aluminium block 28 and shaft 34 are enclosed by a vacuum vessel 40 that has an opening 42.
  • the opening 42 leads to a vacuum pump (not shown).
  • a pressure transducer 44 connected by wires to a computing means (not shown) produces an electrical output signal proportional to the pressure inside the vacuum vessel 40.
  • the computing means detects increases in the pressure inside the vacuum vessel, which is normally constrained to remain constant or to change only slowly. On detecting such an increase the computing means activates a warning signal generating means (not shown) which may be audible or visible.

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Drying Of Solid Materials (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

L'invention concerne un procédé et un appareil de détection de projections de matériau à partir d'échantillons dans une récipient sous vide pendant le séchage par évaporation sous vide desdits échantillons, notamment dans un évaporateur centrifuge ou un évaporateur à vortex. La pression instantanée, qui augmente à l'intérieur de la cuve sous vide, est révélatrice de telles projections, qui sont détectées et qui servent à activer un signal d'avertissement. Celui-ci, visible et/ou audible, attire l'attention de l'opérateur sur les projections. Le signal d'avertissement peut servir de signal de retour dans un système de commande qui régule le moteur d'une pompe sous vide ou le moteur faisant tourner les échantillons.
PCT/GB2000/004276 1999-11-30 2000-11-09 Ameliorations de, ou se rapportant a l'evaporation sous vide WO2001040763A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9928123.0 1999-11-30
GBGB9928123.0A GB9928123D0 (en) 1999-11-30 1999-11-30 Improvements in or relating to vacuum evaporation

Publications (1)

Publication Number Publication Date
WO2001040763A1 true WO2001040763A1 (fr) 2001-06-07

Family

ID=10865310

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB2000/004276 WO2001040763A1 (fr) 1999-11-30 2000-11-09 Ameliorations de, ou se rapportant a l'evaporation sous vide

Country Status (2)

Country Link
GB (1) GB9928123D0 (fr)
WO (1) WO2001040763A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1923112A3 (fr) * 2006-11-18 2010-04-07 Eppendorf AG Concentrateur sous vide et procédé de concentration sous vide
FR3005275A1 (fr) * 2013-05-02 2014-11-07 Afi Centrifuge Centrifugeuse de laboratoire munie de moyens d'identification d'un accessoire rapporte sur son arbre moteur

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3413385A1 (de) * 1984-04-10 1985-10-17 Peter 7600 Offenburg Huber Verfahren zum eindampfen von fluessigkeiten unter vakuum sowie vorrichtung zur durchfuehrung des verfahrens
US5431620A (en) * 1994-07-07 1995-07-11 Beckman Instruments, Inc. Method and system for adjusting centrifuge operation parameters based upon windage
US5569357A (en) * 1994-04-28 1996-10-29 Labconco Corporation Vortex evaporator
GB2332865A (en) * 1997-12-23 1999-07-07 Michael Cole Vacuum centrifugal evaporator
WO2000047975A1 (fr) * 1999-02-09 2000-08-17 Genevac Limited Commande amelioree de vide dans des evaporateurs

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3413385A1 (de) * 1984-04-10 1985-10-17 Peter 7600 Offenburg Huber Verfahren zum eindampfen von fluessigkeiten unter vakuum sowie vorrichtung zur durchfuehrung des verfahrens
US5569357A (en) * 1994-04-28 1996-10-29 Labconco Corporation Vortex evaporator
US5431620A (en) * 1994-07-07 1995-07-11 Beckman Instruments, Inc. Method and system for adjusting centrifuge operation parameters based upon windage
GB2332865A (en) * 1997-12-23 1999-07-07 Michael Cole Vacuum centrifugal evaporator
WO2000047975A1 (fr) * 1999-02-09 2000-08-17 Genevac Limited Commande amelioree de vide dans des evaporateurs

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1923112A3 (fr) * 2006-11-18 2010-04-07 Eppendorf AG Concentrateur sous vide et procédé de concentration sous vide
US8205353B2 (en) 2006-11-18 2012-06-26 Eppendorf Ag Vacuum concentrator and method for vacuum concentration
US8857073B2 (en) 2006-11-18 2014-10-14 Eppendorf Ag Method for vacuum concentration
FR3005275A1 (fr) * 2013-05-02 2014-11-07 Afi Centrifuge Centrifugeuse de laboratoire munie de moyens d'identification d'un accessoire rapporte sur son arbre moteur

Also Published As

Publication number Publication date
GB9928123D0 (en) 2000-01-26

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