EP0571426B1 - Nettoyage de pieces comportant des residus organiques - Google Patents

Nettoyage de pieces comportant des residus organiques Download PDF

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Publication number
EP0571426B1
EP0571426B1 EP92904002A EP92904002A EP0571426B1 EP 0571426 B1 EP0571426 B1 EP 0571426B1 EP 92904002 A EP92904002 A EP 92904002A EP 92904002 A EP92904002 A EP 92904002A EP 0571426 B1 EP0571426 B1 EP 0571426B1
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EP
European Patent Office
Prior art keywords
pressure vessel
liquefied
pressure
supercritical gas
process according
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
EP92904002A
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German (de)
English (en)
Other versions
EP0571426A1 (fr
Inventor
Robert Adler
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.)
Linde GmbH
Original Assignee
Union Industrie Comprimierter Gase GmbH Nfg KG
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 Union Industrie Comprimierter Gase GmbH Nfg KG filed Critical Union Industrie Comprimierter Gase GmbH Nfg KG
Publication of EP0571426A1 publication Critical patent/EP0571426A1/fr
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Publication of EP0571426B1 publication Critical patent/EP0571426B1/fr
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
    • B08B3/104—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid using propellers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0021—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
    • B08B7/0092—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by cooling
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents

Definitions

  • the invention relates to a method for cleaning workpieces which have organic residues, using a compressed gas which is introduced under pressure into a pressure container loaded with the workpieces.
  • a gas compressed to its supercritical pressure or above is placed in a pressure container on the workpieces to be cleaned headed.
  • the temperature of the gas compressed in this way is then changed in various steps, starting from a point close to the critical temperature, in order to influence the solution properties of the gas phase. Before each change, the temperature is kept constant for a certain time interval.
  • the cleaning of the workpieces can also be supported by adding a liquid such as ion-free water to the compressed gas, a chemically reactive one Substance or sound or radiation energy can be introduced.
  • the measures described, which support the cleaning of the workpieces require technically complex additional devices and are also not very effective. The effort involved is not justified by increased cleaning success.
  • the method according to WO 90 06 189 also requires a high level of control engineering.
  • the individual steps in which the temperature is changed follow at intervals of about 10 minutes.
  • the temperature must be kept constant. It must therefore be ensured that a new temperature is set in a large pressure vessel and then kept constant within a very short time.
  • the required complex equipment which is not explained in WO 90 06 189, makes such a cleaning process less attractive for industrial use.
  • the invention is therefore based on the object of developing a method for cleaning workpieces contaminated with organic residues using a compressed gas which avoids the abovementioned disadvantages and increases the cleaning success in an economical manner.
  • This object is achieved in that a liquefied or supercritical gas is circulated in the pressure vessel during the cleaning process.
  • the method according to the invention represents a simple measure which considerably supports the cleaning process.
  • the fluid understood as liquefied or supercritical gas, is circulated in the pressure vessel, for example by rotating a bladed impeller.
  • the onset of fluid flow in the pressure vessel causes a constant exchange of pure fluid loaded with dissolved impurities. As a result, the organic residues adhering to the surfaces of the workpieces can gradually be completely removed.
  • the speed of the circulation is advantageously changed during the cleaning process.
  • This change can be made, for example, by cyclically changing the speed of an impeller that causes the circulation.
  • the suction and pressure areas of the fluid forming during the circulation change in their cross section, and that at the same time the velocity distribution of the fluid can be influenced. This measure prevents that in Form pressure vessel areas in which the fluid would not circulate at a constant speed of the impeller.
  • Suitable fluids for removing organic residues are, for example, noble gases such as helium or argon, hydrocarbons, e.g. Alkanes such as methane, ethane or propane, or alkenes such as ethene or propene, as well as trifluoromethane, carbon dioxide, nitrous oxide and sulfur hexafluoride.
  • noble gases such as helium or argon
  • hydrocarbons e.g. Alkanes such as methane, ethane or propane
  • alkenes such as ethene or propene
  • trifluoromethane carbon dioxide, nitrous oxide and sulfur hexafluoride
  • Carbon dioxide has proven to be a particularly suitable fluid in the method according to the invention, since it has the following advantages:
  • Carbon dioxide is not flammable or explosive, large quantities of carbon dioxide are inexpensively available as a by-product of industrial processes, carbon dioxide is less polluting than other solvents and carbon dioxide is chemically inert.
  • the thermodynamic properties of carbon dioxide meet the process according to the invention.
  • a suitable measure when carrying out the method according to the invention is to keep the temperature of the liquefied or supercritical gas in the pressure vessel constant during the cleaning process.
  • the suitable parameters, temperature and pressure of the fluid for removing the organic residues are first determined in preliminary tests. These parameters are then kept constant during the cleaning process.
  • part of the liquefied or supercritical gas is continuously withdrawn from the pressure vessel, passed through a heat exchanger and then returned to the pressure vessel. Heating of the fluid, i.e. of the compressed gas may be necessary for long-term cleaning processes in non-heat-insulated pressure vessels, on the other hand cooling of the fluid may be necessary especially in heat-insulated vessels if the energy supplied for the circulation of the fluid warms the fluid.
  • the heat exchange of the fluid is of course also suitable for sweeping over a certain temperature range during the cleaning process, should this be necessary.
  • an inadmissible pressure increase can be prevented by using a pressure relief valve or an overflow regulator on the pressure vessel.
  • the fluid contaminated with the organic residues must be removed from the pressure vessel, and then the cleaned workpieces are removed.
  • the potential stress energy of the liquefied or supercritical gas that is released during expansion is used to drive a turbine.
  • This measure allows part of the energy used for the cleaning process to be recovered and the energy efficiency of the cleaning system to be increased.
  • the organic residues are separated from at least part of the liquefied or supercritical gas containing the organic residues and the remaining part is used together with pure liquefied or supercritical gas for a further cleaning process.
  • the fluid mass in the pressure vessel can be used for several cleaning processes before it is saturated with the organic residues. It is therefore sufficient to replace only a part of the fluid used with pure fluid after each cleaning operation without noticeably reducing the cleaning capacity and speed. This measure sensibly limits the consumption and the effort required to provide the amount of fluid required for cleaning.
  • a suitable device for carrying out the method according to the invention with a cylindrical pressure vessel, which has inlet and outlet lines for compressed gases is characterized in that a first cylindrical pressure vessel contains an impeller mounted on its axis within the pressure vessel, that the first pressure vessel with an analog equipped second pressure vessel is connected via valve-provided lines, that a pump is arranged in one of the connecting lines and a heat exchanger is arranged in this or another connecting line, the heat exchanger and the pump being connected to each pressure vessel by additional lines, and that each pressure vessel is connected to one or more storage containers for compressed gases by further lines.
  • Each pressure vessel 38, 39 contains an impeller 6 which causes the compressed gas to circulate and which is separated from the rest of the interior of the pressure vessel 38, 39 by a protective grille 5.
  • the impeller 6 is driven outside the pressure container 38, 39 via the shaft 9 and is mounted in a stuffing box 8.
  • the pressure vessel 38, 39 there is a fixedly mounted guide rail 12 for a pipe slide on which the workpieces to be cleaned are located.
  • the pressure vessel 38, 39 is firmly closed by a high-pressure lid 7.
  • Each pressure vessel 38, 39 also contains a pressure measuring device 3, 34 and safety valve devices 4, 35 as well as a level probe 10, 31 and a pressure switch 11, 32.
  • the pressure vessels 38, 39 are connected to one another by several lines.
  • a direct connecting line contains two shut-off ball valves 2, 33 and a motor-driven control valve 29.
  • a heat exchanger 20 is connected to the pressure vessel 38 via lines via the motor-driven control valves 13, 15, 14 and to the pressure vessel 39 via the control valves 27, 15, 28.
  • This heat exchanger 20 contains a temperature controller 21 and a safety valve 22.
  • a pump 19 is connected to the pressure vessel 38 via lines via the motor-driven control valves 13, 17, 14 and to the pressure vessel 39 via the control valves 27, 17, 28.
  • a safety valve 23 is also fitted in the pump line.
  • both pressure vessels 38, 39 are connected to one another by lines via the heat exchanger 20 and the control valves 13, 15, 28 and via the pump 19 and the control valves 13, 17, 28.
  • a storage container (not shown in the drawing) is used for a compressed gas, in which the latter is compressed under pressure and partly liquefied.
  • the cleaning fluid in the gaseous phase can be removed from the upper part of this storage container, and in the liquid phase from the lower part of this storage container and introduced into the two pressure containers 38, 39.
  • the gaseous fluid can be passed via the heat exchanger 20 via the control valves 16, 15, 14 into the pressure vessel 38 and via the control valves 16, 15, 28 into the pressure vessel 39.
  • the liquid fluid is fed via the pump 19 via the control valves 18, 17, 14 to the pressure vessel 38 and via the control valves 18, 17, 28 to the pressure vessel 39.
  • cleaning fluid can be returned from the pressure container 38 to the storage container.
  • gaseous fluid can be returned to the reservoir via the overflow regulator 1 and the control valve 36 and liquid fluid via the overflow regulator 1 and the control valve 37.
  • cleaning fluid can be returned from the pressure container 39 to the storage container.
  • the device according to the invention contains a ventilation system in which the dissolved organic residues are separated from the fluid by relaxing.
  • the fluid can also be directed into a turbine, which makes part of the energy released during the relaxation process available again by converting this energy into rotational energy and using the latter to generate electricity.
  • This ventilation system is connected via a probe for liquid fluid 26 and a motor-driven control valve 25 to the line system between the two pressure vessels 38, 39.
  • used fluid can be conducted from the pressure vessels 38, 39 into the ventilation system.
  • the method according to the invention is used to clean copper pipes that have just been produced, the surfaces of which are coated with drawing grease during the manufacturing process.
  • About 700 to 800 copper tubes are loaded onto a tube slide and these are then moved on the guide rails 12 into the two pressure vessels 38, 39. Then the high pressure cover 7 are closed.
  • carbon dioxide is used as the fluid, which is removed from a storage container under pressure at a room temperature of approximately 298 ° Kelvin.
  • the carbon dioxide flows in gaseous form through the lines when the control valves 16, 15 and 14 are open into the pressure vessel 38 until pressure equalization with the reservoir has been established.
  • the temperature of the gas is kept constant by the heat exchanger 20 to approximately 298 ° Kelvin.
  • the pressure of the carbon dioxide gas at this temperature is then about 64 bar in the pressure vessel 38. A cooling of the gas should be prevented, as this leads to the stopping of the oil-like residues adhering to the pipes and thereby the Cleaning process would complicate.
  • the pressure vessel 38 is now biased. Now liquid carbon dioxide can be passed into the pressure vessel 38 without the liquefied gas expanding.
  • the connection to the upper part of the storage container is closed, the control valves 18, 17 and 14 are opened and liquid carbon dioxide from the lower part of the storage container is passed via the pump 19 into the pressure container 38.
  • the inflowing liquid pushes the carbon dioxide gas back out of the pressure vessel 38 via the overflow regulator 1 into the storage vessel with the control valve 36 open.
  • the level probe 10 switches off the pump 19 when the desired level is reached.
  • the pressure vessel 38 is now filled with liquid carbon dioxide.
  • good cleaning results were achieved at temperatures between 298 ° Kelvin and 304 ° Kelvin, the pressure was slightly above the corresponding vapor pressure values.
  • Corresponding conditions are now set in the pressure vessel 38, the temperature of the liquid carbon dioxide being able to be regulated with the aid of the heat exchanger 20.
  • the cleaning process is carried out by circulating the liquid carbon dioxide in the pressure vessel 38.
  • the impeller 6 is driven by the shaft 9, the speed of the impeller 6 being changed in cycles by means of a time control. As a result, the zone in which no circulation takes place at constant speed is shifted over the diameter of the pressure vessel 38.
  • the recirculation causes a carbon dioxide flow, which constantly leads new amounts of carbon dioxide to the pipe surface, whereby the solubility capacity of the entire carbon dioxide volume in the pressure vessel 38 can be used and the cleaning process proceeds much faster and more efficiently than when the contact is at rest.
  • the oil-like residues on the copper pipes dissolve and pass into a uniform phase with the liquid carbon dioxide.
  • part of the fluid in order to maintain a constant temperature of the fluid during the cleaning process in the pressure vessel, part of the fluid can be passed continuously through the heat exchanger 20 by opening the control valves 13, 15 and 14. This ensures that the solution properties of the liquid carbon dioxide do not change undesirably during the cleaning process.
  • the cleaning process takes about half an hour in this embodiment. In general, this period is varied depending on the degree of contamination of the copper pipes.
  • the prestressing of the pressure vessel 39 begins.
  • gaseous carbon dioxide is passed from the storage container via the heat exchanger 20 with the valves 16, 15 and 28 open into the pressure container 39.
  • liquid carbon dioxide is pumped from the reservoir via the pump 19 into the pressure vessel 39 with the valves 18, 17 and 28 open.
  • this number is approximately 7 to 8 Cleaning processes, ie it is sufficient to fill the seventh to eighth part of the container volume with pure liquid carbon dioxide during the next cleaning process.
  • valves 13, 17 and 28 are opened and liquid carbon dioxide, which now already contains the oil-like residues in solution, is pumped from the pressure vessel 38 into the pressure vessel 39.
  • the gas used to bias the pressure vessel 39 is passed into the pressure vessel 38.
  • the shut-off ball valves 33 and 2 and the control valve 29 are opened.
  • the level probe 31 ends the filling process with liquid carbon dioxide.
  • the cleaning process now takes place in the pressure container 39.
  • the cleaned copper pipes, the remaining amount of liquid carbon dioxide, which contains the oil-like residues, and the pure carbon dioxide gas introduced to maintain the pressure are located in the pressure vessel 38.
  • This carbon dioxide gas which was introduced from the pressure vessel 38 into the pressure vessel 39, causes an excess pressure in the pressure vessel 38 due to the remaining amount of liquid in the cleaning process, whereby the subsequent removal of the liquid carbon dioxide containing the oil residues guarantees that these residues in the liquid Remain carbon dioxide dissolved.
  • the control valves 13 and 25 are opened, this contaminated amount of carbon dioxide liquid is blown out of the pressure vessel 38 into the ventilation system. This process is complete when the carbon dioxide liquid probe 26 no longer registers a flow of liquid carbon dioxide.
  • the pressure must be reduced to atmospheric pressure.
  • the circulation of the gas is initiated when the probe 26 only registers gaseous carbon dioxide.
  • the valves 13, 15 and 14 are then opened and part of the gas is passed over the heat exchanger 20 due to the flow pressure arising during the circulation.
  • the valve 25 remains open, so that a partial flow of the gas is blown out of the pressure vessel 38.
  • the carbon dioxide can be passed through a simple oil separator, in which the oil-like residues, which stagnate and fail due to the strong cooling of the carbon dioxide when relaxing, are collected, and the carbon dioxide accumulates as gas and snow, which will soon sublimate.
  • This exemplary embodiment shows the economic sequence of the method according to the invention, with which good cleaning results are achieved.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Cleaning In General (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

Le présent procédé se rapporte au nettoyage de pièces comportant des résidus organiques, en utilisant un fluide introduit sous pression dans un réservoir sous pression contenant des pièces. Selon l'invention, le fluide est soumis à une circulation forcée, pendant le processus de nettoyage, et des gaz, de préférence liquéfiés, p. ex. du dioxyde de carbone, sont utilisés comme fluide. Grâce à l'utilisation d'un échangeur de chaleur, il est possible de régler la température du fluide pendant le processus.

Claims (11)

  1. Procédé pour nettoyer des pièces qui comportent des résidus organiques en utilisant un gaz comprimé qui est amené sous pression à un réservoir sous pression chargé de pièces, caractérisé en ce que l'on fait circuler un gaz liquéfié ou surcritique pendant le processus de nettoyage dans le réservoir sous pression (38, 39).
  2. Procédé selon la revendication 1, caractérisé en ce que l'on fait varier la vitesse de circulation pendent le processus de nettoyage.
  3. Procédé selon l'une des revendications 1 à 2, caractérisé en ce que l'on utilise comme gaz liquéfié ou surcritique du dioxyde de carbone.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que l'on maintient constante la température du gaz liquéfié ou surcritique dans le réservoir pressurisé (38, 39) pendant le processus de nettoyage.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que l'on extrait en continu pendant le processus de nettoyage une partie du gaz liquéfié ou surcritique hors du réservoir sous pression (38, 39), on le fait passer dans un échangeur de chaleur (20) et on le ramène ensuite au réservoir sous pression (38, 39).
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce qu'après le processus de nettoyage, pendant l'évacuation du gaz liquéfié ou surcritique contenant les résidus organiques, hors du réservoir sous pression (38, 39), on maintient constante la température du gaz liquéfié ou surcritique.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que pendant l'évacuation du gaz liquéfié ou surcritique contenant les résidus organiques, hors du réservoir sous pression (38, 39), on amène du gaz liquéfié ou surcritique pur dans le réservoir sous pression (38, 39) et on maintient ensuite la pression constante ou bien on l'augmente.
  8. Procédé selon l'une des revendications 1 à 7, caractérisé en ce que l'on sépare les résidus organiques par détente du gaz liquéfié ou surcritique contenant les résidus organiques.
  9. Procédé selon la revendication 8, caractérisé en ce que pendant la détente le gaz liquéfié ou surcritique est envoyé à une turbine.
  10. Procédé selon l'une des revendications 1 à 9, caractérisé en ce que l'on sépare les résidus organiques d'au moins une partie du gaz liquéfié ou surcritique contenant les résidus organiques, et l'on utilise la partie restante avec du gaz liquéfié ou surcritique pur pour processus de nettoyage supplémentaire.
  11. Dispositif pour la mise en oeuvre du procédé selon l'une des revendications 1 à 10, muni d'un réservoir sous pression cylindrique qui comprend des conduites d'amenée et de sortie du gaz comprimé, caractérisé en ce qu'un premier réservoir sous pression cylindrique (38) comporte un rotor de turbine (6) monté sur son axe à l'intérieur du réservoir sous pression (38), en ce que le premier réservoir pressurisé (38) est relié à un deuxième réservoir sous pression (39) équipé de façon analogue, par l'intermédiaire de conduites munies de valves, en ce que dans l'une des conduites de liaison est montée une pompe (19) et dans cette conduite ou dans une autre conduite de liaison est monté un échangeur de chaleur (20), l'échangeur de chaleur (20) et la pompe (19) étant reliés à chaque réservoir sous pression (38, 39) par des conduites supplémentaires, et en ce que chaque réservoir sous pression (38, 39) est relié à un ou plusieurs réservoir de réserve pour gaz comprimé par l'intermédiaires d'autres conduites.
EP92904002A 1991-02-19 1992-02-14 Nettoyage de pieces comportant des residus organiques Expired - Lifetime EP0571426B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT342/91 1991-02-19
AT0034291A AT395951B (de) 1991-02-19 1991-02-19 Reinigung von werkstuecken mit organischen rueckstaenden
PCT/EP1992/000322 WO1992014558A1 (fr) 1991-02-19 1992-02-14 Nettoyage de pieces comportant des residus organiques

Publications (2)

Publication Number Publication Date
EP0571426A1 EP0571426A1 (fr) 1993-12-01
EP0571426B1 true EP0571426B1 (fr) 1994-08-10

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP92904002A Expired - Lifetime EP0571426B1 (fr) 1991-02-19 1992-02-14 Nettoyage de pieces comportant des residus organiques

Country Status (12)

Country Link
US (1) US5980648A (fr)
EP (1) EP0571426B1 (fr)
JP (1) JPH06505189A (fr)
AT (1) AT395951B (fr)
AU (1) AU1226892A (fr)
CA (1) CA2103909A1 (fr)
CZ (1) CZ282595B6 (fr)
DE (1) DE59200370D1 (fr)
DK (1) DK0571426T3 (fr)
ES (1) ES2062889T3 (fr)
NO (1) NO180003C (fr)
WO (1) WO1992014558A1 (fr)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
EP1836242A2 (fr) 2004-10-25 2007-09-26 Nanon A/S Procede de production d'un article en caoutchouc de silicone et produit obtenu par ce procede

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NO180003B (no) 1996-10-21
ATA34291A (de) 1992-09-15
AT395951B (de) 1993-04-26
CZ282595B6 (cs) 1997-08-13
DK0571426T3 (da) 1994-09-26
NO932938L (no) 1993-08-18
AU1226892A (en) 1992-09-15
ES2062889T3 (es) 1994-12-16
DE59200370D1 (de) 1994-09-15
JPH06505189A (ja) 1994-06-16
NO932938D0 (no) 1993-08-18
NO180003C (no) 1997-01-29
WO1992014558A1 (fr) 1992-09-03
CA2103909A1 (fr) 1992-08-20
CZ167693A3 (en) 1994-03-16
EP0571426A1 (fr) 1993-12-01
US5980648A (en) 1999-11-09

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