EP0306810B1 - Method of producing pitting-resistant hard drawn tubes made of copper or copper-based alloys - Google Patents
Method of producing pitting-resistant hard drawn tubes made of copper or copper-based alloys Download PDFInfo
- Publication number
- EP0306810B1 EP0306810B1 EP88114157A EP88114157A EP0306810B1 EP 0306810 B1 EP0306810 B1 EP 0306810B1 EP 88114157 A EP88114157 A EP 88114157A EP 88114157 A EP88114157 A EP 88114157A EP 0306810 B1 EP0306810 B1 EP 0306810B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- pipes
- copper
- tubes
- treated
- pitting
- 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
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
- B24C3/00—Abrasive blasting machines or devices; Plants
- B24C3/32—Abrasive blasting machines or devices; Plants designed for abrasive blasting of particular work, e.g. the internal surfaces of cylinder blocks
- B24C3/325—Abrasive blasting machines or devices; Plants designed for abrasive blasting of particular work, e.g. the internal surfaces of cylinder blocks for internal surfaces, e.g. of tubes
- B24C3/327—Abrasive blasting machines or devices; Plants designed for abrasive blasting of particular work, e.g. the internal surfaces of cylinder blocks for internal surfaces, e.g. of tubes by an axially-moving flow of abrasive particles without passing a blast gun, impeller or the like along the internal surface
Definitions
- the invention relates to a method for producing pitting-resistant hard-drawn pipes made of copper or a copper alloy for the sanitary sector, the pipes being degreased after the cold working and the inner surface of the pipes then being treated with an abrasive.
- the invention further relates to the use of pipes produced by this method in the sanitary area.
- a more or less coherent carbon film can form on the inside of the pipe if the pipes are connected to one another, for example by brazing, or heated to facilitate bending.
- Copper pipes for the clinical area especially pipes for the transport of medical gases, must have an absolutely clean and grease-free inner surface to avoid any risks.
- the document "British Hospital Technical Memorandum" 22, May 1972 edition prescribes a multi-stage cleaning process, the interior of the tube first being degreased with water vapor or an organic solvent, dried, treated with an abrasive and then with medical pure air is blown through.
- degreasing agents for example organic solvents such as per or trichlorethylene.
- Another method involves evaporating the drawing oil and extracting the drawing oil vapors.
- Another type of treatment is to carry out the annealing in a reducing atmosphere and to remove the resulting carbon film by means of an abrasive.
- an abrasive is introduced into the tube either by pressurized water or compressed air.
- the invention has for its object to prevent the formation of carbon and / or oxide films during brazing or hot bending of hard drawn tubes made of copper or copper alloys and thus to improve the pitting resistance of these tubes.
- This object is achieved according to the invention in a method of the type mentioned at the outset by immersing the tubes for degreasing in an organic solvent bath and then treating the inner surface of the tubes with a jet of sand or corundum particles for a period of about 3 to 30 s that the inner surface of the blasted tubes has an average roughness of 0.4 to 1.5 ⁇ m.
- the method according to the teaching of the invention differs from the previously known essentially soft-annealed copper tubes-related methods by a combination of chemical and mechanical treatment stages.
- harmful films eg. B. carbon-containing films or oxide films on the inner surface of hard-drawn copper pipes.
- These films which according to the theory act as bipolar electrodes, are usually produced at the temperatures customary for brazing or hot bending copper pipes.
- the harmful films can essentially be avoided in that the inner surface of copper pipes, which has largely been freed from the drawing oil, has a certain minimum roughness after the additional blasting treatment. It is therefore important that a certain surface structure is achieved on the inner surface of the tubes, which enables only very little adhesion to the films formed during heat treatment. Stable corrosion elements, which are the cause of pitting corrosion, cannot develop.
- the abrasive treatment is carried out in such a way that the inner surface of the tubes has a mean roughness value between 0.8 ⁇ m and 1.0 ⁇ m.
- a felt plug filling the pipe cross-section can be inserted, for example, and the felt plug, which may be soaked with a cleaning agent, can then be transported through the pipe length by means of pressure.
- simply blowing out with compressed air will be sufficient to remove corundum particles adhering to the inner wall of the pipe.
- the average roughness R a was found to be 0.8 ⁇ m.
- the residual carbon content was ⁇ 0.03 mg / dm 2 below the detection limit. Long-term tests in various corrosion-promoting household waters did not show any significant formation of pitting corrosion. Likewise, no corrosion damage occurred after brazing and / or hot bending.
- tubes measuring 22 x 1 mm were used.
- the tubes were treated with corundum for 10 s.
- the average roughness value R a was 1.0 ⁇ m after the blasting agent treatment.
- the residual carbon or lubricant content was again below the detection limit.
- tubes 15 x 1 mm drawn to the final dimension were first degreased with trichloroethane, dried and then briefly immersed in a nitric acid bath.
- the other process conditions for the blasting agent treatment corresponded to those of Example 1.
- Long-term tests of five test benches operated in practice with areas that favor pitting corrosion did not show any signs of pitting attack.
- the inside surface of the pipes had a shiny metallic appearance.
- the water throughput during the flow times was about 1.5 l / min, which corresponds to an average flow velocity of about 0.2 m / s for the test tube.
Abstract
Description
Die Erfindung bezieht sich auf ein Verfahren zur Herstellung lochfraßbeständiger hartgezogener Rohre aus Kupfer oder einer Kupferlegierung für den Sanitärbereich, wobei die Rohre nach der Kaltverformung entfettet werden und die Innenoberfläche der Rohre dann mit einem Strahlmittel behandelt wird. Ferner betrifft die Erfindung die Verwendung von nach diesem Verfahren hergestellten Rohren im Sanitärbereich.The invention relates to a method for producing pitting-resistant hard-drawn pipes made of copper or a copper alloy for the sanitary sector, the pipes being degreased after the cold working and the inner surface of the pipes then being treated with an abrasive. The invention further relates to the use of pipes produced by this method in the sanitary area.
Es ist bekannt, daß nach dem letzten Ziehvorgang weichgeglühte Kupferrohre in aggressiven Leitungswässern korrosionsanfällig sind. Eine besonders charakteristische Erscheinungsform der Korrosionsschäden wird durch die Lochkorrosion verursacht, bei der es auf der Rohrinnenseite zu örtlichen Lochfraßstellen kommt. Die Entstehung derartiger Korrosionsschäden wird kohlenstoffhaltigen Rückständen zugeschrieben, die beispielsweise durch thermische Zersetzung des beim Rohrziehen verwendeten Ziehmittels auftreten.It is known that after the last drawing process, soft-annealed copper pipes are susceptible to corrosion in aggressive tap water. A particularly characteristic form of the corrosion damage is caused by pitting, which results in local pitting on the inside of the pipe. The occurrence of such corrosion damage is attributed to carbon-containing residues, which occur, for example, due to thermal decomposition of the drawing agent used in pipe drawing.
Aber auch bei hartgezogenen Kupferrohren, die keinem Glühvorgang unterzogen werden, kann ein mehr oder weniger zusammenhängender Kohlenstoffilm auf der Rohrinnenseite entstehen, wenn die Rohre beispielsweise durch Hartlöten miteinander verbunden oder zur Erleichterung des Biegens erwärmt werden.However, even with hard-drawn copper pipes that are not subjected to an annealing process, a more or less coherent carbon film can form on the inside of the pipe if the pipes are connected to one another, for example by brazing, or heated to facilitate bending.
Es hat sich herausgestellt, daß der beim Erwärmen entstehende Kohlenstoffilm dann nahezu unschädlich ist, wenn sich weniger als 0,1 mg/dm2 Ziehöl auf der Innenoberfläche des Kupferrohres befindet.It has been found that the carbon film formed during heating is almost harmless if less than 0.1 mg / dm 2 of drawing oil is on the inner surface of the copper tube.
Kupferrohre für den klinischen Bereich, inbesondere Rohre zum Transport medizinischer Gase, müssen zur Vermeidung jeglichen Risikos eine absolut saubere und fettfreie Innenoberfläche aufweisen. Um diese hohen Anforderungen erfüllen zu können, schreibt das Dokument "British Hospital Technical Memorandum" 22, Ausgabe Mai 1972, ein mehrstufiges Reinigungsverfahren vor, wobei das Rohrinnere zunächst mit Wasserdampf oder einem organischen Lösungsmittel entfettet, getrocknet, mit einem Strahlmittel behandelt und anschließend mit medizinisch reiner Luft durchblasen wird.Copper pipes for the clinical area, especially pipes for the transport of medical gases, must have an absolutely clean and grease-free inner surface to avoid any risks. In order to be able to meet these high requirements, the document "British Hospital Technical Memorandum" 22, May 1972 edition, prescribes a multi-stage cleaning process, the interior of the tube first being degreased with water vapor or an organic solvent, dried, treated with an abrasive and then with medical pure air is blown through.
Zur Entfernung des Ziehölfilms ist es aus der Rohrfertigung auch bereits bekannt, Entfettungsmittel einzusetzen, beispielsweise organische Lösungsmittel, wie Per- oder Trichlorethylen. Noch ein anderes Verfahren sieht vor, das Ziehöl zu verdampfen und die Ziehöldämpfe abzusaugen.To remove the drawing oil film, it is also known from tube production to use degreasing agents, for example organic solvents such as per or trichlorethylene. Another method involves evaporating the drawing oil and extracting the drawing oil vapors.
Eine weitere Behandlungsart besteht darin, die Glühung in einer reduzierenden Atmosphäre durchzuführen und den entstandenen Kohlenstoffilm durch ein Strahlmittel zu entfernen. Hierbei wird in das Rohr ein Strahlmittel entweder durch Druckwasser oder Druckluft eingeführt.Another type of treatment is to carry out the annealing in a reducing atmosphere and to remove the resulting carbon film by means of an abrasive. Here, an abrasive is introduced into the tube either by pressurized water or compressed air.
Schließlich ist noch ein Verfahren bekannt, bei dem zur Reinigung der Innenoberfläche installierter Rohrleitungen von ölhaltigen Ablagerungen beispielsweise ein Strahl aus Sandteilchen verwendet wird (EP-A-0 180 228).Finally, a method is known in which, for example, a jet of sand particles is used to clean the inner surface of installed pipelines from oily deposits (EP-A-0 180 228).
Der Erfindung liegt die Aufgabe zugrunde, die Bildung von Kohlenstoff- und/oder Oxidfilmen beim Hartlöten oder Warmbiegen von hartgezogenen Rohren aus Kupfer oder Kupferlegierungen zu verhindern und damit die Lochfraßbeständigkeit dieser Rohre zu verbessern.The invention has for its object to prevent the formation of carbon and / or oxide films during brazing or hot bending of hard drawn tubes made of copper or copper alloys and thus to improve the pitting resistance of these tubes.
Diese Aufgabe wird bei einem Verfahren der eingangs genannten Art erfindungsgemäß dadurch gelöst, daß die Rohre zum Entfetten in ein organisches Lösungsmittelbad getaucht werden und die Innenoberfläche der Rohre anschließend während eines Zeitraums von etwa 3 bis 30 s mit einem Strahl aus Sand- oder Korundteilchen derart behandelt wird, daß die Innenoberfläche der gestrahlten Rohre einen Mittenrauhwert von 0,4 bis 1,5 um aufweist.This object is achieved according to the invention in a method of the type mentioned at the outset by immersing the tubes for degreasing in an organic solvent bath and then treating the inner surface of the tubes with a jet of sand or corundum particles for a period of about 3 to 30 s that the inner surface of the blasted tubes has an average roughness of 0.4 to 1.5 µm.
Vorteilhafte Weiterbildungen sind in den Unteransprüchen angegeben.Advantageous further developments are specified in the subclaims.
Das Verfahren gemäß der Lehre der Erfindung unterscheidet sich von den bisher bekannten im wesentlichen weichgeglühte Kupferrohre betreffenden Verfahren durch eine Kombination chemischer und mechanischer Behandlungsstufen. Mit dem erfindungsgemäßen Verfahren gelingt es in überraschender Weise, die Bildung von schädlichen Filmen, z. B. kohlenstoffhaltigen Filmen oder Oxidfilmen, auf der Innenoberfläche von hartgezogenen Kupferrohren zu vermeiden. Diese nach der Theorie als bipolare Elektroden wirkenden Filme entstehen in der Regel bei den beim Hartlöten oder Warmbiegen von Kupferrohren üblichen Temperaturen.The method according to the teaching of the invention differs from the previously known essentially soft-annealed copper tubes-related methods by a combination of chemical and mechanical treatment stages. With the method according to the invention, it is surprisingly possible to form harmful films, eg. B. carbon-containing films or oxide films on the inner surface of hard-drawn copper pipes. These films, which according to the theory act as bipolar electrodes, are usually produced at the temperatures customary for brazing or hot bending copper pipes.
Eingehende Untersuchungen haben gezeigt, daß die schädlichen Filme im wesentlichen dadurch vermieden werden können, daß die vom Ziehöl weitgehend befreite Innenoberfläche von Kupferrohren nach der zusätzlichen Strahlbehandlung eine gewisse Mindestrauhigkeit aufweist. Es kommt also darauf an, daß an der Innenoberfläche der Rohre eine bestimmte Oberflächenstruktur erzielt wird, die den bei einer Wärmebehandlung entstehenden Filmen nur eine sehr geringe Haftung ermöglicht. Stabile Korrosionselemente, die für das Entstehen der Lochfraßkorrosion ursächlich sind, können sich somit nicht ausbilden. Nach einer bevorzugten Ausführungsform wird die Strahlmittelbehandlung derart durchgeführt, daß die Innenoberfläche der Rohre einen Mittenrauhwert zwischen 0,8 um und 1,0 um aufweist.In-depth investigations have shown that the harmful films can essentially be avoided in that the inner surface of copper pipes, which has largely been freed from the drawing oil, has a certain minimum roughness after the additional blasting treatment. It is therefore important that a certain surface structure is achieved on the inner surface of the tubes, which enables only very little adhesion to the films formed during heat treatment. Stable corrosion elements, which are the cause of pitting corrosion, cannot develop. According to a preferred embodiment, the abrasive treatment is carried out in such a way that the inner surface of the tubes has a mean roughness value between 0.8 µm and 1.0 µm.
Die Erfindung wird nachfolgend anhand von Ausführungsbeispielen noch näher erläutert.The invention is explained in more detail below on the basis of exemplary embodiments.
Auf Endabmessung hartgezogene 5 m lange Rohre aus SF- Cu mit einem Durchmesser von 15 mm und einer Wanddicke von 1 mm wurden in einer ersten Behandlungsstufe zum Entfernen des Ziehöls in ein Lösungsmittelbad aus Trichlorethylen getaucht. In einer weiteren Behandlungsstufe wurden die Kupferrohre an die Strahldüse einer Strahlanlage angeschlossen und 5 s lang mit Korund der Körnung 54 (entsprechend einem mittleren Teilchendurchmesser von 300 bis 350 um) behandelt. Der Strahlmitteldruck betrug etwa 0,55 MPa. Um die Innenoberfläche der Rohre je nach späterem Einsatzfall von Korundteilchen zu reinigen, kann beispielsweise ein den Rohrquerschnitt ausfüllender Filzstopfen eingebracht und der gegebenenfalls mit einem Reinigungsmittel getränkte Filzstopfen dann mittels Druck durch die Rohrlänge transportiert werden. Vielfach wird schon ein einfaches Ausblasen mit Preßluft völlig ausreichend sein, um an der Rohrinnenwand haftende Korundteilchen zu beseitigen. Der Mittenrauhwert Ra wurde mit 0,8 um bestimmt. Der Restkohlenstoffgehalt lag mit < 0,03 mg/dm2 unterhalb der Nachweisgrenze. Langzeitversuche in verschiedenen korrosionsfördernden Haushaltswässern ergaben keine signifikante Ausbildung von Lochkorrosion. Ebenso traten nach dem Hartlöten und/oder Warmbiegen keine Korrosionsschäden auf.5 m long pipes made of SF-Cu with a diameter of 15 mm and a wall thickness of 1 mm, hard-drawn to their final dimensions, were immersed in a trichlorethylene solvent bath in a first treatment step to remove the drawing oil. In a further treatment stage, the copper tubes were connected to the blasting nozzle of a blasting system and treated with 54-corundum (corresponding to an average particle diameter of 300 to 350 μm) for 5 s. The abrasive pressure was about 0.55 MPa. In order to clean the inner surface of the pipes from corundum particles depending on the later application, a felt plug filling the pipe cross-section can be inserted, for example, and the felt plug, which may be soaked with a cleaning agent, can then be transported through the pipe length by means of pressure. In many cases, simply blowing out with compressed air will be sufficient to remove corundum particles adhering to the inner wall of the pipe. The average roughness R a was found to be 0.8 μm. The residual carbon content was <0.03 mg / dm 2 below the detection limit. Long-term tests in various corrosion-promoting household waters did not show any significant formation of pitting corrosion. Likewise, no corrosion damage occurred after brazing and / or hot bending.
Entsprechend den in Beispiel 1 angegebenen Verfahrensbedingungen wurden auf Endmaß gezogene Rohre der Abmessung 22 x 1 mm verwendet. In Abänderung des Verfahrens wurden die Rohre 10 s lang mit Korund behandelt. Der Mittenrauhwert Ra betrug nach der Strahlmittelbehandlung 1,0 um. Der Restkohlenstoff- bzw. Restschmiermittelgehalt lag wiederum unterhalb der Nachweisgrenze.In accordance with the process conditions given in Example 1, tubes measuring 22 x 1 mm were used. In a modification of the process, the tubes were treated with corundum for 10 s. The average roughness value R a was 1.0 μm after the blasting agent treatment. The residual carbon or lubricant content was again below the detection limit.
In weiterer Abwandlung der bisher angegebenen Verfahrensbedingungen wurden auf Endabmessung 15 x 1 mm gezogene Rohre zunächst mit Trichlorethan entfettet, getrocknet und dann kurzzeitig in ein Salpetersäurebad getaucht. Die weiteren Verfahrensbedingungen für die Strahlmittelbehandlung entsprachen denen des Beispiels 1. Langzeitversuche von fünf in Gebieten mit lochfraßbegünstigenden Wässern praxisnah betriebenen Prüfständen ergaben keine Anzeichen von Lochfraßangriff. Die Innenoberfläche der Rohre hatte ein blankes metallisches Aussehen. Der Wasserdurchsatz betrug während der Durchflußzeiten etwa 1,5 I/min, der beim Prüfrohr einer mittleren Strömungsgeschwindigkeit von etwa 0,2 m/s entspricht.In a further modification of the process conditions given so far, tubes 15 x 1 mm drawn to the final dimension were first degreased with trichloroethane, dried and then briefly immersed in a nitric acid bath. The other process conditions for the blasting agent treatment corresponded to those of Example 1. Long-term tests of five test benches operated in practice with areas that favor pitting corrosion did not show any signs of pitting attack. The inside surface of the pipes had a shiny metallic appearance. The water throughput during the flow times was about 1.5 l / min, which corresponds to an average flow velocity of about 0.2 m / s for the test tube.
Claims (7)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT88114157T ATE103225T1 (en) | 1987-09-10 | 1988-08-31 | PROCESS FOR THE MANUFACTURE OF PITTING RESISTANT HARD DRAWN COPPER OR COPPER ALLOY PIPES. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3730367 | 1987-09-10 | ||
DE3730367A DE3730367C2 (en) | 1987-09-10 | 1987-09-10 | Process for the production of pitting-resistant hard drawn tubes made of copper or copper alloys |
Publications (4)
Publication Number | Publication Date |
---|---|
EP0306810A2 EP0306810A2 (en) | 1989-03-15 |
EP0306810A3 EP0306810A3 (en) | 1990-05-30 |
EP0306810B1 true EP0306810B1 (en) | 1994-03-23 |
EP0306810B2 EP0306810B2 (en) | 2000-03-29 |
Family
ID=6335681
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP88114157A Expired - Lifetime EP0306810B2 (en) | 1987-09-10 | 1988-08-31 | Method of producing pitting-resistant hard drawn tubes made of copper or copper-based alloys |
Country Status (11)
Country | Link |
---|---|
EP (1) | EP0306810B2 (en) |
AT (1) | ATE103225T1 (en) |
DE (2) | DE3730367C2 (en) |
DK (2) | DK493288D0 (en) |
ES (1) | ES2050684T5 (en) |
FI (1) | FI94496B (en) |
GR (1) | GR3033568T3 (en) |
IE (1) | IE63028B1 (en) |
PL (1) | PL163146B1 (en) |
PT (1) | PT88473B (en) |
YU (1) | YU46572B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4417455C2 (en) | 1994-05-19 | 1997-09-25 | Wieland Werke Ag | Use of a corrosion-resistant tube with inner oxide layers |
FI107543B (en) | 1998-07-30 | 2001-08-31 | Outokumpu Oy | A method for making a copper tube |
FI20001467A (en) * | 2000-06-20 | 2001-12-21 | Outokumpu Oy | Process for making internally coated copper or copper alloy tubes |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2308436A1 (en) * | 1975-04-25 | 1976-11-19 | Cit Alcatel | Avoiding carbon deposits during annealing, from lubricants - in the bore of drawn copper tubes, by sweeping with nitrogen |
LU81564A1 (en) * | 1979-07-31 | 1981-03-24 | Liege Usines Cuivre Zinc | METHOD FOR MANUFACTURING TUBES, TUBES OBTAINED BY THIS PROCESS AND THEIR USE IN CONDENSERS AND HEAT EXCHANGERS |
DE3018036A1 (en) * | 1980-05-10 | 1981-11-12 | Kabel- und Metallwerke Gutehoffnungshütte AG, 3000 Hannover | METHOD OF TREATING COPPER PIPES |
IT1160196B (en) * | 1983-02-24 | 1987-03-04 | Dalmine Spa | HOT DEOXIDATION PROCESS OF SEMI-FINISHED METAL TUBES |
DE3415376A1 (en) * | 1984-04-25 | 1985-11-07 | Uhlmann, Otto, 3167 Burgdorf | Method and apparatus for degreasing tubes |
US4579596A (en) * | 1984-11-01 | 1986-04-01 | Union Carbide Corporation | In-situ removal of oily deposits from the interior surfaces of conduits |
-
1987
- 1987-09-10 DE DE3730367A patent/DE3730367C2/en not_active Expired - Fee Related
-
1988
- 1988-08-31 EP EP88114157A patent/EP0306810B2/en not_active Expired - Lifetime
- 1988-08-31 DE DE88114157T patent/DE3888605D1/en not_active Expired - Fee Related
- 1988-08-31 ES ES88114157T patent/ES2050684T5/en not_active Expired - Lifetime
- 1988-08-31 AT AT88114157T patent/ATE103225T1/en not_active IP Right Cessation
- 1988-09-02 FI FI884071A patent/FI94496B/en not_active Application Discontinuation
- 1988-09-05 DK DK493288A patent/DK493288D0/en not_active Application Discontinuation
- 1988-09-06 DK DK495488A patent/DK170250B1/en not_active IP Right Cessation
- 1988-09-07 IE IE270788A patent/IE63028B1/en not_active IP Right Cessation
- 1988-09-07 PL PL88274547A patent/PL163146B1/en not_active IP Right Cessation
- 1988-09-08 YU YU171088A patent/YU46572B/en unknown
- 1988-09-09 PT PT88473A patent/PT88473B/en not_active IP Right Cessation
-
2000
- 2000-05-31 GR GR20000401261T patent/GR3033568T3/en not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
ES2050684T3 (en) | 1994-06-01 |
PL274547A1 (en) | 1989-05-02 |
PL163146B1 (en) | 1994-02-28 |
EP0306810B2 (en) | 2000-03-29 |
GR3033568T3 (en) | 2000-09-29 |
YU171088A (en) | 1990-04-30 |
DE3730367C2 (en) | 1997-10-09 |
ATE103225T1 (en) | 1994-04-15 |
DK493288D0 (en) | 1988-09-05 |
EP0306810A3 (en) | 1990-05-30 |
DE3888605D1 (en) | 1994-04-28 |
ES2050684T5 (en) | 2000-07-01 |
FI884071A (en) | 1989-03-11 |
EP0306810A2 (en) | 1989-03-15 |
PT88473B (en) | 1992-11-30 |
FI94496B (en) | 1995-06-15 |
YU46572B (en) | 1993-11-16 |
IE63028B1 (en) | 1995-03-22 |
DK170250B1 (en) | 1995-07-17 |
DK495488A (en) | 1989-03-11 |
DK495488D0 (en) | 1988-09-06 |
IE882707L (en) | 1989-03-10 |
PT88473A (en) | 1988-10-01 |
FI884071A0 (en) | 1988-09-02 |
DE3730367A1 (en) | 1989-03-23 |
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