EP0794902B1 - Method and device for removing oxygen from the headspace of a package - Google Patents
Method and device for removing oxygen from the headspace of a package Download PDFInfo
- Publication number
- EP0794902B1 EP0794902B1 EP95936932A EP95936932A EP0794902B1 EP 0794902 B1 EP0794902 B1 EP 0794902B1 EP 95936932 A EP95936932 A EP 95936932A EP 95936932 A EP95936932 A EP 95936932A EP 0794902 B1 EP0794902 B1 EP 0794902B1
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- European Patent Office
- Prior art keywords
- nitrogen
- package
- nozzle
- packages
- injection
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B31/00—Packaging articles or materials under special atmospheric or gaseous conditions; Adding propellants to aerosol containers
- B65B31/04—Evacuating, pressurising or gasifying filled containers or wrappers by means of nozzles through which air or other gas, e.g. an inert gas, is withdrawn or supplied
- B65B31/041—Evacuating, pressurising or gasifying filled containers or wrappers by means of nozzles through which air or other gas, e.g. an inert gas, is withdrawn or supplied the nozzles acting from above on containers or wrappers open at their top
Definitions
- the invention relates to a method for removing oxygen. head space of aseptically filled packaging, in which the packaging is filled in an air atmosphere sterile, sterile nitrogen is then injected with a nozzle disposed directly above the opening of said packaging at room temperature and under pressure atmospheric in a sterile air atmosphere and we seals the packaging between two sealing elements.
- the invention further relates to the device used for the implementation of this process.
- DE-A-3108817 also relates to a device to remove oxygen from the headspace of a packaging.
- the nozzle allowing to inject nitrogen is integral with one of the elements of sealing, which reduces the efficiency of the nitrogen supply, because said nozzle moves and the nitrogen jet changes direction.
- US-A-4,934,127 and EP-A-479,037 also relate to devices for eliminating the headspace oxygen of a package. The disadvantage of these devices is that the sealing of the packaging is done downstream of the injection station nitrogen, which has the effect of letting the quantity of nitrogen introduced beforehand.
- the object of the present invention is the development of a process for removing oxygen from the headspace packaging that is aseptically filled efficiently. By eliminating is meant reaching a content of very low oxygen in the headspace, i.e. around 2% and even less.
- sterile nitrogen is injected from the nozzle which is fixed and disposed between the two mobile sealing elements, nitrogen injection is done from the top at an angle between 40 and 50 ° with respect to the vertical and against the current the direction of movement of the packaging.
- the packaging used can be of any type, but its upper part is sealable.
- the filling product in the packaging can be of any type.
- liquid type from the food industry, for example a product based on milk, fruit juice or water, which can also contain part of pieces.
- the goal is to get products with a long shelf life, for which there is no degradation of taste and / or certain ingredients during storage.
- the process is implemented on a production line classic industrial, in which there is in particular a filling compartment and sealing compartment : it is necessary to add according to the invention in the sealing compartment a nitrogen injection step.
- the two filling and sealing compartments are under sterile air flow so as to create turbulence conditions: the injection speed of nitrogen is greater than the air injection speed sterile.
- the nitrogen flow per line between 100 and 800 l / min at atmospheric pressure.
- the duration of nitrogen injection per package is around of the second. This rapid nitrogen injection allows save the amount of nitrogen and limit the length of the production line. We can also operate with a continuous nitrogen arrival than discontinuous.
- the invention further relates to the device usable for the implementation of the method described above.
- This device includes a filling compartment for product in packaging, sealing compartment said package with two sealing elements and one conveyor device for conveying the packaging in the two compartments, the second compartment comprising a fixed nozzle for injecting nitrogen, this being disposed between the movable sealing elements and being positioned so that it makes an angle between 40 and 50 ° with the vertical, said angle being against the current the direction of movement of the packaging.
- the conveyor device has a step-by-step advancement system and we arrive at a conventional filling rate at this type of line. It is understood that in this description, all that is said concerns a mode of aseptic filling: the nitrogen and the air used are pre-sterilized.
- the packages 1 arrive via the conveyor device 2 in the direction of the arrows 3 in the compartment aseptic filling 4, then in the compartment sealing 5. Sterile air is injected into both above-mentioned compartments respectively by lines 6 and 7.
- the product 8 arrives through the filling system 9 and is dosed in packaging 1 thanks to the nozzle filling 10.
- the sealing compartment 5 comprises the fixed nitrogen injection nozzle 11, the nitrogen arriving via the line 12 and the two sealing elements 13,14.
- Aseptic 4 filling and sealing compartments 5 have openings 15, 16, 17 allowing the passage of the packaging 1 on the conveyor device 2.
- the operation of the device according to the invention is the next:
- the conveyor device 2 has a system step by step.
- Package 1 is positioned under the filling nozzle 10, which then delivers the dose of product 8.
- the compartment is permanently under sterile air atmosphere.
- the transport device then position the other packages under the nozzle 10 and the filled packages arrive in the compartment of seal 5 and pass under the nozzle 11 for injecting nitrogen.
- the nitrogen flow is 300 l / min, the compartment sealing also being permanently under atmosphere sterile air.
- Fig. 2 we can clearly see the operation of sealing with elements 13 and 14.
- the device carrier 2 then delivers the packaging ready to use or storage.
- packaging is thus obtained which can be stored for at least 6 months, without any degraded product quality and taste.
- vitamins as well as mineral salts are in addition preserved.
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Vacuum Packaging (AREA)
- Control And Other Processes For Unpacking Of Materials (AREA)
- Magnetic Resonance Imaging Apparatus (AREA)
- Separation By Low-Temperature Treatments (AREA)
- Storage Of Fruits Or Vegetables (AREA)
Abstract
Description
L'invention concerne un procédé d'élimination d'oxygène de l'espace de tête d'un emballage rempli aseptiquement, dans lequel on remplit l'emballage sous atmosphère d'air stérile, on injecte ensuite de l'azote stérile avec une buse disposée directement au-dessus de l'ouverture dudit emballage à température ambiante et sous la pression atmosphérique dans une atmosphère d'air stérile et on scelle l'emballage entre deux éléments de scellage. L'invention concerne en outre le dispositif utilisé pour la mise en oeuvre de ce procédé.The invention relates to a method for removing oxygen. head space of aseptically filled packaging, in which the packaging is filled in an air atmosphere sterile, sterile nitrogen is then injected with a nozzle disposed directly above the opening of said packaging at room temperature and under pressure atmospheric in a sterile air atmosphere and we seals the packaging between two sealing elements. The invention further relates to the device used for the implementation of this process.
Dans le domaine du remplissage aseptique avec certains types de machine, il n'est pas possible de remplir un emballage et de le sceller sans y laisser un faible volume gazeux, appelé espace de tête. Comme on travaille normalement dans des systèmes avec de l'air stérile, cet espace de tête contient de l'ordre de 20% d'oxygène. La présence d'oxygène a un effet négatif, en ce sens que lors de la conservation du produit contenu dans ledit emballage, il arrive fréquemment que ce produit soit sensible à l'oxygène, ce qui conduit ainsi à une dégradation de son goût et/ou de certains ingrédients, tels que les vitamines et les sels minéraux. Ce phénomène est inacceptable pour le consommateur ou pour des raisons de législation alimentaire. On a déjà envisagé une solution dans laquelle on cherche à réduire l'espace de tête : on opère dans ce cas en remplaçant juste avant le scellage l'air par de la vapeur d'eau. L'inconvénient de ce système est cependant que la vapeur d'eau se condense sur des surfaces froides : la conséquence est un risque inacceptable d'infection pour les produits neutres et faiblement acides. Une seconde solution consiste à réduire l'espace de tête avec des éléments mécaniques en pressant l'emballage : mais il n'est cependant pas possible d'éliminer totalement ledit espace. Le brevet DE-A-3108817 concerne également un dispositif permettant d'éliminer l'oxygène de l'espace de tête d'un emballage. Dans ce dispositif, la buse permettant d'injecter l'azote est solidaire de l'un des éléments de scellage, ce qui diminue l'efficience de l'arrivée d'azote, car ladite buse bouge et le jet d'azote change de direction. Les brevets US-A-4,934,127 et EP-A-479,037 concernent également des dispositifs pour éliminer l'oxygène de l'espace de tête d'un emballage. L'inconvénient de ces dispositifs est que le scellage de l'emballage se fait en aval de la station d'injection d'azote, ce qui a pour conséquence de laisser repartir la quantité d'azote introduite au préalable.In the field of aseptic filling with certain machine types, it is not possible to fill a packaging and seal it without leaving a small volume gas, called headspace. As we work normally in systems with sterile air, this headspace contains around 20% oxygen. The presence of oxygen has a negative effect, in that when the conservation of the product contained in said packaging, this product is frequently sensitive to oxygen, which thus leads to a degradation of its taste and / or certain ingredients, such as vitamins and mineral salts. This phenomenon is unacceptable to the consumer or for reasons of legislation food. We have already considered a solution in which we try to reduce the head space: we operate in this case by replacing the air just before sealing with water vapour. The downside of this system is however that water vapor condenses on cold surfaces: the consequence is an unacceptable risk of infection for neutral and weakly acidic products. A second solution is to reduce the headspace with mechanical elements by pressing the packaging: but it is not however, it is not possible to completely eliminate said space. DE-A-3108817 also relates to a device to remove oxygen from the headspace of a packaging. In this device, the nozzle allowing to inject nitrogen is integral with one of the elements of sealing, which reduces the efficiency of the nitrogen supply, because said nozzle moves and the nitrogen jet changes direction. US-A-4,934,127 and EP-A-479,037 also relate to devices for eliminating the headspace oxygen of a package. The disadvantage of these devices is that the sealing of the packaging is done downstream of the injection station nitrogen, which has the effect of letting the quantity of nitrogen introduced beforehand.
Le but de la présente invention est la mise au point d'un procédé permettant d'éliminer l'oxygène de l'espace de tête d'un emballage rempli aseptiquement de manière efficiente. Par éliminer, on entend le fait d'atteindre une teneur en oxygène très faible dans l'espace de tête, à savoir de l'ordre de 2% et même moins.The object of the present invention is the development of a process for removing oxygen from the headspace packaging that is aseptically filled efficiently. By eliminating is meant reaching a content of very low oxygen in the headspace, i.e. around 2% and even less.
Selon le procédé de l'invention, on injecte l'azote stérile à partir de la buse qui est fixe et disposée entre les deux éléments de scellage mobiles, l'injection d'azote est faite depuis le haut sous un angle compris entre 40 et 50° par rapport à la verticale et à contre-courant du sens de déplacement des emballages.According to the process of the invention, sterile nitrogen is injected from the nozzle which is fixed and disposed between the two mobile sealing elements, nitrogen injection is done from the top at an angle between 40 and 50 ° with respect to the vertical and against the current the direction of movement of the packaging.
On améliore ainsi l'efficacité d'élimination de l'air résiduel dans l'espace de tête grâce à cette disposition spécifique de l'arrivée du courant d'azote. This improves the efficiency of removing residual air in the headspace thanks to this specific arrangement of the arrival of the nitrogen current.
L'emballage utilisé peut être de tout type, pouvu que sa partie supérieure soit scellable.The packaging used can be of any type, but its upper part is sealable.
Le produit de remplissage de l'emballage peut être de tout type liquide du domaine alimentaire, par exemple un produit à base de lait, de jus de fruit ou d'eau, pouvant en outre contenir une partie de morceaux. On préfère tout particulièrement les produits sensibles à l'oxygène et faiblement acides, comme les produits diététiques contenant des vitamines et des sels minéraux. Le but est d'obtenir des produits à longue durée de conservation, pour lesquels il n'y a pas de dégradation du goût et/ou de certains ingrédients lors du stockage.The filling product in the packaging can be of any type. liquid type from the food industry, for example a product based on milk, fruit juice or water, which can also contain part of pieces. We prefer everything particularly oxygen sensitive products and weakly acidic, such as dietetic products containing vitamins and minerals. The goal is to get products with a long shelf life, for which there is no degradation of taste and / or certain ingredients during storage.
Le procédé est mis en oeuvre sur une ligne de fabrication industrielle classique, dans laquelle il y a notamment un compartiment de remplissage et un compartiment de scellage : il faut rajouter selon l'invention dans le compartiment de scellage une étape d'injection d'azote.The process is implemented on a production line classic industrial, in which there is in particular a filling compartment and sealing compartment : it is necessary to add according to the invention in the sealing compartment a nitrogen injection step.
Les deux compartiments de remplissage et de scellage sont sous courant d'air stérile de manière à y créer des conditions de turbulence : la vitesse d'injection de l'azote est supérieure à la vitesse d'injection d'air stérile. Pour parvenir à un espace de tête ayant une teneur en oxygène de moins de 2 96, il faut travailler avec un débit d'azote par ligne compris entre 100 et 800 l/min à pression atmosphèrique.The two filling and sealing compartments are under sterile air flow so as to create turbulence conditions: the injection speed of nitrogen is greater than the air injection speed sterile. To achieve a headspace with content oxygen less than 2 96, you have to work with a nitrogen flow per line between 100 and 800 l / min at atmospheric pressure.
La durée d'injection d'azote par emballage est de l'ordre de la seconde. Cette rapide injection d'azote permet d'économiser la quantité d'azote et limite la longueur de la ligne de production. On peut aussi bien opérer avec une arrivée d'azote continue que discontinue.The duration of nitrogen injection per package is around of the second. This rapid nitrogen injection allows save the amount of nitrogen and limit the length of the production line. We can also operate with a continuous nitrogen arrival than discontinuous.
L'invention concerne en outre le dispositif utilisable pour la mise en oeuvre du procédé décrit ci-dessus. Ce dispositif comprend un compartiment de remplissage de produit dans un emballage, un compartiment de scellage dudit emballage avec deux éléments de scellage et un dispositif transporteur pour véhiculer les emballages dans les deux compartiments, le second compartiment comportant une buse fixe pour injecter l'azote, celle-ci étant disposée entre les éléments de scellage mobiles et étant positionnée de manière à ce qu'elle fasse un angle compris entre 40 et 50° avec la verticale, ledit angle étant à contre-courant du sens de déplacement des emballages.The invention further relates to the device usable for the implementation of the method described above. This device includes a filling compartment for product in packaging, sealing compartment said package with two sealing elements and one conveyor device for conveying the packaging in the two compartments, the second compartment comprising a fixed nozzle for injecting nitrogen, this being disposed between the movable sealing elements and being positioned so that it makes an angle between 40 and 50 ° with the vertical, said angle being against the current the direction of movement of the packaging.
Le dispositif transporteur à un système d'avancée au pas-à-pas et on arrive à une cadence de remplissage classique à ce type de ligne. Il est bien entendu que dans la présente description, tout ce qui est dit concerne un mode de remplissage aseptique : l'azote et l'air utilisé sont préstérilisés.The conveyor device has a step-by-step advancement system and we arrive at a conventional filling rate at this type of line. It is understood that in this description, all that is said concerns a mode of aseptic filling: the nitrogen and the air used are pre-sterilized.
On dispose dans la buse d'arrivée d'azote un répartiteur et des moyens supplémentaires, tels qu'une ou plusieurs plaques métalliques permettant d'obtenir des flux uniformes à la sortie de la buse.There is a distributor in the nitrogen inlet nozzle and additional means, such as one or more metal plates for uniform flow at the outlet of the nozzle.
Il faut également que le flux d'azote arrive sur une
largeur suffisante pour bien déplacer l'air résiduel de
l'espace de tête : on prévoit une largeur de buse
supérieure à la largeur d'ouverture de l'emballage. La
suite de la description est faite en référence aux dessins
sur lesquels :
Les emballages 1 arrivent par le dispositif transporteur 2
dans le sens des flèches 3 dans le compartiment de
remplissage aseptique 4, puis dans le compartiment de
scellage 5. De l'air stérile est injecté dans les deux
compartiments précités respectivement par les conduites 6
et 7. Le produit 8 arrive par le système de remplissage 9
et est dosé dans l'emballage 1 grâce à la buse de
remplissage 10. Le compartiment de scellage 5 comprend la
buse fixe 11 d'injection d'azote, l'azote arrivant par la
conduite 12 ainsi que les deux éléments de scellage 13,14.The packages 1 arrive via the
Les compartiments de remplissage aseptique 4 et de scellage
5 comportent des ouvertures 15, 16, 17 permettant le
passage des emballages 1 sur le dispositif transporteur 2.Aseptic 4 filling and
Le fonctionnement du dispositif selon l'invention est le
suivant : Le dispositif transporteur 2 a un système
d'avancée pas-à-pas. L'emballage 1 est positionné sous la
buse de remplissage 10, qui délivre alors la dose de
produit 8. Le compartiment est en permanence sous
atmosphère d'air stérile. Le dispositif transporteur
positionne ensuite les autres emballages sous la buse 10 et
les emballages remplis arrivent dans le compartiment de
scellage 5 et passent sous la buse 11 d'injection d'azote.
Le débit d'azote est de 300 l/min, le compartiment de
scellage étant lui aussi en permanence sous atmosphère
d'air stérile. Dans la Fig. 2, on voit bien l'opération de
scellage avec les éléments 13 et 14. Le dispositif
transporteur 2 délivre alors les emballages prêts à
l'emploi ou au stockage.The operation of the device according to the invention is the
next: The
On obtient ainsi selon l'invention des emballages qui peuvent être stockés pendant au moins 6 mois, sans aucune dégradation de la qualité et du goût du produit. Les vitamines ainsi que les sels minéraux sont en outre préservés. Dans l'exemple précité, on arrive à une teneur en oxygène de 1% dans l'espace de tête.According to the invention, packaging is thus obtained which can be stored for at least 6 months, without any degraded product quality and taste. The vitamins as well as mineral salts are in addition preserved. In the above example, we arrive at a content 1% oxygen in the headspace.
Claims (8)
- Method for removing oxygen from the headspace of an aseptically filled package (1), wherein the package (1) is filled in a sterile air atmosphere, sterile nitrogen is then injected with a nozzle (11) disposed directly above the opening of the said package at ambient temperature and at atmospheric pressure in a sterile air atmosphere and the package is sealed with two sealing elements (13, 14), characterized in that sterile nitrogen is injected from the nozzle (11) which is fixed and disposed between the two movable sealing elements (13, 14) and in that nitrogen is injected from above at an angle of the order of 40-50° with respect to the vertical and counter-current to the direction of movement of the packages.
- Method according to claim 1, characterized in that the nitrogen injection lasts for a period of the order of one second per package.
- Method according to either of claims 1 or 2, characterized in that nitrogen is injected in a continuous or discontinuous manner.
- Method according to one of claims 1 to 3, characterized in that the rate of injection of nitrogen is greater than the rate of injection of sterile air.
- Method according to one of claims 1 to 4, characterized in that the rate of injection of nitrogen per line is between 100 and 800 l/min.
- Device for implementing the method according to one of claims 1 to 5, comprising a compartment (4) for aseptically filling a product into a package (1), a compartment (5) for sealing the said package with two sealing elements (13, 14) and a transporting device (2) for conveying the packages into the two compartments (4, 5), characterized in that the second compartment (5) has a fixed nozzle (11) for injecting nitrogen, the said nozzle being disposed between the movable sealing elements (13, 14) and in that the nozzle (11) makes an angle of between 40° and 50° with the vertical, the said angle being counter-current to the direction of movement of the packages.
- Device according to claim 6, characterized in that the nozzle has a distributor.
- Device according to either of claims 6 or 7, characterized in that the nozzle (11) is wider than the package (1).
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP94119203 | 1994-12-06 | ||
| AT94119/20 | 1994-12-06 | ||
| EP94119203 | 1994-12-06 | ||
| PCT/CH1995/000290 WO1996017775A1 (en) | 1994-12-06 | 1995-12-05 | Method and device for removing oxygen from the headspace of a package |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0794902A1 EP0794902A1 (en) | 1997-09-17 |
| EP0794902B1 true EP0794902B1 (en) | 1999-04-07 |
Family
ID=8216506
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP95936932A Expired - Lifetime EP0794902B1 (en) | 1994-12-06 | 1995-12-05 | Method and device for removing oxygen from the headspace of a package |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US5896727A (en) |
| EP (1) | EP0794902B1 (en) |
| JP (1) | JPH11500394A (en) |
| AT (1) | ATE178547T1 (en) |
| AU (1) | AU688160B2 (en) |
| BR (1) | BR9509963A (en) |
| DE (1) | DE69508958T2 (en) |
| DK (1) | DK0794902T3 (en) |
| ES (1) | ES2131869T3 (en) |
| GR (1) | GR3030005T3 (en) |
| PL (1) | PL177976B1 (en) |
| RU (1) | RU2139229C1 (en) |
| WO (1) | WO1996017775A1 (en) |
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| IT987875B (en) * | 1972-06-09 | 1975-03-20 | Hesser Ag Maschf | APPARATUS FOR PRODUCING OXYGEN POOR PACKAGING MEANS |
| US4081942A (en) * | 1976-08-02 | 1978-04-04 | Rexham Corporation | Machine and method for filling, introducing steam into, and sealing flexible pouches |
| DE3108817C2 (en) * | 1981-03-09 | 1984-01-05 | Jagenberg-Werke AG, 4000 Düsseldorf | Device for folding and closing the head part of filled collapsible containers and for removing oxygen from the headspace of the collapsible container |
| FR2572708B1 (en) * | 1984-11-02 | 1990-02-09 | Jujo Paper Co Ltd | PAPER CONTAINER FOR LIQUIDS, AND METHOD AND APPARATUS FOR FILLING AND SEALING THE CONTAINER |
| US4788811A (en) * | 1986-05-17 | 1988-12-06 | Dai Nippon Insatsu Kabushiki Kaisha | Process and apparatus for assembling and liquor-charging of packages of paper and the like |
| DE3834184C1 (en) * | 1988-10-07 | 1989-12-28 | Bernd 7166 Sulzbach-Laufen De Hansen | |
| US4934127A (en) * | 1989-06-07 | 1990-06-19 | Elopak Systems A.G. | Apparatus for packaging in a protective atmosphere |
| US5085035A (en) * | 1990-10-05 | 1992-02-04 | International Paper Company | Gas displacement device for packaging food and non-food products |
| US5271207A (en) * | 1992-11-18 | 1993-12-21 | Moshe Epstein | Dual-function nozzle head for vacuum-packaging tooling |
-
1995
- 1995-12-05 AT AT95936932T patent/ATE178547T1/en not_active IP Right Cessation
- 1995-12-05 BR BR9509963A patent/BR9509963A/en not_active IP Right Cessation
- 1995-12-05 WO PCT/CH1995/000290 patent/WO1996017775A1/en active IP Right Grant
- 1995-12-05 EP EP95936932A patent/EP0794902B1/en not_active Expired - Lifetime
- 1995-12-05 PL PL95320533A patent/PL177976B1/en not_active IP Right Cessation
- 1995-12-05 RU RU97111206A patent/RU2139229C1/en not_active IP Right Cessation
- 1995-12-05 AU AU39218/95A patent/AU688160B2/en not_active Ceased
- 1995-12-05 US US08/849,496 patent/US5896727A/en not_active Expired - Fee Related
- 1995-12-05 ES ES95936932T patent/ES2131869T3/en not_active Expired - Lifetime
- 1995-12-05 DE DE69508958T patent/DE69508958T2/en not_active Expired - Fee Related
- 1995-12-05 DK DK95936932T patent/DK0794902T3/en active
- 1995-12-05 JP JP8517222A patent/JPH11500394A/en active Pending
-
1999
- 1999-04-20 GR GR990401084T patent/GR3030005T3/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| GR3030005T3 (en) | 1999-07-30 |
| ES2131869T3 (en) | 1999-08-01 |
| AU688160B2 (en) | 1998-03-05 |
| RU2139229C1 (en) | 1999-10-10 |
| WO1996017775A1 (en) | 1996-06-13 |
| PL177976B1 (en) | 2000-02-29 |
| EP0794902A1 (en) | 1997-09-17 |
| US5896727A (en) | 1999-04-27 |
| DK0794902T3 (en) | 1999-10-18 |
| JPH11500394A (en) | 1999-01-12 |
| PL320533A1 (en) | 1997-10-13 |
| DE69508958D1 (en) | 1999-05-12 |
| AU3921895A (en) | 1996-06-26 |
| BR9509963A (en) | 1997-11-25 |
| ATE178547T1 (en) | 1999-04-15 |
| DE69508958T2 (en) | 1999-09-09 |
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