EP0322650B1 - Verfahren zur Bleichung und Sterilisierung von Gegenständen aus Kork und gebleichte Korkgegenstände mittels dieses Verfahrens - Google Patents

Verfahren zur Bleichung und Sterilisierung von Gegenständen aus Kork und gebleichte Korkgegenstände mittels dieses Verfahrens Download PDF

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Publication number
EP0322650B1
EP0322650B1 EP88120920A EP88120920A EP0322650B1 EP 0322650 B1 EP0322650 B1 EP 0322650B1 EP 88120920 A EP88120920 A EP 88120920A EP 88120920 A EP88120920 A EP 88120920A EP 0322650 B1 EP0322650 B1 EP 0322650B1
Authority
EP
European Patent Office
Prior art keywords
hydrogen peroxide
articles
cork
peroxide solution
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
EP88120920A
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English (en)
French (fr)
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EP0322650A1 (de
Inventor
Giovanni Zucchini
Amerigo Donati
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.)
Solvay Interox SpA
Original Assignee
Interox Chimica SpA
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 Interox Chimica SpA filed Critical Interox Chimica SpA
Priority to AT88120920T priority Critical patent/ATE74818T1/de
Publication of EP0322650A1 publication Critical patent/EP0322650A1/de
Application granted granted Critical
Publication of EP0322650B1 publication Critical patent/EP0322650B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B67—OPENING, CLOSING OR CLEANING BOTTLES, JARS OR SIMILAR CONTAINERS; LIQUID HANDLING
    • B67B—APPLYING CLOSURE MEMBERS TO BOTTLES JARS, OR SIMILAR CONTAINERS; OPENING CLOSED CONTAINERS
    • B67B1/00—Closing bottles, jars or similar containers by applying stoppers
    • B67B1/03—Pretreatment of stoppers, e.g. cleaning, steaming, heating, impregnating or coating; Applying resilient rings to stoppers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/16—Inorganic impregnating agents
    • B27K3/20—Compounds of alkali metals or ammonium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
    • B27K5/003—Treating of wood not provided for in groups B27K1/00, B27K3/00 by using electromagnetic radiation or mechanical waves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
    • B27K5/02—Staining or dyeing wood; Bleaching wood
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
    • B27K5/04—Combined bleaching or impregnating and drying of wood
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K7/00—Chemical or physical treatment of cork

Definitions

  • the present invention relates to a process for bleaching and sterilizing cork articles using an aqueous solution of hydrogen peroxide.
  • this method has the disadvantage of requiring complex treatment in multiple stages using acidic and basic solutions and of not allowing the cork articles to be bleached at a sufficiently high whiteness level required by most uses of these articles. .
  • the invention overcomes these disadvantages of known methods by providing a new method of bleaching and sterilization of cork articles using an aqueous solution of hydrogen peroxide which makes it possible to obtain high whiteness and which does not require intermediate stages of treatment of the articles between the bleaching stage and the drying step.
  • the invention relates to a process for bleaching and sterilizing cork articles by means of an aqueous alkaline solution of hydrogen peroxide, according to which, after treatment of the articles with the hydrogen peroxide solution, the articles, impregnated with hydrogen peroxide, in the presence of ultraviolet radiation.
  • cork articles to which the process according to the invention applies are indifferently decorative or utilitarian objects made up, at least for the major part of their structure, of the natural product that is the cork supplied by the bark of cork oaks.
  • alkaline aqueous solution of hydrogen peroxide is intended to denote an aqueous solution which contains at least one alkaline substance and hydrogen peroxide at a rate of 10 to 300 g H2O2 per liter.
  • solutions are used which contain from 30 to 150 g H2O2 per liter.
  • the alkaline substance used in the aqueous solution is an inorganic chemical compound capable of fixing the pH of the solution in the alkaline zone greater than 8.5 when it is dissolved in water.
  • One of these compounds can be used alone; it is also possible to incorporate several of these compounds as a mixture into the solution. Buffer mixtures of alkaline substances can, for example, be used.
  • the dose of alkaline substance to be incorporated into the hydrogen peroxide solution is advantageously chosen so that the pH of the solution is established in the range between 9.0 and 10.5.
  • Alkaline substances that have worked well are the hydroxide, carbonate and phosphates of alkali metals used separately or as a mixture. The best results have been obtained with sodium hydroxide used at a rate of 2 to 20 g / l of hydrogen peroxide solution or with sodium carbonate at a rate of 5 to 50 g / l of solution.
  • the aqueous solution of hydrogen peroxide may also contain one or more additives usually used in bleaching solutions, such as, for example, stabilizers of hydrogen peroxide, surfactants, agents optical brightening, viscosity or pH regulators, anti-corrosion agents, cork protecting agents.
  • additives usually used in bleaching solutions such as, for example, stabilizers of hydrogen peroxide, surfactants, agents optical brightening, viscosity or pH regulators, anti-corrosion agents, cork protecting agents.
  • any kind of stabilizer known to prevent premature decomposition of hydrogen peroxide into oxygen and water can be incorporated into the hydrogen peroxide solution.
  • examples of such stabilizers are sodium silicate, polyphosphates of alkali metals, organic stabilizers belonging to the class of polyphosphonates or to that of aminopolycarboxylic acids and their salts.
  • Sodium silicate, used in an amount of 2 to 50 g / l of solution, has given good results and is preferred because of its high availability and its low price.
  • surfactant in the hydrogen peroxide solution used in accordance with the invention often proves to be useful for improving the impregnation of cork articles with the hydrogen peroxide solution.
  • a surfactant which is inert with respect to the hydrogen peroxide present in the alkaline aqueous solution.
  • Surfactants according to this wish generally belong to the classes of surfactants anionic, or nonionic such as, for example, polyalkoxylated alcohols with a linear carbon chain.
  • the bleaching process according to the invention comprises two successive stages: a first stage consisting in treating the cork articles with the aqueous solution of hydrogen peroxide and a second stage consisting in drying the articles treated in the first stage.
  • the drying step is carried out by any known drying means or apparatus such as drying with hot air in a ventilated oven, drying by exposure to infrared radiation or drying under partial vacuum.
  • the drying time and temperature are generally not critical. They depend on the drying technique chosen, the surface porosity of the cork articles and the power of UV irradiation. They can be easily determined by laboratory experimentation within the reach of the skilled person. Drying times between 2 and 10 hours and temperatures in the range of 15 to 95 ° C are generally suitable when drying is carried out at atmospheric pressure.
  • the drying is carried out on cork articles impregnated with hydrogen peroxide and in the presence of ultraviolet radiation.
  • the cork articles it is generally advantageous for the cork articles to still contain more than 0.05 g H2O2 / 100 g of cork and, preferably, more than 0.10 g H2O2 / 100 g of cork when exposure to UV radiation begins. 'drying step.
  • ultraviolet radiation is meant an electromagnetic radiation whose wavelength is in the range starting at 200 nm and ending at 350 nm and whose power is at least 5 watts. This radiation is obtained by means of metallic vapor electric lamps well known in the industry, in particular in disinfection techniques.
  • the cork articles can be subjected to the action of ultraviolet radiation during the entire drying time.
  • the cork articles are subjected to ultraviolet radiation during only a fraction of the drying step, preferably during the first part of drying. For example, after an irradiation of 2 to 6 hours in the presence of an ultraviolet, the drying is continued in the absence of UV radiation.
  • the contacting of the aqueous hydrogen peroxide solution with the cork articles can be done indifferently according to various techniques already known by themselves.
  • a contacting technique which has given good results is the technique of immersing the cork articles in a bleaching bath consisting of the hydrogen peroxide solution for a determined time during which the articles can advantageously be stirred in the solution.
  • An embodiment in accordance with this technique consists, for example, of placing the articles in a basket with an openwork or porous wall, immersing the basket in the hydrogen peroxide solution and imparting to it an alternating rotation movement at slow speed during the period of the first stage of treatment.
  • Another technique for bringing cork articles into contact with the hydrogen peroxide solution consists in depositing the articles on a porous surface and spraying them thereon. solution of hydrogen peroxide by sprinkling with a jet of solution which scans the entire surface of the articles to be treated. The hydrogen peroxide solution is collected under the porous surface supporting the cork articles and is recycled to the sprinkler.
  • An interesting technique for bringing cork articles into contact with the hydrogen peroxide solution consists in placing the articles in a basket with an openwork or porous wall, hanging the basket above the hydrogen peroxide solution containing a surfactant with high foaming power, then blowing air into the hydrogen peroxide solution so as to cause the formation of an upward flow of foam which reaches the items in the basket.
  • the concentration of surfactant, the temperature of the solution and the flow rate of the blown air are adjusted so that, in stationary operating conditions, the flow of foam overflows the basket containing the cork articles, then breaks and falls back into the solution.
  • This technique has the advantage of consuming less energy than the techniques already described for immersing or watering the articles to be treated. It also makes it unnecessary to use anti-foaming agents which are often necessary with other techniques.
  • the invention applies to all cork articles.
  • it advantageously applies to cork tiles, panels and plates as well as to cork stoppers used in the bottle industry. It finds a particularly interesting application for bleaching the cork stoppers used in the food industry, especially for sealing the bottles containing liquids such as wine, cider and spirits.
  • the method according to the invention When applied to the bleaching of stoppers, the method according to the invention has the advantage of simplicity compared to conventional hypochlorite methods which require a washing step. It also makes it possible to obtain more extensive bleaching than known processes using hydrogen peroxide and in particular improves the clarity of the stamping of caps intended for food use.
  • the implementation of the method according to the invention allows the elimination of all the chemical agents used in the known methods in the step of washing the plugs, such as citric and tartaric acids, sulfites and hydrochloric acid.
  • the invention also relates to cork articles treated according to the method described above.
  • it relates to cork stoppers, in particular those used for sealing bottles and flasks of wines and spirits.
  • an aqueous solution of hydrogen peroxide was prepared by dissolving in water at 70 ° C a sufficient quantity of commercial hydrogen peroxide solution at 35 g / 100 g. of solution to achieve a H2O2 concentration equal to 100 g / l.
  • a controlled volume of NaOH N was then dissolved therein to obtain, after homogenization, a concentration of 10 g NaOH / l.
  • the pH of the aqueous alkaline hydrogen peroxide solution thus obtained was 9.7.
  • test 1 a hydrogen peroxide solution containing no stabilizer was used.
  • 38 ° Bé sodium silicate was incorporated into the hydrogen peroxide solution, as stabilizer, in respective amounts of 7 g / l (test No. 2) and 70 g / l (test No. 3).
  • Unbleached cork stoppers were enclosed in a stainless steel basket with numerous openings, then the basket was immersed in the beaker containing the aqueous hydrogen peroxide solution and kept there for 1 hour with stirring. the solution continuously using a magnetic stirrer set at 100 revolutions / minute.
  • the cork stoppers were removed from the metal basket, they were drained and placed, without washing them, in a ventilated oven whose hot air flow was adjusted to 50 ° C and which contained a generator. UV radiation in the form of 3 light tubes of the PHILIPS brand and of the TUV-6W type. The drying was then continued in this oven in the presence of UV radiation for 180 minutes.
  • the bleached and dried stoppers were then subjected to a whiteness measurement using a reflectometer of the PHOTOVOLT brand.
  • the results of the whiteness measurements made it possible to calculate, for each stopper, by subtracting the whiteness measured before treatment, the whiteness gain expressed in degrees PHOTOVOLT.
  • Table I gives the extreme whiteness gains obtained.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Detergent Compositions (AREA)
  • Cleaning Implements For Floors, Carpets, Furniture, Walls, And The Like (AREA)
  • Packages (AREA)
  • Gloves (AREA)

Claims (8)

  1. Bleich- und Sterilisierungsverfahren für Korkartikel mittels einer wässrigen alkalischen Lösung von Wasserstoffperoxyd, die 10 bis 300 g H₂O₂ pro Liter enthält, dadurch gekennzeichnet, daß man nach der Behandlung der Artikel durch die Wasserstoffperoxydlösung und durch Weglassen der Waschstufe die von Wasserstoffperoxyd imprägnierten Artikel trocknet, indem man sie der gleichzeitigen Einwirkung einer ultravioletten Strahlung aussetzt, deren Wellenlänge im Bereich beginnend mit 200 nm und endend mit 350 nm liegt und, deren Leistung wenigstens 5 Watt beträgt.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Wasserstoffperoxydlösung eine Stabilisierungsverbindung des Wasserstoffperoxyds enthält.
  3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß das Stabilisierungsmittel Natriumsilikat ist, das in einer Menge von 2 bis 50 g/l Lösung eingesetzt wird.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Wasserstoffperoxydlösung 30 bis 150 g H₂O₂ pro Liter enthält.
  5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Alkalinität der Wasserstoffperoxydlosung derart ist, daß ihr pH zwischen 9,0 und 10,5 liegt.
  6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Alkalinität der Wasserstoffperoxydlösung durch Einsetzen von 2 bis 20 g Natriumhydroxyd pro Liter erhalten wird.
  7. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Alkalinität der Wasserstoffperoxydlösung durch Einsetzen von 5 bis 50 g Natriumcarbonat pro Liter erhalten wird.
  8. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß die Korkartikel mehr als 0,05 g H₂O₂/100 g Kork enthalten, wenn die Belichtung mit UV-Strahlung in der Trocknungsphase beginnt.
EP88120920A 1987-12-30 1988-12-14 Verfahren zur Bleichung und Sterilisierung von Gegenständen aus Kork und gebleichte Korkgegenstände mittels dieses Verfahrens Expired - Lifetime EP0322650B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88120920T ATE74818T1 (de) 1987-12-30 1988-12-14 Verfahren zur bleichung und sterilisierung von gegenstaenden aus kork und gebleichte korkgegenstaende mittels dieses verfahrens.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT8723281A IT1233447B (it) 1987-12-30 1987-12-30 Procedimento di sbianca e di sterilizzazione di articoli in sughero e articoli in sughero sbiancati mediante detto procedimento
IT2328187 1987-12-30

Publications (2)

Publication Number Publication Date
EP0322650A1 EP0322650A1 (de) 1989-07-05
EP0322650B1 true EP0322650B1 (de) 1992-04-15

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP88120920A Expired - Lifetime EP0322650B1 (de) 1987-12-30 1988-12-14 Verfahren zur Bleichung und Sterilisierung von Gegenständen aus Kork und gebleichte Korkgegenstände mittels dieses Verfahrens

Country Status (8)

Country Link
US (1) US5098447A (de)
EP (1) EP0322650B1 (de)
JP (1) JPH01295801A (de)
AT (1) ATE74818T1 (de)
AU (1) AU603893B2 (de)
DE (1) DE3870190D1 (de)
IT (1) IT1233447B (de)
PT (1) PT89361B (de)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2635292B1 (fr) * 1988-08-12 1990-11-16 Henkel France Procede de traitement de bouchons en liege
NZ237321A (en) * 1991-03-05 1994-12-22 Wool Res Organisation Bleaching process for natural fibres using electromagnetic radiation and alkaline peroxide oxidant
US6008268A (en) 1994-10-21 1999-12-28 Kimberly-Clark Worldwide, Inc. Photoreactor composition, method of generating a reactive species, and applications therefor
US5699589A (en) * 1996-05-03 1997-12-23 Ripley; William G. Laser cleaning and bleaching apparatus
US6152966A (en) * 1998-05-13 2000-11-28 Novo Nordisk A/S Treatment of cork with a phenol oxidizing enzyme
JP2000326312A (ja) * 1999-05-24 2000-11-28 Aoi Kokuban Seisakusho:Kk コルク板とその処理方法
JP2003135572A (ja) * 2001-08-20 2003-05-13 Menicon Co Ltd 消毒方法
US20040166345A1 (en) * 2003-02-26 2004-08-26 Wicht Charles A. Processes and articles useful for preventing cork taint in beverages
EP2286845B1 (de) * 2004-03-05 2016-11-16 Gen-Probe Incorporated Reagentien und Verfahren zur Deaktivierung von Nukleinsäuren
JP4500927B2 (ja) * 2004-03-24 2010-07-14 独立行政法人産業技術総合研究所 繊維構造物の漂白方法
PT103117A (pt) * 2004-05-12 2005-11-30 Ct Tecnologico Da Cortica Processo de tratamento da cortica inibidor do desenvolvimento de substancias causadoras de desvios organolepticos
WO2010119462A1 (en) * 2009-04-16 2010-10-21 Colombin & Figlio S.P.A. Process for the abatement of undesired volatile compounds from manufactured and semi-manufactured cork products
KR101926366B1 (ko) * 2016-10-14 2018-12-07 주식회사 서연이화 천연 코르크 필름의 제조 방법
CN114523537A (zh) * 2022-03-16 2022-05-24 东北林业大学 一种紫外光催化的环保型木材漂白处理方法

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR907518A (fr) * 1939-02-06 1946-03-14 Produits Peroxydes Soc D Procédé pour rendre réutilisables les bouchons de liège usagés
NL6511053A (de) * 1964-09-02 1966-03-03
FR1573944A (de) * 1968-02-23 1969-07-11
IN153503B (de) * 1979-01-11 1984-07-21 Nat Res Dev
AU572470B2 (en) * 1982-09-03 1988-05-12 Cork & Seals Pty. Limited Process for treatment of natural cork
IT1178504B (it) * 1984-08-23 1987-09-09 Montefluos Spa Procedimento per il lavaggio di oggetti di sughero
FR2574696B1 (fr) * 1984-12-19 1987-06-05 Champagne M Sabate Sa Bouchons Procede de traitement special pour des produits en liege

Also Published As

Publication number Publication date
PT89361A (pt) 1989-12-29
IT1233447B (it) 1992-04-01
JPH01295801A (ja) 1989-11-29
AU1608588A (en) 1989-07-06
IT8723281A0 (it) 1987-12-30
ATE74818T1 (de) 1992-05-15
DE3870190D1 (de) 1992-05-21
US5098447A (en) 1992-03-24
EP0322650A1 (de) 1989-07-05
PT89361B (pt) 1993-08-31
AU603893B2 (en) 1990-11-29

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