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EP1061123A1 - Automatic dish-washing machine cleaning process and compositions relating thereto - Google Patents

Automatic dish-washing machine cleaning process and compositions relating thereto Download PDF

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Publication number
EP1061123A1
EP1061123A1 EP00303177A EP00303177A EP1061123A1 EP 1061123 A1 EP1061123 A1 EP 1061123A1 EP 00303177 A EP00303177 A EP 00303177A EP 00303177 A EP00303177 A EP 00303177A EP 1061123 A1 EP1061123 A1 EP 1061123A1
Authority
EP
European Patent Office
Prior art keywords
washing machine
dish washing
automatic dish
cleaner
surfactant
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.)
Granted
Application number
EP00303177A
Other languages
German (de)
French (fr)
Other versions
EP1061123B1 (en
EP1061123B2 (en
Inventor
Alan Digby Unilever Resrch.Vlaardingen Tomlinson
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.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=26073120&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP1061123(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Priority to EP00303177A priority Critical patent/EP1061123B2/en
Publication of EP1061123A1 publication Critical patent/EP1061123A1/en
Publication of EP1061123B1 publication Critical patent/EP1061123B1/en
Priority to TW094305092F priority patent/TWD114205S1/en
Application granted granted Critical
Publication of EP1061123B2 publication Critical patent/EP1061123B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2086—Hydroxy carboxylic acids-salts thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/72—Ethers of polyoxyalkylene glycols
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces

Definitions

  • the present invention is in the field of machine dishwashing. More specifically, the invention encompasses a cleaner for automatic dishwashing machines.
  • the present invention relates to a composition used to clean dish washing machines. Such cleaning compositions are frequently used by the consumer to clean the dish washer itself and so remove deposits after the machine has been used to clean crockery.
  • the present invention relates to a composition for cleaning dish washers in which the problem of co-agulation is mitigated.
  • an automatic dish washing machine cleaner comprising at least 50% wt of the total composition of a partially or fully hydrated organic acid and at least 0.5 % wt of the total composition of a surfactant
  • the present invention also provides the use of citric acid monohydrate in a dish washing machine cleaner to prevent mass solidification.
  • compositions of the present invention comprise a partially or fully hydrated organic acid as an essential element.
  • Suitable partially or fully hydrated organic acids organic acids include, for example, carboxylic acids, such as citric and succinic acids, polycarboxylic acids, such as polyacrylic acid, and also acetic acid, boric acid, malonic acid, adipic acid, fumaric acid, lactic acid, glycolic acid, sulphamic acid, tartaric acid, tartronic acid, maloic acid, their derivatives and any mixtures of the foregoing.
  • Suitable water-soluble monomeric or oligomeric carboxylates can be selected from a wide range of compounds but such compounds preferably have a first carboxyl logarithmic acidity/constant (pK 1 ) of less than 9, preferably of between 2 and 8.5, more preferably of between 2.5 and 7.5.
  • pK 1 first carboxyl logarithmic acidity/constant
  • Polycarboxylic acids containing four carboxy groups include oxydisuccinic acids, 1,1,2,2-ethane tetracarboxylic acids, 1,1,3,3-propane tetracarboxylic acids and 1,1,2,3-propane tetracarboxylic acids.
  • Polycarboxylic acids containing sulfo substituents include the sulfosuccinic derivatives, and the sulfonated pyrolysed citratic acids.
  • the preferred polycarboxylic acids are hydroxycarboxylic containing up to three carboxy groups per molecules, more particularly citric acid monohydrate.
  • the partially/fully hydrated acids have an average particle size from 0.8 to 3 d m (RR)/mm, more preferably from 1.4 to 2.5 d m (RR)/mm.
  • the 95 % of the particles have a particle size greater than lmm and less than 3mm.
  • the organic acid is present at a level of at least 50 wt% of the total formulation, more preferably at a level greater than 70 wt%, most preferably at a level from 85 wt% to 98 wt%.
  • a surfactant system comprising a surfactant selected from nonionic, anionic, cationic, ampholytic and zwitterionic surfactants and mixtures thereof is also present in the composition.
  • the surfactant is a low to non foaming nonionic surfactant, which includes any alkoxylated nonionic surface-active agent wherein the alkoxy moiety is selected from the group consisting of ethylene oxide, propylene oxide and mixtures thereof, is preferably used to improve the detergency without excessive foaming especially preferred are ethoxylated and/or propoxylated straight chain alcohols.
  • nonionic surfactant should be avoided. Normally, an amount of 10% by weight or lower, preferably 7% by weight or lower, most preferably 5% by weight or lower and preferably 0.1% by weight or higher, more preferably 0.5% by weight or higher is quite sufficient.
  • nonionic surfactants for use in the invention are the low- to non-foaming ethoxylated straight-chain alcohols of Plurafac LF series ex BASF, Synperonic series ex ICI; of the Lutensol® LF series, supplied by the BASF Company and of the Triton® DF series, supplied by the Rohm & Haas Company.
  • anionic surfactant may be used but may require the additional presence of an antifoam to surpress foaming. If an anionic surfactant is used it is advantageously present at levels of 2 wt% or below.
  • suitable flow aids include Aluminium silicate (Alusil), Calcium silicate (Calflow) and silicas.
  • Bleach material may optionally be incorporated in composition for use in processes according to the present invention, but preferably are not present.
  • the bleach material may be a chlorine- or bromine-releasing agent or a peroxygen compound. Peroxygen based bleach materials are however preferred.
  • compositions that may be present include crystal-growth inhibitors, threshold agents; perfumes and dyestuffs and the like.
  • the dish washing machine cleaner has gives a pH of 3 or less in a 1% aqueous solution at 20°C. More preferably the composition has a pH from 1 to 2 in a 1% aqueous solution at 20°C.
  • the dish washing composition is preferably granular.
  • Granular in the context of the present invention includes both powdered material and tablets.
  • the cleaning composition may be added to the machine via the dispenser drawer or sprinkled directly into the base of the dish washer. It is particularly advantageous if the composition is added directly to the base of the machine, as this leads to an effective dosing level.
  • Dishwash compositions according to the present invention may be dosed in the wash liquor at levels of from 30 g/l to 2.5 g/l.
  • compositions were tested in a robotised Miele G5953C (total water hardness 17°FH, including temporary hardness of 9°FH).
  • compositions were dosed at a level of 120 g/wash by sprinkling the powder in the base of the machine near the sieve; the main wash time was 20 minutes; the drying time with open door was 10-20 minutes; the washing temperature was up to 65°C.
  • Example 1 A Consecutive No. of runs before pump breakdown No breakdown 10

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)

Abstract

An automatic dish washing machine cleaner comprises at least 50% wt of the total composition of a partially or fully hydrated organic acid and at least 0.5% wt of the total composition of a surfactant, ideally a non-ionic surfactant. The pH of a 1% aqueous solution of the cleaner at 20°C is 3 or less. Also described are a process for cleaning a dish washing machine comprising adding the above machine dish washing cleaner to a machine, and the use of citric acid monohydrate in a dish washing machine cleaner to prevent mass solidification.

Description

    Technical Field
  • The present invention is in the field of machine dishwashing. More specifically, the invention encompasses a cleaner for automatic dishwashing machines.
    • Background of the Invention
  • The present invention relates to a composition used to clean dish washing machines. Such cleaning compositions are frequently used by the consumer to clean the dish washer itself and so remove deposits after the machine has been used to clean crockery.
  • Conventional cleaning machine cleaning products are put in the machine's dispenser and/or sprinkled on the base of machine. However, it has been found that occasionally conventional dish washer cleaning formulations tend to co-aggulate in the sieve in the bottom of the machine thus forming a solid mass that can block the machine and pump.
  • The present invention relates to a composition for cleaning dish washers in which the problem of co-agulation is mitigated.
    • Description of the Invention
  • According the present invention provides an automatic dish washing machine cleaner comprising at least 50% wt of the total composition of a partially or fully hydrated organic acid and at least 0.5 % wt of the total composition of a surfactant
  • The present invention also provides the use of citric acid monohydrate in a dish washing machine cleaner to prevent mass solidification.
    • Detailed Description of the Invention
  • The compositions of the present invention comprise a partially or fully hydrated organic acid as an essential element. Suitable partially or fully hydrated organic acids organic acids include, for example, carboxylic acids, such as citric and succinic acids, polycarboxylic acids, such as polyacrylic acid, and also acetic acid, boric acid, malonic acid, adipic acid, fumaric acid, lactic acid, glycolic acid, sulphamic acid, tartaric acid, tartronic acid, maloic acid, their derivatives and any mixtures of the foregoing.
  • Suitable water-soluble monomeric or oligomeric carboxylates can be selected from a wide range of compounds but such compounds preferably have a first carboxyl logarithmic acidity/constant (pK1) of less than 9, preferably of between 2 and 8.5, more preferably of between 2.5 and 7.5.
  • Polycarboxylic acids containing four carboxy groups include oxydisuccinic acids, 1,1,2,2-ethane tetracarboxylic acids, 1,1,3,3-propane tetracarboxylic acids and 1,1,2,3-propane tetracarboxylic acids. Polycarboxylic acids containing sulfo substituents include the sulfosuccinic derivatives, and the sulfonated pyrolysed citratic acids.
  • Of the above, the preferred polycarboxylic acids are hydroxycarboxylic containing up to three carboxy groups per molecules, more particularly citric acid monohydrate.
  • It is preferable if the partially/fully hydrated acids have an average particle size from 0.8 to 3 dm (RR)/mm, more preferably from 1.4 to 2.5 dm (RR)/mm.
  • It is also preferable if the 95 % of the particles have a particle size greater than lmm and less than 3mm.
  • The organic acid is present at a level of at least 50 wt% of the total formulation, more preferably at a level greater than 70 wt%, most preferably at a level from 85 wt% to 98 wt%.
  • A surfactant system comprising a surfactant selected from nonionic, anionic, cationic, ampholytic and zwitterionic surfactants and mixtures thereof is also present in the composition.
  • Typically the surfactant is a low to non foaming nonionic surfactant, which includes any alkoxylated nonionic surface-active agent wherein the alkoxy moiety is selected from the group consisting of ethylene oxide, propylene oxide and mixtures thereof, is preferably used to improve the detergency without excessive foaming especially preferred are ethoxylated and/or propoxylated straight chain alcohols.
  • However, an excessive proportion of nonionic surfactant should be avoided. Normally, an amount of 10% by weight or lower, preferably 7% by weight or lower, most preferably 5% by weight or lower and preferably 0.1% by weight or higher, more preferably 0.5% by weight or higher is quite sufficient.
  • Examples of suitable nonionic surfactants for use in the invention are the low- to non-foaming ethoxylated straight-chain alcohols of Plurafac LF series ex BASF, Synperonic series ex ICI; of the Lutensol® LF series, supplied by the BASF Company and of the Triton® DF series, supplied by the Rohm & Haas Company.
  • Other surfactants such as anionic surfactant may be used but may require the additional presence of an antifoam to surpress foaming. If an anionic surfactant is used it is advantageously present at levels of 2 wt% or below.
  • It is advantageous if a flow aid is present in the composition suitable flow aids include Aluminium silicate (Alusil), Calcium silicate (Calflow) and silicas.
  • Bleach material may optionally be incorporated in composition for use in processes according to the present invention, but preferably are not present.
  • The bleach material may be a chlorine- or bromine-releasing agent or a peroxygen compound. Peroxygen based bleach materials are however preferred.
  • Further optional ingredients that may be present include crystal-growth inhibitors, threshold agents; perfumes and dyestuffs and the like.
    • pH of wash liquor
  • Preferably the dish washing machine cleaner has gives a pH of 3 or less in a 1% aqueous solution at 20°C. More preferably the composition has a pH from 1 to 2 in a 1% aqueous solution at 20°C.
    • Product Form
  • The dish washing composition is preferably granular. Granular in the context of the present invention includes both powdered material and tablets.
    • Method of Using the Composition.
  • The cleaning composition may be added to the machine via the dispenser drawer or sprinkled directly into the base of the dish washer. It is particularly advantageous if the composition is added directly to the base of the machine, as this leads to an effective dosing level.
  • Dishwash compositions according to the present invention may be dosed in the wash liquor at levels of from 30 g/l to 2.5 g/l.
  • The invention will now be illustrated by the following non limiting Examples. Examples of the invention are illustrated by a number, comparative Examples are illustrated by a letter.
  • All percentages are on a weight basis.
    • EXAMPLE I
  • WT/%
    1 A
    Citric acid monohydrate 92.1 -
    Citric acid Anhydrous 92.1
    Starch based flow aid 5.5 5.5
    Perfume 0.2 0.2
    Nonionic surfactant 2.0 2.0
    minors to 100 to 100
    Particle Size 1.8 mm 1.8 mm
  • The compositions were tested in a robotised Miele G5953C (total water hardness 17°FH, including temporary hardness of 9°FH).
  • The compositions were dosed at a level of 120 g/wash by sprinkling the powder in the base of the machine near the sieve; the main wash time was 20 minutes; the drying time with open door was 10-20 minutes; the washing temperature was up to 65°C.
    Example 1 A
    Consecutive No. of runs before pump breakdown No breakdown 10

Claims (8)

  1. An automatic dish washing machine cleaner comprising:
    a) at least 50% wt of the total composition of a partially or fully hydrated organic acid and;
    b) at least 0.5 % wt of the total composition of a surfactant
  2. An automatic dish washing machine cleaner according to claim 1 in which the partially or fully hydrated organic acid is citric acid monohydrate.
  3. An automatic dish washing machine cleaner according to claim 1 or claim 2 in which the surfactant is a nonionic surfactant.
  4. An automatic dish washing machine cleaner according to claim 3 in which the nonionic surfactant is an ethoxylated and/or propoxylated straight-chain alcohol.
  5. An automatic dish washing machine cleaner according to any preceding claim in which the pH of a 1% aqueous solution at 20°C is 3 or less.
  6. An automatic dish washing machine cleaner according to any preceding claim which further comprises a flow aid.
  7. A process for cleaning a dish washing machine comprising adding a machine dish washing cleaner as claimed in any preceding claim to a machine dish washer.
  8. Use of citric acid monohydrate in a dish washing machine cleaner to prevent mass solidification.
EP00303177A 1999-05-28 2000-04-14 Automatic dish-washing machine cleaning process and compositions relating thereto Expired - Lifetime EP1061123B2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP00303177A EP1061123B2 (en) 1999-05-28 2000-04-14 Automatic dish-washing machine cleaning process and compositions relating thereto
TW094305092F TWD114205S1 (en) 2000-04-14 2005-08-24 Toy-car

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP99304182 1999-05-28
EP99304182 1999-05-28
EP00303177A EP1061123B2 (en) 1999-05-28 2000-04-14 Automatic dish-washing machine cleaning process and compositions relating thereto

Publications (3)

Publication Number Publication Date
EP1061123A1 true EP1061123A1 (en) 2000-12-20
EP1061123B1 EP1061123B1 (en) 2004-06-30
EP1061123B2 EP1061123B2 (en) 2007-02-14

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EP00303177A Expired - Lifetime EP1061123B2 (en) 1999-05-28 2000-04-14 Automatic dish-washing machine cleaning process and compositions relating thereto

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EP (1) EP1061123B2 (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001062886A1 (en) * 2000-02-23 2001-08-30 The Procter & Gamble Company Detergent tablet
FR2831181A1 (en) * 2001-10-23 2003-04-25 Rhodia Polyamide Intermediates Scale inhibitor composition in tablet form for prewashing dishes in automatic dishwashers
WO2006063231A1 (en) * 2004-12-08 2006-06-15 The Procter & Gamble Company Method of cleaning a washing machine or a dishwasher
WO2007068920A1 (en) * 2005-12-13 2007-06-21 Reckitt Benckiser N.V. Method and composition
DE102006009138A1 (en) * 2006-02-24 2007-08-30 Henkel Kgaa Detergent for removing greasy or oily soil and cleaning and conditioning hard surface, e.g. washing machine or automatic dishwasher contains nonionic surfactant mixture of (poly)alkylene oxide mono- or di-ether and amine oxide
EP2039750A1 (en) * 2007-09-21 2009-03-25 Brauns-Heitmann GmbH & Co. KG Mixture for removing limescale, cleaning and/or disinfecting
DE102012014268A1 (en) * 2012-07-19 2014-01-23 Brauns-Heitmann Gmbh & Co. Kg Device useful for cleaning or decalcifying household appliances, preferably e.g. washing machines, comprises container comprising water, and first composition which comprises active substance whose partial amount is solidified by water
EP2333042B1 (en) 2009-12-10 2015-07-01 The Procter and Gamble Company Automatic dishwashing product and use thereof
WO2025131739A1 (en) * 2023-12-20 2025-06-26 Henkel Ag & Co. Kgaa Care product for automatic dishwashers

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1396678A (en) * 1972-12-07 1975-06-04 Hoechst Ag Method for the automatic washing of tableware
US4392977A (en) * 1980-01-26 1983-07-12 Henkel Kommanditgesellschaft Auf Aktien Liquid cleaning and maintenance composition especially for dishwashers
EP0256148A1 (en) * 1986-08-12 1988-02-24 Joh. A. Benckiser GmbH Liquid, granulated or powdery detergent, in particular for dish-washing machines
EP0612843A1 (en) * 1993-02-22 1994-08-31 Unilever N.V. Granular acidic cleaners

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1396678A (en) * 1972-12-07 1975-06-04 Hoechst Ag Method for the automatic washing of tableware
US4392977A (en) * 1980-01-26 1983-07-12 Henkel Kommanditgesellschaft Auf Aktien Liquid cleaning and maintenance composition especially for dishwashers
EP0256148A1 (en) * 1986-08-12 1988-02-24 Joh. A. Benckiser GmbH Liquid, granulated or powdery detergent, in particular for dish-washing machines
EP0612843A1 (en) * 1993-02-22 1994-08-31 Unilever N.V. Granular acidic cleaners

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001062886A1 (en) * 2000-02-23 2001-08-30 The Procter & Gamble Company Detergent tablet
US7153817B2 (en) 2000-02-23 2006-12-26 The Procter & Gamble Company Detergent tablet
FR2831181A1 (en) * 2001-10-23 2003-04-25 Rhodia Polyamide Intermediates Scale inhibitor composition in tablet form for prewashing dishes in automatic dishwashers
WO2003035819A1 (en) * 2001-10-23 2003-05-01 Rhodia Polyamide Intermediates Acid scale preventive tablet and the use thereof in automatic dishwashing
WO2006063231A1 (en) * 2004-12-08 2006-06-15 The Procter & Gamble Company Method of cleaning a washing machine or a dishwasher
WO2007068920A1 (en) * 2005-12-13 2007-06-21 Reckitt Benckiser N.V. Method and composition
DE102006009138A1 (en) * 2006-02-24 2007-08-30 Henkel Kgaa Detergent for removing greasy or oily soil and cleaning and conditioning hard surface, e.g. washing machine or automatic dishwasher contains nonionic surfactant mixture of (poly)alkylene oxide mono- or di-ether and amine oxide
EP2039750A1 (en) * 2007-09-21 2009-03-25 Brauns-Heitmann GmbH & Co. KG Mixture for removing limescale, cleaning and/or disinfecting
EP2098587A1 (en) * 2007-09-21 2009-09-09 Brauns-Heitmann GmbH & Co. KG Mixture for removing limescale, cleaning and/or disinfecting
EP2333042B1 (en) 2009-12-10 2015-07-01 The Procter and Gamble Company Automatic dishwashing product and use thereof
DE102012014268A1 (en) * 2012-07-19 2014-01-23 Brauns-Heitmann Gmbh & Co. Kg Device useful for cleaning or decalcifying household appliances, preferably e.g. washing machines, comprises container comprising water, and first composition which comprises active substance whose partial amount is solidified by water
DE102012014268B4 (en) * 2012-07-19 2014-02-20 Brauns-Heitmann Gmbh & Co. Kg Device for cleaning and / or descaling for use in dishwashers or washing machines
WO2025131739A1 (en) * 2023-12-20 2025-06-26 Henkel Ag & Co. Kgaa Care product for automatic dishwashers

Also Published As

Publication number Publication date
EP1061123B1 (en) 2004-06-30
EP1061123B2 (en) 2007-02-14

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