WO2008029163A2 - Traitement de sorgho à sucre destiné à une production de bioéthanol - Google Patents

Traitement de sorgho à sucre destiné à une production de bioéthanol Download PDF

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Publication number
WO2008029163A2
WO2008029163A2 PCT/GB2007/003395 GB2007003395W WO2008029163A2 WO 2008029163 A2 WO2008029163 A2 WO 2008029163A2 GB 2007003395 W GB2007003395 W GB 2007003395W WO 2008029163 A2 WO2008029163 A2 WO 2008029163A2
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WIPO (PCT)
Prior art keywords
biomass material
sweet sorghum
sugar
cane
cut
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PCT/GB2007/003395
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English (en)
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WO2008029163A3 (fr
Inventor
Arsen Badalov
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Nasamax Limited
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Publication date
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Publication of WO2008029163A2 publication Critical patent/WO2008029163A2/fr
Publication of WO2008029163A3 publication Critical patent/WO2008029163A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
    • C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B10/00—Production of sugar juices
    • C13B10/02—Expressing juice from sugar cane or similar material, e.g. sorghum saccharatum
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/02—Glucose; Glucose-containing syrups obtained by saccharification of cellulosic materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the present invention describes a productive and efficient method of processing sweet sorghum (sorghum bicolour) whereby the sweet sorghum cane is cut into very fine fibres so that the sugar juice in the sweet sorghum can easily be extracted from the fibrous material for subsequent fermentation into bioethanol.
  • the lignocellulose material in the residual baggasse from the juice extraction process is also in suitable fibrous state for prehydrolysis with mild acid or alkali to break down the lignocellulose into its lignin, cellulose and hemicellulose constituents for subsequent conversion into fermentable sugars.
  • Natural ethanol produced from cultivated sugar or starch bearing plants is a clean burning renewable fuel that is being increasingly used as a substitute fuel for road transport applications.
  • the market for bioethanol road fuel is growing so rapidly that demand is starting to exceed supply, and there is an urgent need for alternative plant species that can produce substantial volumes of feedstock for conversion into cost effective bioethanol on a large industrial scale.
  • sweet sorghum is a unique sugar bearing plant in that it has a rapid and prolific growth rate and it can also be grown in different climates. Under the right climatic conditions, sweet sorghum has such rapid growth that it is possible to grow more than one crop of sweet sorghum a year; for example three crops a year are feasible under tropical conditions and between two and three crops a year are possible under subtropical conditions. Sweet sorghum is therefore a very productive energy plant species that can provide large amounts of sugar and lignocellulose material for conversion into bioethanol.
  • the sugar would be fermented by yeast into ethanol, whilst the lignocellulose would be digested with acid or alkali to separate out the lignin, convert the hemicellulose into sugars, and expose the cellulose for conversion into fermentable sugars by enzymatic hydrolysis.
  • Sweet sorghum is not widely used for food production and sweet sorghum is therefore an ideal plant for cultivation as an energy crop.
  • a system that combines the cultivation of sweet sorghum with the production of bioethanol has been developed for tropical and subtropical climates. The system allows sweet sorghum to be grown all year round so that there is continual supply of fresh sugar juice and lignocellulose material readily available for the ethanol production plant. Under the combined cultivation and bioethanol production system, there would be enough freshly harvested sweet sorghum available each day to meet the sugar and lignocellulose feedstock requirements of an integrated bioethanol production plant.
  • the ethanol production plant would be located immediately adjacent to the land dedicated to the cultivation of the sweet sorghum so that the raw material feedstock can easily be shipped to the ethanol plant, which helps to reduce transport costs and environmental pollution.
  • the sugar in the juice of sweet sorghum tends to deteriorate quickly, and a further advantage of the combined system is that freshly harvested sweet sorghum will be delivered each day to the ethanol plant so that the sugar content of the cane will always be near its peak level.
  • Effluent water rich in plant nutrients from the ethanol plant would also be used as fertiliser to promote the growth of the sweet sorghum in the nearby plantations.
  • a typical large integrated bioethanol plant would produce about 160,000 litres of ethanol a day, which is equivalent to 56 million litres a year.
  • a plant of this size would need 1280 tonnes of fresh sweet sorghum delivered every day to meet the sugar and lignocellulose feedstock requirements of the ethanol conversion processes. It is therefore imperative that the sweet sorghum cane is processed quickly and efficiently so that there is a continual supply of fresh sugar juice and lignocellulose material available for the ethanol conversion processes, and that as much sugar and lignocellulose as possible is extracted from the cane to maximise the yield of bioethanol.
  • Conventional methods of extracting sugar juice from sugarcane usually entail stripping or
  • sweet sorghum Like sugarcane, the cane from sweet sorghum is a tough material and it has been established by practical trials that conventional methods of juice extraction tend to work poorly with sweet sorghum cane. For example, when sweet sorghum cane was cut into small pieces about 13 mm long and the pieces of cane were then crushed in a roller press, only 70% of the sugar that was available in the original unprocessed cane was retrieved from the cane.
  • baggasse material remaining from conventional cane crushing operations is usually in relatively large size pieces that would be unsuitable for prehydrolysis with acid or alkali.
  • the baggasse would therefore have to be ground, milled or pulverised into very small pieces before the lignocellulose material in the baggasse was in a suitable state for effective digestion with acid or alkali.
  • industrial food processing equipment may be used to cut and chop sweet sorghum into a fibrous state.
  • equipment conventionally used to emulsify meat into a slurry for the processed food industry may be used to cut sweet sorghum into very fine fibres.
  • This type of food processing equipment is similar to a domestic food blending machine and includes rapidly rotating blades which pass over a perforated plate and gradually cut and slice raw material down to a fine size. The perforations allow cut material to pass through the plate and out of the processing equipment once the material has been cut to a predetermined size.
  • Karl Schnell GmbH of Germany manufacture a typical industrial food processing machine, otherwise known as an emulsifier, which is normally used to emulsify fresh meat for the processed food industry, and this equipment was found to be suitable for cutting sweet sorghum into fine fibres.
  • the Karl Schnell emulsifier, reference KS-F 320 had never been used to process tough fibrous vegetable matter; however, practical trials with sweet sorghum cane showed that the equipment was able to quickly and effectively cut sweet sorghum into fine fibrous state.
  • the sweet sorghum cane would initially be cut into small pieces approximately 13mm long by the harvesting equipment used to harvest the sweet sorghum in the field.
  • the cut cane would be delivered to the ethanol plant immediately after harvest so that the cane would always be in a fresh condition on arrival at the plant.
  • other biomass material from harvested sweet sorghum plants such as leaves and seeds, may be present or mixed with the pre-cut cane before processing at the ethanol production plant.
  • Ripe sweet sorghum typically consists of about 75% cane, 10% leaves, 5% seeds and 10% roots by weight. Processing other biomass as well as the cane ensures that there is as much convertible lignocellulose material available as possible to produce bioethanol.
  • the cut cane would be processed into fine fibres at the ethanol plant by passing the cane through coarse and fine emulsifiers combined together in series.
  • the 13 mm pieces of sweet sorghum cane would be transferred by screw conveyor into a coarse emulsifier, such as a KS-F 320 coarse emulsifier, where the rotating blades would reduce the 13 mm pieces of cane into small slivers/shavings approximately 5mm long.
  • the small slivers of cane would then be transferred from the coarse emulsifier into a fine emulsifier, such as a KS-F 320 fine emulsifier, where the rotating blades in the emulsifier would reduce the cubes into very fine fibres of between lmm and 5mm in length.
  • a fine emulsifier such as a KS-F 320 fine emulsifier
  • the rotating blades in the emulsifier would reduce the cubes into very fine fibres of between lmm and 5mm in length.
  • a major benefit of this method of processing is that the material from the fine emulsifier is in such a fine, fluffy state that a relatively light pressure is sufficient to extract the sugar juice from the fibrous material.
  • the residual baggasse material remaining after the extraction of the juice consists of fine fibres of lignocellulosic material which are ideal for prehydrolysis with acid or alkali.
  • sweet sorghum cane can contain up to 80% moisture and it was confirmed that fresh cane worked particularly well in the emulsifying equipment. Dry cane contains much less moisture and dry cane is therefore appreciably tougher than fresh cane.
  • sweet sorghum Efficient processing of sweet sorghum is therefore dependent on the cane being in a fresh condition and having a high moisture content.
  • the sweet sorghum cane from the combined cultivation and ethanol production system will be ideal because freshly harvested sweet sorghum will be delivered every day to the ethanol production plant.
  • the cane introduced into the emulsifiers will not only be fresh but also have high moisture and sugar contents.
  • a further advantage of the proposed cane processing technique is that sugar juice is not released during the emulsifying process because the fibrous matter is able to hold a large amount of moisture and the juice is therefore retained inside the cut fibres.
  • the fibrous material from the fine emulsifier is so saturated with sugar juice that very little pressure is required to squeeze the juice from the fibres; for example it is even possible to squeeze the juice from a ball of fibres by hand pressure only, which would be impossible with either cut pieces of cane or coarsely milled cane.
  • the juice can therefore be extracted from the fibrous material by relatively light pressure in either a screw or roller press, although laboratory trials indicated that a screw press is probably the preferable method of juice extraction.
  • a screw press is probably the preferable method of juice extraction.
  • fibrous sweet sorghum produced by passing pre-cut cane through combined coarse and fine KS-F 320 emulsifiers was crushed very easily and effectively by a small laboratory screw press, reference CP4, manufactured by the Vincent Corporation of the USA.
  • Vincent screw presses are normally used for relatively lightweight pressing operations such as the extraction of juice from easily crushed fruit and vegetables, such as citrus fruits, soft fruits and tomatoes.
  • the amount of juice extracted from the processed fibrous sweet sorghum cane by the CP4 screw press was exceptionally high, and a laboratory evaluation indicated that the juice from the press contained over 80% of the sugar that was originally present in the unprocessed cane. From a first aspect therefore fresh sweet sorghum is progressively reduced in size by passing pieces of pre-cut cane 13 mm in size through combined coarse and fine industrial emulsifiers until the cane is in such a fine fibrous state that a relatively light pressure by a screw or roller press is sufficient to extract a substantial amount of the sugar juice originally present in the cane.
  • the residual compressed cake from the Vincent screw press contained about 40% moisture.
  • a further novel feature of the proposed method of cane processing is that the compressed cake from the screw press is easily reconstituted back into a moist fibrous state, and the moist fibre can then be pressed a second time to extract more sugar.
  • the pressed cake is easily reconstituted by agitating the cake until it returns to a fluffy fibrous state and moisture is reintroduced back into the fibres by finely spraying the cake with water during the agitation process.
  • Approximately 1 part water to 1 part compressed cake by weight is sufficient to return the cake to an adequately moistened fibrous state.
  • the water reintroduced into the fibrous material picks up sugar remaining in the fibres after the first press operation, and when the damp reconstituted fibre is pressed a second time, the liquor released can contain at least a further 15% of the sugar that was originally present in the fresh cane.
  • Processing fresh sweet sorghum cane into very fine fibres and then subjecting the fibrous matter to a double press operation is therefore a very effective way of extracting a substantial amount of the sugar that was originally present in the cane.
  • Potentially at least 95% of the sugar present in unprocessed sweet sorghum cane can be retrieved by the proposed technique.
  • the sugar juice from the first and second press operations would be combined together, and after filtration and concentration the concentrated sugar juice would be in a suitable state for fermentation into ethanol. From a second aspect therefore the compressed residual cake from the first screw press operation is reconstituted back into a damp fibrous state by agitating the compressed cake and simultaneously finely spraying the cake with an appropriate amount of water.
  • the fibrous material can then be pressed a second time to extract more sugar juice and the proposed method of processing could potentially extract at least 95% of the sugar originally available in the fresh sweet sorghum.
  • the proposed method of cane processing and juice extraction is energy efficient.
  • a relatively light pressure in a screw press is sufficient to extract the sugar juice from the fibrous material. It is estimated that the proposed method of processing and juice extraction will use less than 50% of the energy associated with conventional stripping, milling and high pressure juice extraction techniques.
  • the lignocellulose in the residual compressed fibre cake from the second press operation is also in an ideal state for prehydrolysis with acid or alkali, which is an essential step in an ethanol enzymatic hydrolysis production process.
  • the cake from the second press is basically a compressed mass of fine lignocellulosic fibres, and when the cake is agitated in the prehydrolysis reactor the fibres easily separate. The fibres are then in an ideal state for effective digestion by acid or alkali to break the lignocellulosic material down into its lignin, hemicellulose and cellulose constituents.
  • Established prehydrolysis techniques with conventionally milled residual biomass such as, for example, shredded sugarcane baggasse, corn stover or wheat straw, can involve relatively strong solutions of acid or alkali, high temperatures, high pressures and long digestion times.
  • the lignocellulose material from the emulsified sweet sorghum is in the form of very fine fibres and the material appears to be particularly susceptible to digestion with acid or alkali. Consequently it should be possible to use relatively mild reaction conditions in the prehydrolysis reactor.
  • emulsified fibrous sweet sorghum baggasse has been subjected to relatively mild prehydrolysis in the laboratory using potassium hydroxide as the digestion reactant. Prehydrolysis reactions were carried out at normal atmospheric pressure using potassium hydroxide as the digestion reactant.
  • reaction temperatures 40 0 C, 50 0 C and 60 0 C; and reaction times of 30 minutes and 60 minutes.
  • the fibrous lignocellulose material in the residual compressed cake from the second screw press is in a suitable state for prehydrolysis under mildly acid or alkali conditions to separate the lignin, hydrolyse the hemicellulose into sugars and expose the cellulose for subsequent enzymatic hydrolysis into sugars.
  • the hemicellulose and cellulose sugars would then be jointly fermented with the concentrated sugar juice extracted from the sweet sorghum to produce bioethanol.
  • the method of cane processing described in the invention produces high yields of sugar juice and lignocellulose, which in turn helps to produce high yields of ethanol.
  • This is illustrated in Table 1, which gives the predicted ethanol yield from fresh sweet sorghum processed by the method described in the invention. It is assumed in Table 1 that the sweet sorghum would have been grown by the combined cultivation and integrated ethanol production system described earlier.
  • the integrated process could have a potential bioethanol yield equivalent to 50,000 litres/ha/year, whereas the yield of ethanol from the fermentation of just the sugar in sugarcane or sugarbeet is normally only about 6000 litres/ha/year.
  • the sweet sorghum cane will have been cut into 13 mm pieces when harvested in the field, and the pieces of cane will be transferred by a conveyor 1 into the feed hopper 2 of a transfer elevator 3.
  • the elevator transfers the pieces of cane into the in-feed hopper 5 of a coarse industrial food emulsifier 4.
  • Other biomass, such as leaves and seeds, from harvested plants may be added to the pre-cut cane in the transfer elevator 3 to ensure that as much biomass as possible is used to produce bioethanol.
  • the coarse emulsifier 4 is driven by an adjustable motor 6.
  • the sweet sorghum material is reduced into small slivers about 5 mm long by the coarse emulsifier 4.
  • the slivers of material are then fed into the in-feed hopper 8 of a fine emulsifier 7, which is driven by an adjustable motor 9, and the slivers are reduced to fine fibres between 1 mm and 5 mm in length by the fine emulsifier 7.
  • the fibrous material is transferred to the in- feed hopper 11 of a screw press 10.
  • the press is driven by a motor 12 and the pressure is controlled by gearing 13.
  • the press 10 squeezes the sugar juice from the fibrous material and the juice exits the screw press at outlet 14. At least 80% of the sugar originally present in the sweet sorghum cane should be extracted by the screw press 10.
  • the compressed cake inside the press 10 collects at outlet 15 and is transferred into a rotary agitator 16 where the cake is reconstituted into a fibrous state and the fibres are moistened with a fine spray of water.
  • the damp fibrous cane is then fed into the in- feed hopper 17 of a second screw press 18 driven by motor 19 and controlled by gearing 20.
  • the second press 18 squeezes the liquor from the fibrous material and the liquor exits the screw press at outlet 21.
  • a further 15% of the sugar originally present in the sweet sorghum cane should be extracted by press 18, so that over 95% of the sugar originally available in the sweet sorghum should have been extracted by the double press operation.
  • the sugar juice from the first press 10 and the liquor from the second press 18 are combined together for filtration, concentration and then subsequent fermentation by active yeast into bioethanol.
  • the compressed cake inside press 18 collects at outlet 22 and the cake is transferred to the in- feed hopper 23 of a transfer elevator 24.
  • the elevator 24 transfers the cake into a prehydrolysis reactor 25 where agitation reconstitutes the cake into fine lignocellulosic fibres. Mildly acid or alkali conditions 26 in the reactor are then sufficient to break down the fibrous lignocellulose into lignin, hemicellulose and cellulose constituents.
  • the invention therefore provides an effective method of processing sweet sorghum biomass material that allows a substantial amount of the sugar available in the sweet sorghum to be efficiently extracted from the sweet sorghum cane.
  • the lignocellulose material in the residual baggasse from the juice extraction process is also in a fine fibrous state that is ideal for prehydrolysis with mild acid or alkali to separate the lignin, hydrolyse the hemicellulose into sugars and expose the cellulose for subsequent enzymatic hydrolysis into sugars.
  • the invention is primarily aimed at processing sweet sorghum cane, the principles of the invention could probably be applied to other energy plant species, such as sugarcane, where it is desirable to remove as much sugar juice as possible from the biomass feedstock to maximise the yield of ethanol that can be obtained from sugar fermentation.
  • the residual baggasse from the sugarcane would also be in a suitable fibrous state for effective prehydrolysis with a mild acid or alkali.

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

L'invention concerne un procédé de traitement de canne de sorgho à sucre destiné à une extraction de sucre. Ce procédé consiste à passer la canne dans un premier système de coupe (4) pour couper la matière de manière grossière, puis à la passer dans un second système de coupe (7) pour la couper en fibres fines. La matière fibreuse est ensuite passée dans une presse (10) pour extraire un jus sucré destiné à la fermentation dans une installation de production de bioéthanol (25).
PCT/GB2007/003395 2006-09-08 2007-09-10 Traitement de sorgho à sucre destiné à une production de bioéthanol WO2008029163A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0617762.0 2006-09-08
GB0617762A GB2447062A (en) 2006-09-08 2006-09-08 Processing of Sweet Sorghum for Bioethanol Production

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WO2008029163A2 true WO2008029163A2 (fr) 2008-03-13
WO2008029163A3 WO2008029163A3 (fr) 2008-08-28

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PCT/GB2007/003395 WO2008029163A2 (fr) 2006-09-08 2007-09-10 Traitement de sorgho à sucre destiné à une production de bioéthanol

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009124370A1 (fr) * 2008-04-11 2009-10-15 Dow Brasil Sudeste Industrial Ltda . Processus d'extraction de sucre à partir de matière végétale contenant du sucre
FR2932815A1 (fr) * 2008-06-23 2009-12-25 Cie Ind De La Matiere Vegetale Procede de pretraitement de la matiere premiere vegetale pour la production, a partir de ressources sacchariferes et lignocellulosiques, de bioethanol et/ou de sucre, et installation.
WO2010086158A3 (fr) * 2009-01-28 2010-12-29 Michael Niederbacher Installation de chargement pour fermenteur pour une biomasse fermentable d'une installation de production de biogaz, et procédé de fonctionnement de cette installation
US7943363B2 (en) 2008-07-28 2011-05-17 University Of Massachusetts Methods and compositions for improving the production of products in microorganisms
EP2792739A1 (fr) * 2013-04-15 2014-10-22 Michael Niederbacher Installation de biogaz dotée d'un dispositif d'alimentation en ferments

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CUNDIFF J S ET AL: "CHOPPING PARAMETERS FOR SEPARATION OF SWEET SORGHUM PITH AND RIND-LEAF" BIORESOURCE TECHNOLOGY, vol. 39, no. 3, 1992, pages 263-270, XP002483912 ISSN: 0960-8524 *
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009124370A1 (fr) * 2008-04-11 2009-10-15 Dow Brasil Sudeste Industrial Ltda . Processus d'extraction de sucre à partir de matière végétale contenant du sucre
US8828142B2 (en) 2008-04-11 2014-09-09 Dow Brasil Sudeste Industrial Ltda. Processes for extraction of sugar from sugar-bearing plant material
FR2932815A1 (fr) * 2008-06-23 2009-12-25 Cie Ind De La Matiere Vegetale Procede de pretraitement de la matiere premiere vegetale pour la production, a partir de ressources sacchariferes et lignocellulosiques, de bioethanol et/ou de sucre, et installation.
WO2010006840A3 (fr) * 2008-06-23 2010-05-06 Compagnie Industrielle De La Matiere Vegetale - Cimv Procédé pour prétraiter un matériau de départ de plante pour la production, à partir de ressources saccharifères et lignocellulosiques, de bioéthanol et/ou de sucre, et plante
EA019188B1 (ru) * 2008-06-23 2014-01-30 Компани Эндюстриель Де Ля Матьер Вежеталь - Кимв Способ предварительной обработки исходного растительного материала для получения биоэтанола и сахара из сахаросодержащих и лигниноцеллюлозных источников
US7943363B2 (en) 2008-07-28 2011-05-17 University Of Massachusetts Methods and compositions for improving the production of products in microorganisms
WO2010086158A3 (fr) * 2009-01-28 2010-12-29 Michael Niederbacher Installation de chargement pour fermenteur pour une biomasse fermentable d'une installation de production de biogaz, et procédé de fonctionnement de cette installation
EP2792739A1 (fr) * 2013-04-15 2014-10-22 Michael Niederbacher Installation de biogaz dotée d'un dispositif d'alimentation en ferments

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GB0617762D0 (en) 2006-10-18
GB2447062A (en) 2008-09-03

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