PHYSICAL CHEMICAL METHOD TO REMOVE THE CORK TASTE AND IN GENERAL ANOMALOUS SMELLS OF CORK MATERIALS.
TECHNICAL FIELD
Innovative technology of washing cork materials as cork of different dimension of natural type, washers, agglomerated corks, mono- agglomerated corks and biwashered. granulated cork produced by cork firms, with the use of a suspension of active carbons
PREEXISTENT TECHNIQUE
At present the oenological area suffers, in a large way, of the negative effects caused by the use of cork materials considered responsible, in many cases . for undesirable organoleptic characters transferred by them to the wine and to the drinks in general. The problem has repercussions on the productive and distributing firms of cork materials causing financial damages that are expressed in the restitution of the goods and sometimes in the loss of credibility with a possible remission of contracts. In more emphasised way the problem linked to the cork taste whose harmful effects are charged to the possible presence in the cork, appointed to the oenological area of particular halogen compounds, is noticed.
Several are the searches and issues that face the problem linked to the presence in the quercus kind, of some parasitics of fungin nature that, in their vital cycle are able to attack the different parts of the plant. In the cork- oak, the attack besides being located in the wood involves, at the same way, the layer of the cork too. Such considerations lead to argue that the undesirable effect is to charge to the activity of the micro-organisms in hand. More recent studies, strengthened by reliable analytical inquiries, lead to conclude that the fungin attacks are responsible of some chemical transformations, in particular way of substances of phenolic nature present in the cork, in halogenated derivatives ύ. responsible for the typical smell or cork taste abovementioned.
The organoleptic character of the cork taste is expressed in unpleasant olfactory sensations comparable to . for example . the smell issued by wet cardboard . by moulas by hides or aged leather etc. A simple organoleptic routine investigation for the area operators ponts out, in a valuable way . the presence of particular anomalous smells, among which those ascribed to the cork taste, dipping the cork in a hvdroalcoholic solution at 10%V or in white wine for a period equal to twenty four hours.
At the present time an application such as that consequent from the following proposal doesn't exist and has never existed.
EXPOSURE OF THE INVENTION
We would like to suggest a physical chemical method, completely innovatory, for the washing of cork materials: this method foresees the use of suitable activated carbons in an aqueous suspension to remove the responsible substances of the cork taste and of the unpleasant smells from cork materials. The special absorbing abilities of activated carbons are well-known.
The most important characteristic showed bv these substances is pointed out bv the selective absorption in connection to the substances to absorb and to the particular typology of the activated carbon utilised.
The absorbing action of the activated carbons is linked to different criteria joined to the technologies used in the preparation of the activated carbon, to the specific granulometry.
The method which is proposed is innovatory for the materials to treat because it has never been thought to use the activated carbons in an aqueous suspension to apply to cork industry for the washing of materials different dimension corks of natural type, cork washers, agglomerated corks . mono- agglomerated corks and bi - washered. cork granulated) to remove all those substances considered responsible for the taste of cork and anomalous odors.
The method is innovatory also because activated carbons are used through a technology that foresees the use of the same in an aqueous suspension.
In a suspension consisting of water as transmitting mean, bv activated carbons and bv cork materials a physical chemical mechanism starts for which we have an absorption bv the carbon with a consequent removal of the substances responsible for the cork taste for unwanted possible smells present in the cork.
The application of the method to the cork materials becomes, accordingly an innovatory application with a polyvalent outcome: a) The use of activated carbon in aqueous suspension adapted for cork materials. b) The operative simplicity in the applicability to the cork industry c) The execution of the whole process at room temperature. d) The use of an harmless product for the area operators and for the materials to treat e) The use of a not aggressive, not irritating and not polluting product. f) The chance of collecting the used water for the whole process g) The elimination of the problem of the cork taste and other anomalous smells present in the cork. h) The use of an aqueous suspension of activated carbons in dust allows an optimal contact among the particles of activated carbon and surface of the cork materials.
The particular granulometry of the activated carbon utilised allows the micro particles of this, present in the aqueous suspension, to penetrate in the interstices of the surface of the cork materials, inside the lenticels or pores and in their whole surface.
The whole is supported bv the transmitting action of the water that allows the particles of the activated carbon to come into contact with the all superficial parts of the cork materials allowing accordingly an efficient contact among the particles of the carbon and the absorbable substance present and linked to the surface of cork materials.
There fore a mechanism of physical chemical type begins that leads to the formation of new bonds among the particles of the activated carbon and the different absorbable substances from this with a consequent removal of the same from the surface of the materials.
The washing is carried out at room temperature and foresees the treatment of cork material with a suspension of activated carbon in dust obtained from coconut shells. The granulometry of the dust of the activated carbon is inferior to 0.075 millimetres The concentration of the suspension of washing is of a gram of activated carbon for every litre of water of fountain utilised in the treatment of the materials.
The activated carbon in hand, for the treatment of the activation suffered, turns out very micro- porous and presents accordingly, a very remarkable surface of absorption.
The several proof carried out on cork materials with a suitable technology that characterises this method allow to establish the special efficacy of the suspension of the particular activated carbon to remove the halogenated substances and in this case of the whole substances responsible for the cork taste and possible anomalous smells ( the halogens, the halogen aliphatic derivatives, the halogen arenes. the polv-halogen arenes. the halogen phenols, the poly-halogen phenols, and in this case the trichloro-anisol known with the abbreviation T.C.A.. the trichloro-phenol and their isomers). It presents, also, a good absorbing action to the substances of phenolic nature and polv phenolic not halogenated such as the tannins, aromatic aldehydes present in the cork materials. The mechanism is a physical chemical one because bounds among the particle of the activated carbon present in the suspension and the different substances responsible for the cork taste or anomalous smells are established.
The method makes use of natural products completely harmless for the area operators and for the materials to treat and reflects faithfully, in its applicability, the sever rules foreseen for the use materials to assign to the control and preservation of foods.
The material (cork, granular cork, washers) is subjected to a prewash to remove possible splinters of cork, dust of cork, soil and other material in case present. It is then dipped in a suspension of activated carbons in dust of a concentration equal to one gram of activated carbon per litre of
suspension utilised and the whole subjected to an interrupted slow agitation for a period of at least ninety minutes.
It happens, for contact between the suspension and the material to treat, an absorption of all those substances responsible for the cork taste and in general for the anomalous smells because of the begin, in the case, of the physical chemical balance moved towards the forming of links among the activated carbons and the different absorbable species.
When the treatment ends, the material is freed from the suspension for the discharging of the same and then subiected to an active washing with water of fountain to complete the removal of remainders of the activated carbons and possible splinters of treated material and at last sent to a special desiccator
The waste flows in a tank of settling and the water of the reaction and washing, seasonably filtrated. could be used again for others treatments.
THE BEST WAY TO CARRY OUT THE INVENTION
The proofs were carried out on samplings of cork materials with controlled organoleptic problems and on samplings coming from whole lost of industrial production of cork so called natural, agglomerated cork and washers.
The investigation, in any case, has always been carried out in parallel on materials treated with the above mentioned method and on no-treated materials belonging to the same lot taking, for the test, the same number of corks or washers.
The methods used to find the presence of the substances responsible for the cork taste are sensory ones and are those official.
METHOD TO WASH THE CORKS IN THE LABORATORY TO CONFIRM
THE RESULTS.
THE PREPARATION OF THE SAMPLE
The proofs has been carried out on corks of natural type of different dimensions and on mono - agglomerated corks or biwashered corks in a fortuitous way one hundred of corks are collected from one lot of production esteemed in fifty thousands corks.
They are divided, in a fortuitous way, into two groups of fifty corks called A and B: The A group is subiected to the treatment with the activated carbons as below showed, the B group is left as it is and closet in a plastic bad till the sensory investigation
THE PROCESS
The fifty corks of the A group are rinsed out, under an uninterrupted stream of water fountain to remove from them dust of cork, soil, splinters of cork or other materials that cold interfere negatively in the execution of the method. The initial cleaning of the corks can be carried out rising out them, inside a container, for some times utilising suitable portions of water of fountain end going on every time to the removal of the water of washing.
They are then, inserted in a container of glass of four litres supplied with a hermetic seal cork .
In another container of glass four litre of capacity, at room temperature, the suspension of activated carbons is prepared in the following way: for litres of water of fountain are poured out in the container to whom four grams of activated carbons are added: the suspension is agitated to suspend in an optimal way, the activated carbon in the water.
The prepared suspension is poured out inside the container that contains the corks till a completed filling of the same.
The container is closed: the corks must result completely dipped into the suspension and this is maintained under slow agitation which is secured bv the action of a magnetic agitator.
The washing with the suspension of the activated carbons has a length of ninety minutes.
After the treatment with the aqueous suspension of the activated carbons . the corks are, again and again, rinsed out, for a period of twenty minutes, with an uninterrupted stream of water of fountain to remove possible traces of activated carbons, dried in a special desiccator or stove at a temperature of 35° C- 40° C for a period equal to twenty- four hours and then subiected to a sensory investigation.
METHOD FOR THE WASHING OF THE CORK WASHERS
The method above mentioned for the washing of the corks is applied faithfully to the treatment of the cork washers.
In the particular case, esteemed that the volume of the washers is clearly inferior (eight- then washers for a cork) to the volume of the container for the washers, accordingly, in a proportional way, the quantity of the suspension of activated carbons to be utilised for the washing of fifty washers is reduced. The volume of the container for the washers is : 0.5 litres.
Also in the particulars case one hundred washers, coming from lot
Of production esteemed in two hundred thousands of washers were taken, in a random way. They are divided, in a fortuitous way, into two groups of fifty washers called A end B: the A group is subjected to the treatment with the suspension of activated carbons as shown below
The B group is left as it is and closed in a plastic bag till the sensory investigation.
PROCESS
The fifty washers of the A group are rinsed out, under an uninterrupted stream of water of fountain to remove from them dust of cork, soil, splinters of cork or other material that could interfere negatively in the execution of the method.
They are, then inserted into a container of glass of half al litre, provided with a hermetic seal cork.
I another container of glass, of a volume one litre, at room temperature, the suspension of activated carbons is prepared in the following way: a litre of water of fountain is poured into a container to whom a gram of activated carbon is added, the suspension is shaken to suspend in an optimal way the activated carbon into the water.
The suspension so prepared is poured out inside the container with the washers till a complete filling of the same.
The container is closed: the washers must result completely dipped into the suspension and this is maintained under a slow agitation secured bv the action of a magnetic agitator.
The washing with the suspension of the activated carbons lasts ninety minutes.
After the treatment with the activated carbons, the washers are again and again, rinsed out for a period of twenty minutes, with an uninterrupted stream of water of fountain to remove possible traces of activated carbons, dried in a special desiccator or stove at a temperature of 35° C - 40°C and then subiected to a sensory investigation.
RESULTS OF LABORATORY TEST
The analytical investigations utilised for the search of the cork taste or other possible anomalous smells are those official of sensory type the method used foresees the immersion of the material (corks-washers) in a hydroalcoholic solution at 10-12%V of alcoholic containing tartaric acid at 0,2% as acidulating, at room temperature and for a period of twenty- four hours. In order to, white wine of the same alcoholic gradation can be used.
INVESTIGATION OF THE CORKS.
Both the A and B fractions of washer above mentioned are inserted into two different sterile containers of glass each of a volume of four litres provided with a hermetic seal cork- Inside of each the hydroalcoholic solution prepared as above shown or some whit wine till a complete filling is poured, in such a way that the corks result completely dipped into the solution. Both the containers are hermetically closed and let to rest, at room temperature, for twenty-four hours. When the time is over you proceed with the sensory investigation of both fractions and analyse every single cork checking the presence or the absence of possible anomalous smells. You
record the number of the corks found with problems of cork taste or other possible anomalous smells. The percentage of the anomalous corks of the whole lot is given multiplying the number of the corks found bv two.
From the several analytical investigation carried out it is emerged: the samplings relative to the treated corks with the method of the suspension of activated carbons don't show any of the imperfections above mentioned.
On the contrary, the investigations led in parallel on samplings of not treated materials have always shown, with a changeable percentage the organoleptic problems above delineated.
INVESTIGATION OF THE WASHERS
Both the A and B fractions of washers above mentioned are inserted into different sterile containers of glass each of a volume of half a litre provided with a hermetic seal cork. Inside of each the hydroalcoholic solution prepared as above shown or some white wine till a complete filling is poured in such a way that the washers result completely dipped into the solution. Both the containers are closed hermetically and let to rest, at room temperature, for twenty-four hours. When the time is over you proceed with the sensory investigation of both fractions and analyse every single washer checking the presence or the absence of possible anomalous smells. The percentage of the washers with anomalous smells of the washers with anomalous smells of the whole stock is given multiplying the number of the washers found by two.
From the several analytical investigation carried out it is emerged that the samplings relative to the treated washers with the method of the suspension with activated carbons don't show any of the imperfections above mentioned. On the contrary, the investigations led in parallel on samplings of not treated materials have always shown, with a changeable percentage, the organoleptic problems above delineated.
INDUSTRIAL APPLICABILITY
The use of the suspension of activated carbons is studied in a particular way for the cork industry, but its applicability spreads also over treatments with wineshops, food packaging industry, distilleries ancj n general for all the firms of the area that in their cycle of production foresee the use of cork material.
The utilised technology and The whole process are addressed to:
♦ treatment of corks defined natural
♦ treatment of corks defined industrial (agglomerated type)
♦ treatment of corks defined industrial (agglomerated type with washer)
♦ Cork granulated
Cork washers of several dimensions the technology for the whole process is very simple and for this the traditional machines of washing already present in the cork firms can be used (fig. 1-2-3) They can contain, according to the dimension of construction and to the different size of the corks a changeable number of these included between ten thousands and twenty thousands. The estimated capacity is at least ten times superior to that estimated for a cork of medium dimension.
The industrial application foresees the following stages a) Insertion in the machine of washing of the corks or washers . b) Opening prewash of the cork material with a cylinder in slow rotation sending uninterrupted streams of water of fountain for a term of five minutes to remove, from these dust, splinters of corks, soil or other material in case present. c) Centrifugation of the material to get out prewash water d) preparation in the tank of washing of the suspension of activated carbons. Such suspension is prepared in the following way: to two hundred and forty litres of water of fountain two litres of aqueous suspension are added containing two hundred and forty grams of activated carbon. The homogeneity of the suspension is assured by the continuous rotation of the cylinder inside the tank of washing e) washing, with a slow rotation, for a suggested time not below at ninety minutes discharging of washing water f) at this stage the centrifugation the material for a period of two-three minutes is suggested g) rinse with a cylinder in slow rotation of the cork material subjected to uninterrupted streams of water of fountain for at least twenty minutes h) final centrifugation of the material i) consignment of washed material to desiccator