Final Report Summary - ENCORK (ELECTRONIC NOSE TO DETECT HALOANISOLES IN CORK STOPPERS)
The wine industry is one of the leading segments in European agriculture, accounting for a significant 4.3% of the total turnover of the sector. With a production of 17.4 billion liters and a revenue of 16.4b€, EC-27 countries account for 60% of worldwide wine production.
The use of natural cork stoppers in bottled wine is the preferred option by both wine producers and consumers. The unique properties of cork guarantee the proper sealing of the bottles while providing the best conditions for the ageing process of the wine. However, the use of cork has a major drawback: cork taint, a common fault in wine associated to the presence of haloanisole compounds (e.g. TCA), which alter the quality parameters of the wine. Recent studies have proven that TCA contamination affects more than 5% of commercial bottled wine.
At the moment the most common solution is the detection of contaminated cork stoppers in the manufacturing plant. However, cork stoppers that successfully pass the quality controls can get re-contaminated at the bottling line. The problem leads to great economic losses and affects the competitiveness of SMEs in the whole wine production chain: cork producers, wine bottlers and winemakers.
The main goal of the project was to develop a solution to detect TCA in wine bottling facilities by using a non-invasive sensing device known as an electronic-nose for the fast detection of TCA at a level of 2 parts per trillion (2 ng/L). The developed system is currently able to test 250 corks per hour and can detect TCA in the level of ppt.
ENCORK has brought together a core group of European SMEs and prestigious R&D organizations with the common aim to develop a prototype to test the effectiveness and potential of an innovative sensing technology for TCA detection in bottling facilities. The work performed by the ENCORK R&D organizations (ATEKNEA-C, ICS, UNITOV and ATEKNEA-H) observes the specifications provided by wine producers SAP and QH and has the technical support from technology manufacturers Szervin and Innosensor. ENCORK also counts with the participation and support of the Province of Modena, one of the most active wine producing regions in Europe.
Project website: www.encork.eu
Project Context and Objectives:
Cork contamination by TCA affects over 5% of wine production, resulting in economic losses of €700M in Europe annually, according to “Salon Alimentaria” of Barcelona. TCA contamination does not pose any health risk at typical concentration but it affects negatively the wine flavour and taste. Due to the relatively high occurrence of haloanisoles contamination and its significant economic impact, the sector is particularly concerned about this problem.
The most straightforward and costs effective way to prevent the haloanisoles contamination consists in detecting cork stoppers at the cork manufacturing plant, however corks can be re-contaminated at the bottling line. In the recent years, wine producers have gradually introduced new methodologies to minimise the impact of haloanisoles contamination. Many cellars require TCA-free certificates for any material they may use in their plants and in addition, they periodically perform analyses to identify possible TCA contamination sources in the environment or in the materials used.
Due to the impossibility of ensuring TCA-free cork stoppers, wine industry demands for an effective method to detect and discard TCA-contaminated corks. Furthermore, wineries require a method that can be implemented in line during the bottling process, right before sealing the bottle.
Therefore, the overall goal of the project was the development of an electronic nose to detect TCA in cork stoppers, and to integrate into an automatized system capable of discarding the contaminated corks detected in the bottling line, keeping the overall production cost of the system below €18,000. The proposed system would detect haloanisoles in cork stoppers at level of parts per trillion and at a speed of 1000 stoppers per hour.
In order to achieve this major goal, the following specific scientific and technological objectives were defined:
• Develop the appropriate sensor arrays to be used in the e-noise
• Develop software/hardware capable to process the sensor information
• Develop gas based sampling system and mechanical system
• Develop an effective prototype at competitive price, adding only a minimum increment to the stopper cost (will not exceed 2% of the cork value). This cost includes power consumption and other consumables as sensor replacement and gases for sampling. Furthermore, the overall initial capital outlay for the ENCORK equipment placed in a process line will need to be in the region of 30,000 Euros in order to make it accessible for SME wineries.
• To grant that the process does not affect the quality and properties of the cork due to the sampling and handling during analysis. Two kind of stopper will be considered: natural cork stoppers and technical stoppers (agglomerated based cork). The risk of technical stoppers is higher and must be investigated beside the classic natural cork because various adjuvants (such as glues) are used to manufacture these products and these could affect the ability of haloanisoles to migrate.
• To ensure that the system is adaptable to the process existing lines as a module just before bottling and has a throughput of 1000 cork stoppers/hour.
Besides the technological and scientific objectives, other objectives related to knowledge transfer and IPR issues were defined:
• Assist the consortium SMEs in taking up the knowledge generated during the project and ensure that the achieved objectives are disseminated to the scientific community.
• To protect the Intellectual Property Rights and to promote the exploitation generated during the whole duration of the project. Facilitating the take-up of results.
• To carry out training activities in order to facilitate the take-up of the project results by the partners of the consortium
• To optimise the applications of resources and to ensure that all aspects of the EC requirements for communication and reporting are met.
The ENCORK project started in January 2014 and had a total duration of 24months. During the project, a solid partnership has been created between SMEs and RTD performers, allowing the consortium to reach the project objectives. The consortium has also counted with the valued support from PROVMO in promoting the project activities. During the first period of the project R&D efforts were devoted to (i) defining the optimal operational conditions to extract the maximum quantity of contaminant from the cork stoppers, (ii) selecting the most adequate sensing material to be integrated in the e-nose and (iii) performing preliminary tests that have yielded very promising results. Starting in October 2014, R&D work was focused on the integration of the e-nose with the sample acquisition system in a laboratory environment, with the aim to minimize response time and maximize reproducibility of the measurements to meet the requirements of an industrial environment. In December 2015, the prototype was sent and tested at SAP facilities in Modena (Italy). Several tests were performed in December and January 2016.
Periodic general project meetings allowed the SMEs to follow up on the progress of the R&D activities, while providing the necessary platform for sharing the multidisciplinary know-how of the different partners in their respective areas of expertise (wine cellars, sensors, machinery for the wine industry, cork industry).
Several milestones were set along the second period of the project with the final goal of having a prototype validated in real conditions, which means at the end user´s facilities.
The main milestone for the first period was the development of the sensor subsystem (WP1). The sensor array, Electronic Nose, is the part of the final system in charge of detecting TCA contamination in the analysed cork stopper. The first task has been devoted to select the sensing materials having the performances required to allow the TCA detection. Different metalloporphryins have been deposited as thin films onto Quartz Crystal Microbalances, used as nanogravimetric trasducers. The receptors showing the best performances in terms of selectivity and sensitivities towards model analytes have been individuated and then exploited in the final sensor array. The next step has been to test the developed array in the laboratory conditions, using the selected sensor array and a manual sampling system, already available at UNITOV facilities. The lab tests were focused on the evaluation of the properties of the e-nose to detect TCA contaminated cork caps, evaluating: 1) QCM sensing properties, 2) external factors influence, in terms of temperature and humidity. For these tests artificially tainted cork stoppers have been used, prepared by the ICS partner. The e-nose performances were checked by measuring two “lots” of cork caps were analysed: one containing TCA contaminated corks (using two different methods: immersion and injection) and the other comprising only TCA-free corks. The e-nose demonstrated a good sensitivity towards the target analyte, showing a good discrimination property among TCA contaminated and control cork caps. The variability of the artificially contaminated cork caps did not allow a reliable test of the system reproducibility, although a clear discrimination was well evident. The next experiments were devoted to determine the sensitivity and the low detection limits toward TCA detection and the sensor response time, in order to determine the number of corks that can be contemporaneously evaluated. The experiments confirmed that the sensors have the sensitivity for the TCA detection in the target application.
The requirements for the ENCORK system are very strict, the e-nose should analyse 3 corks every second. According to the requirements, we designed the electronic board for sensors signal acquisition, the power supply board, as well as the sensor chamber and a software for controlling the system and analysing the measurements. To perform preliminary tests with the system, a temporary pneumatic path that collects the cork stopper headspace and address it to the sensor chamber was also set up. All factorsa affecting the measurement protocol were investigated, temperature and flow of carrier gas.
WP2 deals with the design and integration of a sample handling system that allows the extraction and delivery of the haloanisole compounds from the cork to the e-nose for detection. During the first period, a good progress was made in the development of the sample handling system (WP2). With the main technical support from ICS, the main parameters enhancing the extraction of the TCA from the cork samples were identified. During the second period the laboratory scale sampling chamber and the required auxiliary systems were completed. The control system fully developed and the testing period was undertaken at ATEKNEA-C facilities before the integration with the sensing subsystem was done at UNITOV facilities in Rome. Based on these initial tests, some improvements on the pre-heating system were needed. The low value of gas flow rates required some adaptations in the heating monitoring and control elements. The control system was developed in such a way that it is flexible enough to fulfill the needs of the laboratory set-up, integrating already the main signals required by the e-nose at this stage (mainly to switch between cleaning and measuring). On the other hand, the hardware was selected in such a way that it can accommodate the adaptations required by the final industrial system developed in WP3. This approach allowed the consortium to overcome delays incurred during the first months of WP2.
Integration of the laboratory set-up of the sample handling system (WP2) with the sensing subsystem (WP1) was done in November 2014 at UNITOV facilities in Rome and tests with the integrated system started in December 2014. The conclusions from the testing performed in WP2 served as specifications for the industrial prototype (WP3), whose development started in early 2015. Samples used for the testing were provided by ICS. ICS prepared the contaminated corks using two different methodologies (direct injection and immersion), besides the effect on the temperature on the contaminated corks was checked.
WP3 (Industrial Prototype Design) main objective was to design and develop an industrial prototype based on the laboratory scale system capable of operating in real conditions. Mechanical specification and design, gas handling system, electrical and automation design as well as the control system were developed. Two new features were incorporated in the final prototype in order to fulfill the requirements specified by end users: implementation of 2 e-noses to reduce analysis time and full automation of the cork feeding mechanism into newly designed inspection chambers, designed as a standalone unit. The gas heating and temperature control system was redesigned in order to ensure a more stable and controllable delivery of nitrogen gas to the cork inspection chambers. Much of the automation hardware was reused from WP2 with elements added to power and control the automatic cork handling system and new gas handling system. The control strategy of the industrial prototype follows generally the strategy developed for the pre-prototype WP2, but was further developed to incorporate the fully automatic functionality of the industrial prototype.
WP4 (Construction and System Integration) had the objective of setting up the system integrating all modules developed during WP3. The ENCORK final prototype system construction commenced in June 2015 following approval of the final design by the SME partners. Construction was carried out on a module by module basis by each responsible RTD partner with final construction and integration of the overall system taking place in Ateknea CT’s facilities in Barcelona in September. The prototype was then sent over to UNITOV facilities to calibrate the eNoses with artificially contaminated corks provided by ICS.
WP5 (System Validation) aimed to validate the prototype system in real environment, therefore it was delivered to SAP facilities in December 2015. ATEKNEA-C together with UNITOV installed the prototype and trained the SAP staff on the use of the ENCORK prototype. This training was done together with the Final Project Meeting the 14th of December. Tests continued along January 2016 and report on the results was prepared and submitted in February 2016. Results are promising although further improvements are needed; mainly increase the analysis speed. The analysis speed of the developed system is 250 corks/hour and it is capable to detect TCA in the ppt range as expected. Nevertheless, it is important to mention that validation with real corks are needed and a more robust calibration model based on the real environmental conditions of the cellars.
The consortium created a visual identity for ENCORK. The project website (http://encork.eu/) was used as a platform by the project partners for the diffusion of all the news related to the project and its results. In addition, a project video has been recorded, which is available on youtube (http://www.youtube.com/watch?v=eJufYUbCa04) and also accessible through the website and to all consortium members to use in trade fairs, conferences, etc. for project promotion. Moreover, a Facebook page was created to disseminate ENCORK project https://www.facebook.com/Encork-278903492286346/
A poster and brochure were created and used by the partners during conferences or fairs along the project lifetime.
The wine sector, a pillar of the European economy, is currently facing a number of problems that hinder its competitiveness. The extension of vineyards in the EU-27 is progressively decreasing, shaken by the competition of exports from overseas (North and South America, Australia, South Africa or even China), which are hitting the market with high quality exports. One of the most important problems threatening the competitiveness of the wine industry is the alteration of wine test and aroma caused by migration of odorous organic compounds from cork stoppers to bottled wine, commonly known as cork taint.
This is a problem for which, to date, no effective solution has been found. State of the art methods to detect haloanisole compounds in cork stoppers are based on the use of costly and time consuming instrumental analysis methods that require skilled personnel to operate the equipment and interpret the analytical results. Such analytical methods are destructive and thus they are implemented as quality control methods on a limited number of cork stoppers at the manufacturing plant. Therefore, there is a high probability of recontamination when the cork stoppers are stored in the cellar.
ENCORK is the first non-invasive analysis solution, allowing in-situ analysis of each cork stopper individually, prior to use in the bottling line. The ENCORK technology has been conceived to comply with the main requirements of an industrial environment, which calls for rapid, robust, reliable and easy to operate alternative analytical techniques.
The ENCORK project has put together a group of SMEs with a common interest in developing a solution for a global problem of the wine industry with a group of RTDs with combined expertise in advanced sensor technology, cork research and process engineering. ENCORK is based on the use of chemical sensors able to detect a wide range of chemical compound, which have allowed the development of the so-called electronic-noses. UNITOV and INNO lend their extensive knowledge on this field to develop a system adapted to the needs of wine cellars for the detection of cork taint. To bring this concept to success ENCORK also counts with ICS and their extensive know-how on research related to cork and ATEKNEA with extensive background in process engineering, control and automation.
The project aimed to develop a pre-competitive industrial prototype that complies with the main requirements of a wine cellar, taking as a reference our end users Cantina Paltrinieri (SAP) and Quinta Holminhos (QH). The prototype was tested in the industrial facilities of end user SMEs, allowing the consortium to evaluate the full potential of the technology and to identify the necessary improvements and steps to be followed to reach industrialization level. The obtained results provided a valuable case study to estimate the uptake potential in a wider market.
Through the potential commercialization of the ENCORK technology, technical SMEs (INNO, SZERVIN) could see their competitiveness increased thanks to the manufacturing and marketing a new and promising technology. End user SMEs in turn would directly benefit from the use of this cutting-edge technology in their own facilities. Indeed, the potential for the technology is extremely promising: the estimated market for the ENCORK system was preliminarily estimated at 750M€.
The implementation of the ENCORK technology will allow wine cellars to gain back the confidence of customers in their products, contributing to boosting sales. A detailed Plan for the Use and Dissemination of Foreground was developed at the end of the project, which includes a Business plan for the future exploitation of the technology as well as the Exploitation Agreement that technical SMEs and End users signed as owners of the generated foreground. The foreground belongs in equal shares to the two technical SMEs and two end-users.
Since March 2014 the ENCORK project was using the project website (http://encork.eu/) as a platform for the promotion of all the project activities. Moreover, the consortium used a specific Facebook page to disseminate the project and the different events carried out along the project (https://www.facebook.com/Encork-278903492286346/?fref=ts). ENCORK profile got 79 likes and several hundreds of people were reached through the different posts posted along the project life. Moreover, the questionnaire developed by the partners to gather information about end-users requirements was also posted and promoted via Facebook. Technical SMEs and end-users played a key role in the dissemination of the project, joining several events and promoting the project and the technology, such as Vinitaly, Feira Porto Douro Wine Show, Barcelona Food Technology (BTA 2015), Innovation fair B2B in Toulousse, Exhibition in CNS (Italian conference of sensors), etc. A promotional video of the project was produced and used as dissemination tool. Besides, several TV clips have been shown in Portugal and Italy. Provincia de Modena played a key role in dissemination of the project through their wide presence in relevant events related to the wine industry.
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