EDITORIAL

Welcome to the 3rd E4Water Newsletter!

There are news at the Dow Case Study site – The pilot plant in Terneuzen (The Netherlands) was successfully started and of-ficially opened in November 2013. The E4Water Consortium will meet there in April for the project’s Midterm Meeting. This is a good opportunity to link the discussion of the progress in E4Water with learning about the progress directly at a pilot site.

In this issue we continue our series of presenting the case studies in E4Water. The partners from the SolVin case are working on technologies for a treatment train concerning the loop closure in their PVC production plant at the site in Martorell (Spain). After developing and optimizing technologies the first part of the pilot plant is already under preparation and planned to be started soon.

In order to be able to treat and reuse the wash water in the process at affordable costs, the partners from the Procter & Gamble case study are working on the development of a technology train. Several tests are ongoing. Selected technologies need to be

optimized before building up, starting and running a test pilot in a real plant. This is scheduled for by the end of the year.

Please feel invited to visit our website (www.e4water.eu), which gives further details on the E4Water project and on upcoming events related to Industrial Water Management.

Your E4Water Team

Ec onomic a l ly a nd Ec olog ic a l ly Eff ic iEn t Wat Er m a n ag EmEn t in t hE EuropE a n chEmic a l indus t ry

Issue 3 – February 2014

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E 4 wAT E R N E w s L E T T E R c O N T E N T s :

The SolVin Case 5

The Procter&Gamble Case 8

Announcements 10

www.e4water.eu

successful start-up of the Dow case study “Mild Desalination Pilot” at Evides site

The aim of this case study is to find the best way to treat different locally available slightly brackish water sources in a cost effective way to produce a multifunctional water source for agriculture or industrial purposes. The main water quality limit to achieve is an electrical conductivity of <1 mS/cm. Three different raw wa-

ter sources were selected as being most interesting for testing and final reuse: Spuikom water (runoff rainwater from Dow-site stored in an open reservoir), biox effluent from the WWTP of Dow and cooling tower blowdown water (for the pilot we use the cool-ing tower blowdown from the neighbouring powerplant Elsta).

Official opening of the pilot by Lambert van Nistelrooij in presence of Evides and Dow executives

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Selection of the technologies

After a literature study to select the most interesting desalination technologies, lab-testing and evaluation, two desalination tech-niques were selected for testing: nanofiltration (NF) and electro dialysis reversal (EDR). As a start, one joined pre-treatment with

coagulation, lamella sedimentation (LS) and ultrafiltration (UF) is selected. Later on the pre-treatment can be adapted if necessary for tech-nological or economic reasons (to optimise treatment costs).

www.e4water.eu

Opening of the pilot

After quite an extensive search for equipment suppliers and evaluation of offers, Logisticon Water Treatment (LWT) was se-lected to build this pilot. After two weeks of installation on site the first water went through the pilot at the end of October 2013. Pre-treatment and nanofiltration were installed, only the EDR will

follow by the end of April 2014. At November 29th, the pilot was officially opened by Lambert van Nistelrooij, member of the Eu-ropean parliament by pushing a button which gave way to the water for flowing through the pilot.

Pilot testing

A research plan for the pilot plan testing was set up to address all research questions in the timeframe until the beginning of 2016. The main approach is to perform a quick scan per water type of one month each followed by a more elaborate work after these three first months. Detailed study is required to determine the effect of the seasonal fluctuations of the water quality on the pilot performance, optimisation of process parameters and long term effects (like fouling). The quick scan per water source is also divided in different steps. First the coagulation/sedimentation is tested under various conditions (different coagulant dosages, mixing energy and flows). The pilot results are also compared with accompanying (lab scale) “jar tests”. After determining the rough optimum settings of the coagulation/sedimentation step, the UF-unit is started. For this unit the interesting parameters are flux, backwash frequency, cleaning chemical usage (concentra-

tions and frequencies), and permeability decline. When the UF is operating stable the NF is taken into operation and tested.

Scheme of pilot set-up

Evides ongekend betrouwbaar

Pilot E4Water

Mild desalination of different water streams

Nanofiltration

Electro Dialysis Reversal (EDR)

Permeate (= Process water)

Ultrafiltration Lamella separator

Concentrate

Diluate (= Process water)

Concentrate

Flocculator

Backwashwater

Sludge

Biox effluent

Spuikom

Cooling tower blowdown

Toast for a successful pilot research

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DOw cAsE sTUDY: FIRsT PILOT REsULTs The first water source tested was the Spuikom water. As feed water for the pilot, water from the adjacent ditch, which has an open connection with the Spuikom, is used. Next the biox ef-fluent was tested and finally in January 2014 the cooling tower blowdown water.

Turbidity, pH and conductivity of the water are continuously monitored. In fig 1 the quality of the Spuikom water is shown. The conductivity will be dependent on the rainfall. In this period there was quite some rainwater and therefore the conductivity was rather low.

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Pilot E4Water DowWaterquality: spuikomwater

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Fig 1 Raw water quality of Spuikom water

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Fig 2 Effect of iron dosage (mg Fe/l) on the turbidity of the effluent of the LS

Coagulation and sedimentation

For each of the water types the dosage of the flocculant (FeCl3) has been varied and tested. For the biox effluent the results of the turbidity are shown in the graph (Fig 2). The mixing velocity in the flocculator was 15 rpm and the flow through the LS was

4 m3/h (=0,33 m/h). The effluent quality is not that much affected by the dosage rate, but the results with 10 ppm Fe are slightly better than with 5 ppm.

Ultrafiltration

The ultrafiltration unit currently consists of one Inge Dizzer 60 0.9 mm module with a possibility to put a second module in parallel if needed to achieve a higher flow. There is also a possibility to make some adaptions to the unit in order to be able to test other membranes (e.g. Dow UF). The flux for the tests was 60 lmh, backwash frequency was each 15 min, and two different CEB’s

(Chemical Enhanced Backwashes) were performed. At the start there was a separate citric acid (4 g/l) CEB and caustic soda CEB (0.4 g/l). Caustic CIP was transformed in a combined CEB (first caustic and then citric acid) to remove possible scaling occurring during the caustic CEB.

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Fig 3 Trans membrane pressure for UF on Spuikom water (until Dec. 5th) and biox effluent

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As can be seen in Fig 3 in the beginning the TMP increases with time. Due to optimisations such as the change of the CEB’s, a stable operation has been reached for the Spuikom water. At the 5th of December the change was made towards biox efflu-

ent with a higher temperature (red line). The blue dots mark the period with biox effluent and in this period the Fe-dosage was changed several times. The periods with 10 ppm Fe (marked by an ellipse) were the most stable.

Nanofiltration

The nanofiltration unit consists of 6 modules (Dow Filmtec NF90-4040) with recycle flow. Fresh feed water is 1.2 m3/h and 1.4 m3/h recycle flow is used to maintain the minimum cross flow velocity. The recovery is set at 75% with a flux over the mem-branes of 20 lmh. Key performance indicators are: NPD (nor-malised pressure drop across feed spacer), MTC (membrane transfer coefficient) and NSP (normalised salt passage). These will be tracked to monitor the membrane performance. Beside online measurements, also water samples are taken on a regular basis and analyzed on key components. In Table 1 the results for

the NF on biox effluent are presented. A good removal (> 90%) is achieved for nearly all components (except nitrate), even for TOC.

Further research will be focussed on long term experiments. Be-side this, the first results of treating cooling tower blow down water are indicating bad coagulation and rapid fouling of the UF. Therefore special efforts will be devoted to find a solution for treating this waters source.

Table 1 Overview analysis of biox effluent treatment with NF: feed, permeate and concentrate

Parameter unit NF fresh feed NF permeate NF concentrate

Temperature °C 20 20 20

pH - 6,9 5,7 7,7

TOC mg/l 8,7 <1 35

Chloride mg/l 162 12 585

Sulphate mg/l 134 1 500

Ortho phosphate mg/l P 0,021 0,006 0,26

Bicarbonate mg/l 77 8 282

Ammonium mg/l NH4 <0,03 <0,03 0,04

Nitrate mg/l NO3 16 4,6 47

Sodium mg/l 110 9 380

Potassium mg/l 14 1 51

Calcium mg/l 57 0,6 210

Magnesium mg/l 13 0,1 52

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The solVin case: Towards water Loop closure

Ensure the process continuation by closing the water loop and minimizing fresh water use

Owned 75% by Solvay and 25% by BASF, SolVin is an uncon-tested leader on the vinyls market. SolVin covers the entire vinyl chain, from salt to chlorine and soda through dichlorethane, PVDC and vinyl. SolVin’s products are sold from several manu-facturing plants in Belgium, Germany, Italy, France and Spain and through commercial agencies elsewhere in Europe and on export markets. The even geographic distribution of these sites enables us to optimize the flow of raw materials and finished products.

1400 employees work in this motivating environment of team-work, open communication, knowledge sharing and leading edge technology. At SolVin, clearly defined industrial, commer-cial and human values support a long-term and highly innovative sustainable devel-opment strategy. Constant investment in product improvement and advanced pro-duction technology profile SolVin as the long-term partner of choice for vinyl pro-cessors.

In 1968, the SOLVAY Group bought 30 acres of land on the farm “La Torre de Mar-torell,” and after obtaining the appropriate licenses, the production started on 4 De-cember 1972, with half the current capac-ity. Since the chemical factory in Martorell pvc Solvay has covered several stages to reach its current state of industrial maturity. With ongoing policy of upgrading its facili-ties, with major investment efforts and the

ongoing training of its staff to progress in the technological in-novations successive World PVC chemical industry have made possible the current reality, a factory with facilities originates in which 60% of PVC products produced in Spain. SOLVAY factory in Martorell employs 400 workers (70% of them live in Martorell and nearby areas.)

In Martorell, thousands of tons of products are being produced for various industries: water treatment and purification, paper industry, textile industry, bleach and detergent, food and glass industry and mainly to the processing industry of plastic, bound industries as diverse as construction, automotive, decoration, agriculture, packaging, toys or medical applications.

INTRO of Martorell Solvin Spain is located in a region where a water scarcity is a fact since one or two decades. Thus, both water abstraction and disposal are regulated by law and permits, having stringent limitations which cannot be trespassed.

In the region, the supply of water to both municipal and indus-try comes from storage reservoirs that are supplied by snow-water from the Pyrenees. Located in a coastal area with small river basin in southern Europe, the area is facing periodical water shortage since the 1990’s. The natural water resource availability can sometimes be lower than the water demand in the highly populated area and touristic. This situation leads to the need to find alternative resources in order to ensure the water supply in the entire water network.

Inside E4water: Presentation of two case studies: solVin and Procter&Gamble

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What is the issue?

In a typical PVC production site as SolVin, there are three dif-ferent waste water qualities. These are the mother water (water from the reactor after separation of the PVC-product on cen-trifuges) which is clarified in a physico-chemical treatment, the blow-down coming from the cooling tower and the purged water of the demineralization unit (RO or Ion Exchange).

The blow-down and purged streams contain mainly salt and probably airborne suspended solids which are rather easy to treat, when necessary. On the opposite, with the mother water stream, the issue is the presence of the reagents and additives that have been introduced during the polymerization. The most problematic reagent, in the water recovery purposes, is the PVA (polyvinyl alcohol, a dispersing agent) which can be found in the mother water.

SolVin has already experienced membrane separation on mother water: however, the presence of polymeric PVA blocks the membranes. In addition, the salts are known to interact with the reaction of polymerization and thus affect the final PVC quality specifications.

The objective

The mother water is qualified as a complex organic load and high flow (in the case of Martorell approx. 100 m³/h). The PVC production unit under consideration uses about 33 % of the total on-site water consumption. The aim is to close the water loop for this production and to realize additional water savings of 25 %. The technologies under investigation for the new treat-ment trains are membrane bioreactors (MBR) for the removal of the biodegradable PVA and ammonia, pre-treatment for demineralization (multimedia filter or granular activated carbon), followed by a demineralization step to reduce the salt concentra-tion (reverse osmosis, ion exchange or membrane distillation).

In the first stage the most efficient MBR design has been screened and 4 types have been tested in different module de-

signs (new and existing). For the demineralization ion exchange and membrane distillation have been tested and evaluated against reverse osmosis.

In the second stage treatment options for the concentrates will be evaluated. Membrane distillation crystallization will be tested to generate a dry solid fraction and a pure water fraction. In syn-ergy with the microalgae developments for Case Study 6 (CBD/Kalundborg) microalgae treatment will be demonstrated on-site and will be tested at lab scale with 2 other typical PVC waste-water streams. The resulting treatment train concepts will be ap-plicable for a wide range of polymerization processes in industry.

Increase in the demand of the product followed by an increase in productivity makes a larger water consumption for the site. Suspension PVC is produced in an aqueous process. Approx. 2 m3 of precious water are used in a conventional process per ton of PVC. Up to now this water could mainly be re-used in flushing purposes, but the demand for flushing water is small compared with the water demand to polymerize the PVC. So the water is usually discharged after treatment in a physico-chemical waste water treatment to a receiving body.

In the early 2000, Martorell was pioneering the water recovery technology in PVC production: a recovery of more than 60% of the water reduced significantly the fresh water abstraction volume.The real challenge of the PVC production site like Martorell is now starting from here, a higher water recovery is needed to be able of nearly close the water loop of the production unit.

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What will happen next?

In 2013, technical specification of the MBR and RO pilot units have been launched to several membrane water treatment unit suppliers. A pilot unit applying hollow fiber membranes has been chosen and the industrial pilot trial will be started during the first quarter of 2014 with a total operation period of 1 year.

The project team is now pursuing to get a RO unit to equip as a modular unit downstream the MBR unit.

During the trial period, the quality of demin water after a sequen-tial MBR&RO treatment will be verified and demonstration of the compatibility of the recovered water quality with process needs (polymerization trials) will be also conducted at industrial scale. The aim of the whole pilot plant is to show that the selected desalination plant was the right choice and to demonstrate the stability/robustness/reliability of the technology in terms of water quality.

What has been done so far

The E4Water Case Study 3 consists on the design, development and validation of a treatment train for the decontamination of the final effluent from the PVC plant in order to reuse the treated water in the process. SolVin is working together with partners from UCM and VITO.

Different membrane technologies have been tested in the MBR: flat-sheet, flat-sheet with back-flush (VITO-IPC) and hollow fiber. All tested technologies proved to deliver similar stable results after an adaptation phase of the biomass to the specific COD (mainly PVA) and under classical operating conditions of Biologi-cal wastewater treatment.

Considering the need for desalination of the effluent from MBR in view of its recycling as process water for polymerization, additional specifications have been set and met for the final effluent. Among the parameters to carefully check during the MBR piloting trials, mass load, pH control and foaming tendency are identified as sensitive parameters.

The desalination was performed applying 5 different technolo-gies. The best produced water conductivity was reached with membrane distillation, 2-pass RO and two-stage CDI; a good performance is possible with electrodialysis; the one-pass RO produced a water with a slightly lower water quality. After the technical and commercial validation, RO is the technology of choice for piloting due to the much lower production cost (investment & operation) of this technology.

Thanks to the wide review of MBR and desalination technolo-gies, the input for up-scaling to on-site pilot trials is very well documented and enables contacting suppliers with trustful data-sets.

Next to technical tests, a modelling has been launched at TUB: A material and energy balance for the major process units of PVC polymerisation and wastewater treatment has been computed. With this model, two typical compounds in the water cycle can be computed.

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The Procter&Gamble case – Reuse of water In-Process

Enhance in-process water loop closure by integrating biocidal with wastewater treatment technologies

What’s the issue?

PGB produces a wide variety of consumer goods products which are liquid in nature: Fabric care (fabric detergents, fabric enhancers, etc.), Home care (dish washing liquids, hard surface cleaners), Hair care (shampoos, conditioners, etc.), and Beauty care (Skin care, etc.). The production facilities have ‘making units’, where the product is produced into bulk storage tanks, and ‘packing departments’ where the product is bottled and then packed for distribution to clients.

The targeted waste water stream in the E4Water case study is the wash water from cleaning and sanitization activities in mak-ing and packing departments: This water is created during the wash-out, which is done to avoid product contamination when switching between product variants. Similar type of wash water is generated during the hot water sanitization which needs to happen to avoid bacterial growth and contamination of the liquid detergents. This wash water is in general a mixture of clean wa-

ter and detergent product but bacterial contamination and bac-terial growth in this water is the main issue and barrier why this wash water needs to be discharged.

P&G has since many years a strong sustainability program in place which has led globally to a 55% water consumption reduction in the period 2001-2010 (volume adjusted). This general water effi-ciency increase has cause that the wash-water is getting more and more concentrated and cannot be treated anymore in traditional waste water plants. The current practice is that the wash water is separated from the rest and that this stream (COD>20,000 mg/l) is treated externally at a high cost (>100 Euro/ton) by incineration or advanced treatment systems as wet oxidation. So the more a production site becomes water efficient, the more it cost to treat the waste water. This fact is making further progress on water efficiency very challenging. In addition, the low volumes of these wash-waters are making high capital investments difficult to justify.

The objective:

The objective is to develop the technology to be able to recycle the wash water back into the process at affordable cost versus the current external treatment. Procter&Gamble is working to-gether with TNO, Campden, Ondeo, Vito, and UCM. The team investigates 2 possible recycling options: (I) blend the streams directly back into the specific process or (II) upgrade wastewater to generic process water.

To achieve this: three innovation pathways are combined:

•Segregation technology (to split the wash-water into a low concentration (< 2,500 mg/l COD) and a high concentration (>150,000 mg/l COD) stream.

•Biocidal technology as pasteurization, etc.

• Innovative wastewater treatment technology as MBR, etc.

Procter and Gamble (P&G) is world’s largest non-food con-sumer goods production and distribution and world’s largest detergents manufacturer and employees more than 130.000 people. In the EU, P&G has 45 manufacturing sites and 6 R&D centers. Partner in this E4WATER consortium are the engineer-ing and R&D centers located in P&G Brussels Innovation Cen-tre in Strombeek-Bever in Belgium, which is the largest P&G technical centre in Europe.

Process integrated solutions are developed by Procter & Gam-ble Eurocor N.V. Involved in this project are 5 R&D Departments (Process Breakthrough, 3 Platform R&D groups, R&D Analytical).

Technical know-how about water efficiency and end-of-pipe waste water recycling techniques + general engineering sup-port is provided by Procter & Gamble Services Company NV. Involved in this project are 3 supporting Engineering depart-ments (Corporate Engineering Business Solutions, F&HC Pro-cess Breakthrough engineering, Platform Engineering) and sev-eral Manufacturing sites.

© Procter & Gamble

E4Water: Progress beyond state of the art: combine ‘waste water treatment technology’ and ‘pasteurization/sterilization’ technology to recycle HIGH CONCENTRATED WASH water generated during Cleaning and Sanitisation (COD 20,000 - 50,000 mg/l)

Pre- treatment

foodsterilizationtechnologyapplied onchemical wastewater

In-line sensors

Waste water technology

Processes

WWTP

Natural water recources scarcity, factors: quantity, quality, regulation

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What has been done so far?

Technology development on segregation with membranes; 2 case studies.

Membrane technology has been tested to treat the water from liquid detergent manufacturing. Tests were done on liquid detergents as Dash, fabric enhancer products as Lenor and hand dish wash liquid as Fairy/Dreft.

The selected treatment concept for wash wa-ters coming from a Lenor production plant is based on the application of ultrafiltration (UF) or nano-filtration (NF). Pre-screening of various membranes demonstrat-ed a high retention of the organic components. The permeate contains low concentrations of detergents and may be reused in the production after reverse osmosis.

In preliminary NF tests with spiral wound membrane elements, the flux recovery cleaning phase was identified as critical point for long-term stable filtration of the P&G Lenor waste stream. Within the new focus on tubular membrane systems, with their advantageous properties like lower fouling tendency and supe-rior cleanability, two filtration strategies were evaluated on pilot scale: membrane-selective NF and open UF with gel layer-ren-dered separation capacity.

The permeate production rates and quality (COD content below 2500 ppm spec) were satisfactory in both systems for the batch filtration of Lenor solution. At the same time, total flux recoveries could be obtained by flushing with mild caustic solution. On the other hand, only the NF separation was sufficiently selective for cationic detergents (<10 ppm) at room temperature. The long-term NF membrane performance and cleaning efficiency was confirmed and preserved in consecutive batch filtration cycles. In the filtration of Lenor:Dreft/Fairy mixture solution, membrane fouling remained absent and higher COD rejection rates could be obtained.

At elevated temperatures, the NF membrane becomes less se-lective for cationic detergents, by which the envisaged permeate quality spec is not achieved. In search of the optimal membrane

system, further lab scale screening of tighter (pre-treated) NF and Reverse Osmosis membranes will be performed at elevated feed temperatures.

For wash waters coming from a Dash production unit, an alter-native treatment train is required. The first step is an UF step similar to the strategy for the Lenor streams. However, the for-mulation of Dash contains various small organic components which are difficult to retain by membrane filtration. These com-ponents proved to be well biological degradable. Therefore the membrane filtration step is combined with a biological treatment of the membrane permeate before discharge. This permeate is characterized by COD of 4000 – 5000 ppm (BOD/COD ~ 0.8) and ± 10 ppm of surfactants. In order to prove the biological treatability of this permeate, VITO operated an aerobic mem-brane bioreactor in their lab facility. After a short period of sludge adaption, the unit was operated stable. The analyses of perme-ate samples showed good bio-degradation (COD < 50 ppm and BOD <5 ppm) and full nitrification. The MBR was operated up to a F/M ratio of 0.4 with a sludge concentrations of 9 g/l.

Membrane Bioreactor (MBR) pilot unit at VITO.

What will happen next:

Further lab testing will be done to understand better why at el-evated temperatures, the NF membrane becomes less selective for cationic detergents. In search of the optimal membrane sys-tem, further lab scale screening of tighter (pre-treated) NF and Reverse Osmosis membranes will be performed at elevated feed temperatures. Also changing operational parameters (e.g. re-ducing pressure across membranes, pre-conditioning the mem-branes, etc.) will be investigated.

As alternative, cooling of the water will be considered.

Detailed engineering on a 6 ton/day membrane and MBR unit has started. The intent of P&G is to build this and to have this installed in one of the sites by end 2014 so testing in a real plant can start. The aim is that the concentrated stream would be re-used externally. The water would be used to feed cooling towers.

Plan of the 6 ton/day membrane unit for the Procter & Gamble E4Water pilot site.

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This project has received funding from the

European Union’s Seventh Programme for

research, technological development and

demonstration under grant agreement

No 280756.

FP7-NMP-2011.3.4-1 – Start Day: May 1st 2012 – Duration: 48 months

Dr. Thomas Track / Dr. Renata Körfer / Dr. Christina Jungfer

DECHEMA e.V.Theodor-Heuss-Allee 2560486 Frankfurt am MainGermany

Phone: +49 (0)69 7564 -427/-619/-364Fax: +49 (0)69 7564 -117E-Mail: track@dechema.de koerfer@dechema.de jungfer@dechema.de Disclaimer notice: The European Commission is neither responsible nor liable for

any written content in this newsletter.

CONTACT

DisclaimerThe E4Water project has received funding from the European Union’s Seventh Programme for research, technological devel-opment and demonstration under grant agreement No 280756. The content of this newsletter cannot be considered as the Eu-ropean commission’s official position and neither the European Commission nor any person acting on behalf of the European Commission is responsible for the use which might be made of it; its content is the sole responsibility of the E4Water project partners.

Although the E4Water consortium endeavors to deliver high quality, no guarantee can be given regarding the correctness and completeness of the content of this newsletter due to its general informational character.

The E4Water consortium is not responsible and may not be held accountable for any loss suffered as a result of reliance upon the content of this newsletter.

Aachener Membran Kolloquium (AMK)12 - 13 March 2014 · Aachen/Germanyhttp://www.avt.rwth-aachen.de/AMK

Industrial Technologies 20149 - 11 April 2014 · Athens/Greekwww.industrialtechnologies2014.eu

IFAT ENTSORGA5 - 9 May 2014 · Munich/Germanywww.ifat.de/en

IwA world water congress & Exhibition21 - 26 September 2014 · Lisbon/Portugalwww.iwa2014lisbon.org

IWRM Karlsruhe 201419 - 20 November 2014 · Karlsruhe/Germanywww.iwrm-karlsruhe.com/de/home/homepage.jsp

Since the section of the website on upcoming eventsis regularly updated we invite you to visit our website for most recent changes.

E4Water Consortium at the Executive Board Meeting and the ChemH2O/ChemWater Final Conference in Madrid.

ANNOUNcEMENT OF UPcOMING EVENTs - Where you can meet E4Water