This work was supported by the BOF grant for SG from Ghent University. AL is supported by the Rutgers University NSF Fuels-IGERT. SA is supported by the European Union Framework Programme 7 project &#8220;ProEthanol 2G.&#8221; SA and KR are supported by Ghent University Multidisciplinary Research Partnership (MRP)&#8212;Biotechnology for a sustainable economy (01 MRA 510W). JD is supported by an IOF Advanced grant (F2012/IOF-Advanced/094). KR is supported by by the ERC Starter Grant &#8220;Electrotalk&#8221;. The authors thank Tim Lacoere for designing the TOC art figure, Robin Declerck for building the strip and absorption columns and Kun Guo for providing the inoculum source.

1. Assembling the Reactor and Connecting the Stripping and Absorption Units
<ol>
	<li>Collect all necessary material to build the reactor: electrodes, frames and rubbers (See List of Materials). Carefully cut all parts to the same dimensions to avoid leaks while assembling the reactor.</li>
	<li>Drill holes in the reactor compartments to fit a male to male connector. Drill one additional hole in the middle of the side of one of the reactor compartments to fit the reference electrode.</li>
	<li>Prepare a stock of 1 M H<...

<ol>
	<li>Verstraete, W., Van de Caveye, P., Diamantis, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Maximum+use+of+resources+present+in+domestic+&#34;used+water&#34;.">Maximum use of resources present in domestic &#34;used water&#34;.</a> Bioresource Technology. 100 (23), 5537-5545 (2009).</li><li>Lei, X., Sugiura, N., Feng, C., Maekawa, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pretreatment+of+anaerobic+digestion+effluent+with+ammonia+stripping+and+biogas+purification.">Pretreatment of anaerobic digestion effluent with ammonia stripping and biogas purification.</a> Journal of Hazardous Materials. 145 (3), 391-397 (2007).</li><li>Siegrist, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nitrogen+removal+from+digester+supernatant-comparison+of+chemical+and+biological+methods.">Nitrogen removal from digester supernatant-comparison of chemical and biological methods.</a> Water Science and Technology. 34 (1), 399-406 (1996).</li><li>Desloover, J., Abate Woldeyohannis, A., Verstraete, W., Boon, N., Rabaey, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+Resource+Recovery+from+Digestate+to+Prevent+Ammonia+Toxicity+during+Anaerobic+Digestion.">Electrochemical Resource Recovery from Digestate to Prevent Ammonia Toxicity during Anaerobic Digestion.</a> Environmental Science &amp; Technology. 46 (21), 12209-12216 (2012).</li><li>Kim, J. R., Zuo, Y., Regan, J. M., Logan, B. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Analysis+of+ammonia+loss+mechanisms+in+microbial+fuel+cells+treating+animal+wastewater.">Analysis of ammonia loss mechanisms in microbial fuel cells treating animal wastewater.</a> Biotechnology and Bioengineering. 99 (5), 1120-1127 (2008).</li><li>Emerson, K., Russo, R. C., Lund, R. E., Thurston, R. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Aqueous+ammonia+equilibrium+calculations:+effect+of+pH+and+temperature.">Aqueous ammonia equilibrium calculations: effect of pH and temperature.</a> Journal of the Fisheries Board of Canada. 32 (12), 2379-2383 (1975).</li><li>Kuntke, P., Sleutels, T. H. J. A., Saakes, M., Buisman, C. J. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogen+production+and+ammonium+recovery+from+urine+by+a+Microbial+Electrolysis+Cell.">Hydrogen production and ammonium recovery from urine by a Microbial Electrolysis Cell.</a> International Journal of Hydrogen Energy. 39 (10), 4771-4778 (2014).</li><li>Guo, K., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surfactant+treatment+of+carbon+felt+enhances+anodic+microbial+electrocatalysis+in+bioelectrochemical+systems.">Surfactant treatment of carbon felt enhances anodic microbial electrocatalysis in bioelectrochemical systems.</a> Electrochemistry Communications. 39, 1-4 (2014).</li><li>Guo, K., Chen, X., Freguia, S., Donose, B. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spontaneous+modification+of+carbon+surface+with+neutral+red+from+its+diazonium+salts+for+bioelectrochemical+systems.">Spontaneous modification of carbon surface with neutral red from its diazonium salts for bioelectrochemical systems.</a> Biosensors and Bioelectronics. 47, 184-189 (2013).</li><li>Rice, E. W., Greenberg, A. E., Clesceri, L. S., Eaton, A. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Standard Methods For The Examination Of Water And Wastewater. , (1992).</li><li>Andersen, S. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrolytic+Membrane+Extraction+Enables+Production+of+Fine+Chemicals+from+Biorefinery+Sidestreams.">Electrolytic Membrane Extraction Enables Production of Fine Chemicals from Biorefinery Sidestreams.</a> Environmental Science &amp; Technology. 48 (12), 7135-7142 (2014).</li><li>Harnisch, F., Rabaey, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Diversity+of+Techniques+to+Study+Electrochemically+Active+Biofilms+Highlights+the+Need+for+Standardization.">The Diversity of Techniques to Study Electrochemically Active Biofilms Highlights the Need for Standardization.</a> Chemsuschem. 5 (6), 1027-1038 (2012).</li><li>Clauwaert, P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Minimizing+losses+in+bio-electrochemical+systems:+the+road+to+applications.">Minimizing losses in bio-electrochemical systems: the road to applications.</a> Applied Microbiology and Biotechnology. 79 (6), 901-913 (2008).</li><li>Atkins, P., De Paula, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Elements of Physical Chemistry. , (2012).</li><li>Aelterman, P., Freguia, S., Keller, J., Verstraete, W., Rabaey, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+anode+potential+regulates+bacterial+activity+in+microbial+fuel+cells.">The anode potential regulates bacterial activity in microbial fuel cells.</a> Applied Microbiology and Biotechnology. 78 (3), 409-418 (2008).</li><li>Kuntke, P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ammonium+recovery+and+energy+production+from+urine+by+a+microbial+fuel+cell.">Ammonium recovery and energy production from urine by a microbial fuel cell.</a> Water Research. 46 (8), 2627-2636 (2012).</li><li>Liu, H., Cheng, S., Logan, B. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Power+Generation+in+Fed-Batch+Microbial+Fuel+Cells+as+a+Function+of+Ionic+Strength.">Power Generation in Fed-Batch Microbial Fuel Cells as a Function of Ionic Strength.</a> Temperature, and Reactor Configuration. Environmental Science &amp; Technology. 39 (14), 5488-5493 (2005).</li><li>Gimkiewicz, C., Harnisch, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Waste+Water+Derived+Electroactive+Microbial+Biofilms:+Growth,+Maintenance,+and+Basic+Characterization.">Waste Water Derived Electroactive Microbial Biofilms: Growth, Maintenance, and Basic Characterization.</a> JoVE. (82), e50800 (2013).</li><li>Ping, Q., Cohen, B., Dosoretz, C., He, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Long-term+investigation+of+fouling+of+cation+and+anion+exchange+membranes+in+microbial+desalination+cells.">Long-term investigation of fouling of cation and anion exchange membranes in microbial desalination cells.</a> Desalination. 325, 48-55 (2013).</li><li>Guerin, T., Mondido, M., McClenn, B., Peasley, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Application+of+resazurin+for+estimating+abundance+of+contaminant-degrading+micro-organisms.">Application of resazurin for estimating abundance of contaminant-degrading micro-organisms.</a> Letters in Applied Microbiology. 32 (5), 340-345 (2001).</li></ol>

This manuscript provides the necessary tools to set up a bioelectrochemical and an electrochemical cell for ammonium recovery. The calculations presented in the results section provide the parameters for evaluation of the system performance. The biological and electrochemical systems are similar in setup and function. The main difference between the two systems is the choice of a fixed current for the electrochemical cell versus a fixed anode potential for the bioelectrochemical setup. The fixed current for the abiotic s...

Recovery of valuable products from wastewater gains importance as valuable resources become scarce and treatment without recovery represents only a cost. Wastewater contains both energy and nutrients that can be recovered, and nutrient recovery can help to close the production loop1. Recovery of energy through anaerobic digestion is a well-established process, while recovery of nutrients is less common. Recovery of nutrients from liquid waste streams such as urine and manure has been widely investigated, e.g., through the production of struvite and direct stripping of ammonia2,3. However, the need for chemical addition is a downside of these processes4. Here we present a technique for the recovery of cationic nutrients from waste streams, including both potassium and ammonium. The cationic form of these nutrients allows recovery using an ion selective membrane in an electrochemical system. In this case, the electrochemical system consists of an anode chamber (where oxidation takes place), a cathode chamber (where reduction takes place) and an ion selective membrane to separate the compartments. A voltage is applied across the cell to produce a current flow from anode to cathode. This voltage can be generated by an external power source to drive water oxidation and reduction reactions. Alternatively the anodic oxidation, e.g., of organics, can be catalyzed by electroactive bacteria, requiring less power. To close the circuit and maintain the charge balance, a charged species must migrate between the electrodes for each electron generated. Ammonium transport from the anode chamber to the cathode chamber across a cation exchange membrane (CEM) can thus compensate the flux of electrons 4,5.
The technique presented here not only removes ammonium from waste streams, but also enables its recovery. Total ammonia nitrogen (TAN) exists in equilibrium of both ammonium (NH4+) and ammonia (NH3), and is dependent on pH and temperature6. NH4+ is abundantly available due to high TAN concentration and near neutral pH in the anode chamber and this positively charged species can therefore be driven by the current across the CEM into the cathode chamber. The current drives the reduction of water at the cathode, leading to the production of hydroxide ions and hydrogen gas. The TAN equilibrium shifts to nearly 100% NH3 due to the high pH in the cathode chamber (&#62; 10.0). NH3 is a gas that can be easily transferred via air circulation from the stripping unit to the absorption column where it is trapped and concentrated in an acid solution.
This technology has the potential to decrease ammonium toxicity during anaerobic digestion of N-rich streams like manure, thus increasing the energy recovery from these waste streams, while simultaneously recovering nutrients4. Electrochemical and bioelectrochemical extraction of ammonium can also be applied as nutrient recovery technique on waste streams with a high TAN content such as urine thereby avoiding costs for nutrient removal at a WWTP7.
The protocol presented here can serve as a basis for many different electrochemical and bioelectrochemical experiments, as we use a modular reactor. Different electrode types, membranes and frame thicknesses can be combined as explained in the protocol below. The main aim of the protocol is to provide a means for the comparison of electrochemical ammonium recovery and bio-electrochemical ammonium recovery using an electrolysis cell. The systems are evaluated in terms of extraction efficiency, power input and reproducibility.

<table border="0" cellpadding="0" cellspacing="0" width="876">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Name of Material/ Equipment</td>
			<td style="width:192px;">Company</td>
			<td style="width:301px;">Catalog Number</td>
			<td style="width:167px;">Comments/Description</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Carbon Felt 3.18 mm Thick&#160;</td>
			<td style="width:192px;">Alfa Aesar</td>
			<td style="width:301px;">ALFA43199</td>
			<td>Used as bioanode, 110 mm x 110 mm</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Ti electrode coated with Ir MMO&#160;</td>
			<td style="width:192px;">Magneto Special Anodes (The Netherlands)</td>
			<td style="width:301px;"></td>
			<td>Used as stable anode for electrochemical tests</td>
		</tr>
		<tr height="73">
			<td height="73" style="height:74px;width:216px;">Stainless steel mesh</td>
			<td style="width:192px;">Solana (Belgium)</td>
			<td style="width:301px;">RVS 554/64: material AISI 316L, mesh width: 564 micron, wire thickness: 140 micron, mesh number: 36,6</td>
			<td>Used as cathode, 110 mm x 110 mm</td>
		</tr>
		<tr height="24">
			<td height="24" style="height:24px;width:216px;">Stainless steel plate</td>
			<td style="width:192px;">Solana (Belgium)</td>
			<td style="width:301px;">inox 304 sheet, thickness: 0,5mm</td>
			<td>Used as current collector for the bioanode</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Ag/AgCl Reference Electrode</td>
			<td style="width:192px;">Bio-Logic (France)</td>
			<td style="width:301px;">A-012167 RE-1B</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Potentiostat (VSP Multipotentiostat)&#160;</td>
			<td style="width:192px;">Bio-Logic (France)</td>
			<td style="width:301px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">EC Lab</td>
			<td style="width:192px;">Bio-Logic (France)</td>
			<td style="width:301px;"></td>
			<td>software for performing electrochemistry measurements</td>
		</tr>
		<tr height="44">
			<td height="44" style="height:44px;width:216px;">Cation Exchange Membrane</td>
			<td style="width:192px;">Membranes International (USA)</td>
			<td style="width:301px;">Ultrex CMI-7000</td>
			<td>Pretreated according to the manufacturers&#39; instructions</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Turbulence Promotor mesh</td>
			<td style="width:192px;">ElectroCell Europe A/S (Tarm, Denmark)</td>
			<td style="width:301px;">EPC20432-PP-2</td>
			<td>spacer material, 110 mm x 110 mm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Connectors</td>
			<td style="width:192px;">Serto</td>
			<td style="width:301px;">1,281,161,120</td>
			<td>Other sizes possible, dependant on tubing type and size of holes in frames</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Strip and absorption column</td>
			<td style="width:192px;"></td>
			<td style="width:301px;"></td>
			<td>In house design</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Tubing</td>
			<td style="width:192px;">Masterflex</td>
			<td style="width:301px;">HV-06404-16</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Gas bag</td>
			<td style="width:192px;">Keika Ventures</td>
			<td style="width:301px;"></td>
			<td>Kynar gas bag with Roberts valve</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Rashig Rings</td>
			<td style="width:192px;">Glasatelier Saillart (Belgium)</td>
			<td style="width:301px;">Raschig rings 4 x 4 mm</td>
			<td>Put inside the strip and absorption column to improve the air/liquid contact. Available with many suppliers</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Rubber sheet</td>
			<td style="width:192px;"></td>
			<td style="width:301px;"></td>
			<td>Cut to fit on the perspex frames</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Perspex reactor frames</td>
			<td style="width:192px;">Vlaeminck, Beernem</td>
			<td style="width:301px;"></td>
			<td>In-house design, see tab &#34;reactor frames&#34; in this file</td>
		</tr>
	</tbody>
</table>

electrochemically and bioelectrochemically induced ammonium recovery

Streams such as urine and manure can contain high levels of ammonium, which could be recovered for reuse in agriculture or chemistry. The extraction of ammonium from an ammonium-rich stream is demonstrated using an electrochemical and a bioelectrochemical system. Both systems are controlled by a potentiostat to either fix the current (for the electrochemical cell) or fix the potential of the working electrode (for the bioelectrochemical cell). In the bioelectrochemical cell, electroactive bacteria catalyze the anodic reaction, whereas in the electrochemical cell the potentiostat applies a higher voltage to produce a current. The current and consequent restoration of the charge balance across the cell allow the transport of cations, such as ammonium, across a cation exchange membrane from the anolyte to the catholyte. The high pH of the catholyte leads to formation of ammonia, which can be stripped from the medium and captured in an acid solution, thus enabling the recovery of a valuable nutrient. The flux of ammonium across the membrane is characterized at different anolyte ammonium concentrations and currents for both the abiotic and biotic reactor systems. Both systems are compared based on current and removal efficiencies for ammonium, as well as the energy input required to drive ammonium transfer across the cation exchange membrane. Finally, a comparative analysis considering key aspects such as reliability, electrode cost, and rate is made.
This video article and protocol provide the necessary information to conduct electrochemical and bioelectrochemical ammonia recovery experiments. The reactor setup for the two cases is explained, as well as the reactor operation. We elaborate on data analysis for both reactor types and on the advantages and disadvantages of bioelectrochemical and electrochemical systems.

Chronoamperometry results from the bioreactor
The chronoamperometry results, calculated according to Equation 1, show a typical graph for a continuous reactor (Figure 4). At the start of the experiment, the anode and cathode were operated in recirculation mode. This allows a biofilm to develop and the onset of the current production. After 5 days of operation, the current density reached a maximum, followed by a decrease in current production. This is an indic...

Watch this Scientific Journal Video about Electrochemically and Bioelectrochemically Induced Ammonium Recovery at JoVE.com

Electrochemically and Bioelectrochemically Induced Ammonium Recovery

We demonstrate the extraction of ammonium from an ammonium-rich stream using an electrochemical and a bioelectrochemical system. The reactor setup, operation and data analysis are discussed.

Streams such as urine and manure can contain high levels of ammonium, which could be recovered for reuse in agriculture or chemistry. The extraction of ...

electrochemically-and-bioelectrochemically-induced-ammonium-recovery

Research

Education

JoVE Journal

JoVE Core

Chemistry

Chemical Equilibrium

SCIENTISTS IN ACTION

12.6K vistas.  Ghent University. We demonstrate the extraction of ammonium from an ammonium-rich stream using an electrochemical and a bioelectrochemical system. The reactor setup, operation and data analysis are discussed. 