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10 protocols using nafion 117 membrane

1

Synthesis of CNT-based Fuel Cell Catalyst

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Zirconium oxychloride hydrate (ZrOCl2 .8H2O), sodium hydroxide pellets (NaOH), hydrogen peroxide, methanol solution, sulphuric acid, carbon nanotubes (CNTs), nitric acid and Nafion® 117 membranes (EW = 1100, thickness 180) were purchased from Sigma. All the chemicals with analytical grade were used as received, without any further purification.
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2

Nafion 117 Membrane Preparation

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Nafion 117 membranes (equivalent weight EW = 1100 g eq.−1, thickness 180 μm) were supplied by Sigma-Aldrich. Dimethyl sulfoxide (DMSO) and all the other chemical reagents were Carlo Erba RP products.
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3

Synthesis of Polymer-Carbon Composites

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N,N-dimethylacetamide, ethylene glycol (EG), hydrogen hexachloroplatinate hexahydrate (H2PtCl6·6H2O), 2-propanol, methanol, sulfuric acid and nitric acid were purchased from Wako Pure Chemical, Ltd., and used as received. Nafion solution (5 wt%) and Nafion® 117 membrane were purchased from Sigma-Aldrich. Multi-walled carbon nanotubes (MWNTs; ca. 20-nm diameter) were kindly supplied from the Nikkiso Co. Carbon black (Vulcan XC-72R) was purchased from Cabot Chemical Co., Ltd. Poly[2,2’-(2,6-pyridine)-5,5′-bibenzimidazole] (PyPBI) (Fig. 1a) was synthesized according to a previously reported method40 . The MWNT/PyPBI, CB/PyPBI, CB/PyPBI/Pt and MWNT/PyPBI/Pt composites were prepared according to our previous reports12 14 .
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4

Two-Chamber Microbial Fuel Cell Design

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Two-chamber H-type BESs reactors were constructed by combining two 300-mL borosilicate glass bottles with 250-mL individual working volume (Duran, Germany) as anodic and cathodic chambers (Fig. S8). These were separated by a Nafion 117 membrane (Sigma-Aldrich, USA). Graphite plates sized 5 cm × 2.5 cm × 1 cm (Olmec, UK) were used as anode; these were soaked in 10% HCl overnight and rinsed with deionized water to remove the residuals on the surface. Platinum meshes sized 5 cm × 2.5 cm (Ti-shop, UK) were used as cathode after rinsing with deionized water. The electrodes were connected with a 1.0-mm-diameter stainless steel wire (Goodfellow, UK). The ohmic resistance of each electrode setup was tested with a voltammeter to ensure that the resistance was less than five ohms.
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5

Phosphoric Acid-Based Membrane Synthesis

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Materials used were phosphoric acid (Sigma), ammonium sulphate (Sigma), zirconium oxychloride hydrate (Merck), sulfuric acid (Merck), Nafion® 117 membrane (Sigma), methanol (Sigma), and hydrogen peroxide (Merck). All of the chemicals were used exactly as they were received, with no further purification.
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6

Electrochemical CO2 Reduction Catalyst Optimization

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All chemicals were obtained from commercial suppliers and used without further purification unless otherwise stated: glacial acetic acid (Fisher Chemical), 2-propanol (Honeywell), methanol (Fischer Scientific), absolute ethanol (VWR Chemicals), DL-dithiotreithol (DTT, BioXtra >99.5%, Sigma), 2-(N-morpholino)ethanesulfonate (MES) sodium salt (Bioreagent >99%, Sigma-Aldrich), MES acid monohydrate (BioXtra >99.5%, Sigma-Aldrich), sodium hydrogen carbonate (>99.998% trace metal basis, Puratronic), tris(hydroxymethyl)aminomethane hydrochloride (TRIS HCl, >99.0%, Sigma), potassium chloride (KCl, >99.999% trace metal basis, Fischer Scientific), potassium ferricyanide (>99.95%, Sigma Aldrich), InCl3 (>99.95%, Acros Organics), SnCl3.5H2O (>99.9%, Fisher Scientific), ethylene glycol (>99%, Sigma Aldrich), NaOH (>97%, Sigma Aldrich), formate solution (1 g L−1, Sigma Aldrich, ≥ 99.0%) and Carbonic Anhydrase from bovine erythrocytes (CA, Sigma Aldrich, EC 4.2.1.1, >95%, ≥3500 WA U mg−1). A Nafion® 117 Membrane (Sigma-Aldrich), Parafilm® M (Sigma-Aldrich), rubber septa (Subaseal), ITO-coated glass slides (Visiontek, 7 Ω sq−1) were used, ultrapure water was used for all electrode and electrolyte preparation (Simplicity UV MilliQ system, >18.2 MΩ cm). N2 (>99.998%) and CO2 (>99.8%) were supplied by BOC.
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7

Electrochemical Nitrogen Reduction in HCl

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All the electrochemical measurements (nitrogen reduction reaction and electrochemical characterization) were conducted in an H-cell (GaossUnion Photoelectric Technology Company). The counter electrode (graphite) was kept separated from the reference (4 M Ag/AgCl) and working electrode (GC mentioned above) via a Nafion 117 membrane (Sigma Aldrich). Before analysis, the membrane was pretreated by heating in H2O2 for 1 h, followed by in water for 1 h, both at 80 °C. All electrochemical and NRR measurements were conducted in Ar- or N2-saturated 0.1 M HCl aqueous solution. The potential was controlled using a Bio-Logic SP-300 potentiostat. The potentials against reference were converted to the reversible hydrogen electrode (RHE) using E (vs RHE) = E (vs Ag/AgCl) + 0.199 + 0.0591 × pH. The chronoamperometry tests were carried out at applied potentials ranging from − 0.15 V to − 0.55 V versus RHE.
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8

Electrochemical CO2 Reduction Catalyst Optimization

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All chemicals were obtained from commercial suppliers and used without further purification unless otherwise stated: glacial acetic acid (Fisher Chemical), 2-propanol (Honeywell), methanol (Fischer Scientific), absolute ethanol (VWR Chemicals), DL-dithiotreithol (DTT, BioXtra >99.5%, Sigma), 2-(N-morpholino)ethanesulfonate (MES) sodium salt (Bioreagent >99%, Sigma-Aldrich), MES acid monohydrate (BioXtra >99.5%, Sigma-Aldrich), sodium hydrogen carbonate (>99.998% trace metal basis, Puratronic), tris(hydroxymethyl)aminomethane hydrochloride (TRIS HCl, >99.0%, Sigma), potassium chloride (KCl, >99.999% trace metal basis, Fischer Scientific), potassium ferricyanide (>99.95%, Sigma Aldrich), InCl3 (>99.95%, Acros Organics), SnCl3.5H2O (>99.9%, Fisher Scientific), ethylene glycol (>99%, Sigma Aldrich), NaOH (>97%, Sigma Aldrich), formate solution (1 g L−1, Sigma Aldrich, ≥ 99.0%) and Carbonic Anhydrase from bovine erythrocytes (CA, Sigma Aldrich, EC 4.2.1.1, >95%, ≥3500 WA U mg−1). A Nafion® 117 Membrane (Sigma-Aldrich), Parafilm® M (Sigma-Aldrich), rubber septa (Subaseal), ITO-coated glass slides (Visiontek, 7 Ω sq−1) were used, ultrapure water was used for all electrode and electrolyte preparation (Simplicity UV MilliQ system, >18.2 MΩ cm). N2 (>99.998%) and CO2 (>99.8%) were supplied by BOC.
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9

Synthesis and Characterization of Metal-Polymer Composites

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Mo powder (Metco), B powder (Sigma-Aldrich, > 95%, < 1 µm), Al powder (Australian Metal Powders Supplies, > 99%, 45 µm), Nafion® perfluorinated resin solution (Sigma-Aldrich, 5 wt%), Nafion® 117 membrane, potassium hydroxide (Sigma-Aldrich, 90%), low-level ammonia pH adjusting ISA (Thermo SCIENTIFIC), ammonia standard solution (Thermo SCIENTIFIC), phenol (BDH Laboratory Supplies), ammonium sulfate (BDH Chemical, Australia Pty. Ltd.), ethanol (Merck KGaA), sodium nitroferricyanide (III) dehydrate (Sigma-Aldrich, > 99%), trisodium citrate dehydrate (Sigma-Aldrich), sodium hydroxide (Sigma-Aldrich), sodium hypochlorite solution (Sigma-Aldrich) and deionized water (Millipore, 18.2 MΩ cm) was used as the solvent, N2 gas (99.99%) and Ar gas (99.99%). All chemical regents were used as received without further purification.
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10

Phosphoric Acid Zirconium Membrane Fabrication

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Phosphoric acid (Sigma), Zirconium oxychloride hydrate (Merck), Sulfuric acid (Merck), Nafion® 117 membrane (Sigma), Methanol (sigma) and hydrogen peroxide (Merck) were used as received.
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