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Methods The room temperature CV measurements were performed in a 30mL polypropylene cylindrical container with a glassy carbon electrode (BASi, West Lafayette, IN), a platinum wire counter electrode (CH Instruments, Inc. Austin, TX), and a silver / silver chloride (Ag/AgCl) reference electrode (BASi, West Lafayette, IN). The temperature controlled CV measurements were performed in a 100mL water- jacketed glass cell (BASi, West Lafayette, IN) with a glassy carbon electrode, a platinum wire counter electrode residing in a counter electrode chamber, and a mercury / mercury oxide (MMO) reference electrode (CH Instruments, Inc. Austin, TX). Photographs of the two cells are shown in Figures S1a and S1b, respectively, in the SI. A refrigerated water circulator (VWR International, Radnor, PA) was connected to the water-jacketed cell to control the experiment temperature. In all CV measurements, the baseline CV curves of the supporting electrolyte were first collected. A stir bar in the cell was turned on after adding the active material, and turned off before the CV curves of the active material were collected. All CV measurements were performed on a Bio-Logic VSP potentiostat (Bio-Logic USA, Knoxville, TN). The starting chemicals sodium chlorate, sodium chlorite, sodium hypochlorite, sodium sulfate, and zinc chloride were purchased from Sigma-Aldrich (St. Louis, MO). Sodium chloride and sodium hydroxide were purchased from Alfa Aesar (Haverhill, MA). Potassium hydroxide was purchased from Brenntag (Essen, Germany). The proof of concept Zn-ClO2 cell was assembled as follows. The positive electrode and the positive current collector was a continuous piece of vitreous carbon foam 60 pores per inch (ppi) (McMaster Carr, Elmhurst, Illinois). The negative electrode was 2 pieces of zinc sheet, each of 24 mm x 13.5 mm x 0.2 mm, placed in close contact with a piece of nickel mesh which serves as the negative current collector. The cell housing material is acrylic, and EPDM gaskets were used. A set of 8 stainless steel screws, washers, and nuts, uniformly distributed around the perimeter of the exterior of the cell was used to clamp all cell parts together. The positive electrolyte was 1.5 mL of 2 molality (m) NaClO2 (which is 1.95 mol/L in molarity), with a theoretical capacity of 78 mAh. 6 mL of synthetic saturated hydrocarbon solvent with a similar range of carbon number to that of diesel fuel was added to the positive electrolyte. This solvent formed a segregated layer on top of the aqueous electrolyte due to its lower density and immiscibility. The negative electrolyte was a mixture of 1.5 mL of 2 m ZnCl2 and 1.5 mL of 2m NaCl, which upon mixing forms 3 mL of a mixture having 0.96 mol/L ZnCl2 and 0.98 mol/L NaCl. A silver/silver chloride (Ag/AgCl) wire pseudo reference electrode was placed in the negative electrolyte of the cell. The cell was designed to ensure the negative electrode and the reference electrode were not in contact with each other. A piece of sodiated Nafion 117 (Na-N117) was placed to separate the positive electrolyte and the negative electrolyte. The Na-N117 was prepared by soaking Nafion 117 (purchased from Fuel Cell Store, College Station, TX) in 2 m NaOH at room temperature for at least 1 week before use. The active area of the Na-N117 is 2 cm2 (2.5 cm x 0.8 cm). The Zn-ClO2 cell was cycled as follows. The cell was first cycled through shallow cycles of 5 mA (2.5 mA/cm2) charging for 1 min followed by 5 mA (2.5mA/cm2) discharging for 1 min, for a total of 10 cycles. The purpose of this conditioning step was to identify any cell assembly related issues. Subsequently, the cell was charged at a constant current of 5 mA/cm2 to a capacity of 10mAh following which it was discharged at 5 mA/cm2 to a lower voltage limit of 0.8V (full cell voltage). The full cell cycling experiments were performed in a temperature controlled incubator held at 0.5 +/- 0.5 °C. The full cell cycling experiments were performed on an Arbin battery cycler (Arbin Instruments, College Station, TX). 10PDF Image | Reversible Chlorite Chlorine Dioxide Anion Redox Storage
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