Understanding Electrochemically Activated Persulfate and Its Application to Ciprofloxacin Abatement

  • Laura W. Matzek
    Laura W. Matzek
    Department of Civil and Environmental Engineering, University of Tennessee, 325 John D. Tickle Building, Knoxville, Tennessee 37996-2313, United States
  • Matthew J. Tipton
    Matthew J. Tipton
    Department of Civil and Environmental Engineering, University of Tennessee, 325 John D. Tickle Building, Knoxville, Tennessee 37996-2313, United States
  • Abigail T. Farmer
    Abigail T. Farmer
    Department of Chemistry, University of Tennessee, 552 Buehler Hall, Knoxville, Tennessee 37996-1600, United States
  • Andrew D. Steen
    Andrew D. Steen
    Department of Earth and Planetary Sciences, University of Tennessee, 602 Strong Hall, Knoxville, Tennessee 37996-1526, United States
  • , and 
  • Kimberly E. Carter*
    Kimberly E. Carter
    Department of Civil and Environmental Engineering, University of Tennessee, 325 John D. Tickle Building, Knoxville, Tennessee 37996-2313, United States
    *Kimberly E. Carter, Phone: (865) 974-7731; Email: [email protected]
Cite this: Environ. Sci. Technol. 2018, 52, 10, 5875–5883
Publication Date (Web):April 13, 2018
https://doi.org/10.1021/acs.est.8b00015
Copyright © 2018 American Chemical Society
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Abstract

This study offers insight into the roles anodic and cathodic processes play in electrochemically activated persulfate (EAP) and screens EAP as a viable technique for ciprofloxacin degradation in wastewater. Sulfate radical formation at a boron-doped diamond (BDD) anode and persulfate activation at a graphite cathode were experimentally elucidated using different electrolytes and electrochemical setups. Rapid ciprofloxacin transformation occurred via pseudo-first-order mechanisms with respect to ciprofloxacin in persulfate electrolyte, reaching 84% removal in 120 min using EAP. Transformation pathways were compared to those in nitrate and sulfate electrolytes. Ciprofloxacin removal rates in the electrochemical system were 88% and 33% faster in persulfate than nitrate and sulfate electrolytes, respectively. Total organic carbon removal rates were 93% and 48% faster in persulfate than nitrate and sulfate, respectively. Use of sulfate electrolyte resulted in removal rates 6–7 times faster than those in nitrate solution. Accelerated removal in sulfate was attributed to anodic sulfate radical formation, while enhanced removal in persulfate was associated with cathodic persulfate activation and nonradical persulfate activation at the BDD anode. Quenching experiments indicated both sulfate radicals and hydroxyl radicals contributed to degradation. Comparisons between platinum and graphite cathodes showed similar cathodic persulfate activation and ciprofloxacin degradation.

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The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.est.8b00015.

  • Single-cell reactor with rotating disk electrode (RDE) (Schematic S1b); split-cell reactor with rotating disk electrode (RDE) (Method S1); LC-MS method for ciprofloxacin byproduct detection (eq S1); normalization of reaction time based on reactor volumes (eq S2); electrochemical hydrogen peroxide evolution (eq S3); energy consumption per unit mass TOC (eq S4); second-order kinetic model (eq S5a–d); competition kinetics for ciprofloxacin in quenchers (eq S6); mass-transfer coefficient (Table S1); HPLC multistep gradient program (Table S2a); effects of cathodes on removal rates of ciprofloxacin (Table S2b); effects of cathodes on removal rates of TOC (Table S3); reaction rate constants of quenching experiments (Table S4); mass-transfer coefficients of ciprofloxacin in electrolytes (Table S5); charge transfer coefficient, α Figure S1; pseudo-first-order kinetics for degradation of ciprofloxacin (Figure S2); initial stages of ciprofloxacin degradation (Figure S3); ciprofloxacin removal versus specific electrical charge (Figure S4); persulfate behavior during ciprofloxacin degradation (Figure S5); persulfate reduction to sulfate (Figure S6); second-order reaction modeling of ciprofloxacin and persulfate (Figure S7); quenching experiments (Figure S8); ciprofloxacin oxidation peak during cyclic voltammetry using a BDD anode (Figure S9); complete cyclic voltammetry of ciprofloxacin in nitrate, sulfate or persulfate using a BDD anode at different scan rates (Figure S10); multiple-cycle cyclic voltammetry of ciprofloxacin in nitrate, sulfate or persulfate using a BDD anode (Figure S11); modeling of C-V scans for Ciprofloxacin (Figure S12); complete cyclic voltammetry of ciprofloxacin in nitrate, sulfate and persulfate using Pt or Gr (Figure S13); reduction peak during cyclic voltammetry of cathode materials (Figure S14); ciprofloxacin transformation pathways (Figure S15); defluorination of 0.043 mmol L–1 ciprofloxacin with a BDD anode and graphite or platinum cathode (Figure S16); mass spectra for byproducts are shown for (a–h) nitrate, (i) sulfate, and (j–u) persulfate at various time points during the degradation of ciprofloxacin (Figure S17); ciprofloxacin transformation through hydroxyl radical attack for (a) multipoint hydroxylation, piperazine substitution and defluorination, (b) hydroxylation without defluorination, (c) hydroxylation without defluorination, (d) piperazaine-ring cleavage, (e) cyclo-propyl group breakdown, (f) amine loss, and (g) decarboxylation (PDF)

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