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Muthuraman, G.,Silambarasan, P.,Moon, I.S. Elsevier 2019 ELECTROCHIMICA ACTA Vol.295 No.-
<P><B>Abstract</B></P> <P>An ex-situ potentiometric titrations were normally performed using an oxidation/reduction potential (ORP) electrode to monitor the electrochemically generated active electron mediators, either oxidants or reductants, in a mediator generation plant. In the present investigation, an attempt was made to monitor electron mediator [Ni<SUP>1+</SUP>(CN)<SUB>4</SUB>]<SUP>3-</SUP> (Ni(I)) in-situ in a high electrolyte concentration (9 M KOH) during its electrochemical generation. A ring type flow cell developed using a 0.6 cm diameter electrode was tested on a standard redox couple of [Fe<SUP>3+</SUP>(CN)<SUB>6</SUB>]<SUP>3-</SUP> (Fe(III))/[Fe<SUP>2+</SUP>(CN)<SUB>6</SUB>]<SUP>4-</SUP> (Fe(II)) at different ratios during solution flow. The found results suggested that direct determination of an electrochemically prepared electron mediator is possible using a potentiometric method. A periodical potential change in the in-situ linear sweep voltammetry of electrogenerated Ni(I) during its electrochemical generation allowed the direct determination of electrogenerated Ni(I) by the ring type flow cell. A calibration plot derived from chemically synthesized Ni(I) using an ex-situ potentiometric titration or UV–visible spectra was used to monitor electrogenerated Ni(I) by the in-situ method. The electrochemically generated Ni(I) concentration detected in the 0–4.5 mmol/L region that followed non-Nernstian behavior. A change in the Ni(I) concentration during N<SUB>2</SUB>O removal at the scrubber column suggesting that air pollutant removal can be monitored using the in-situ flow sensor cell, once how many electron involved in the removal process.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Established a macro flow sensor for in-situ monitoring low valent metal ions during its electrogeneration. </LI> <LI> Periodical limiting peak potential change during electrolysis favors to sense Ni(I). </LI> <LI> A 0–5 mm Ni(I) range derived with a slope of non-Nernstian behavior. </LI> <LI> A defined Ni(I) concentration change when N<SUB>2</SUB>O removal correlates automation is possible by in-situ sensor. </LI> </UL> </P>
( Perumal Silambarasan ),( G. Muthuraman ),문일식 한국공업화학회 2019 한국공업화학회 연구논문 초록집 Vol.2019 No.0
Instead of off-line potentiometric titrations for electron mediator’s quantification, in-situ determination can be an accurate method. Here in, we have initiated to monitor the electrochemically prepared mediator [Co(I)(CN)<sub>5</sub>]<sup>4-</sup> by in-situ flow sensor cell coupled with paired electrolysis cell. First, cyclic voltammetry peak current for a standard redox couple Fe(II)/Fe(III) with different concentration ratios was used in the flow sensor cell to check the developed method. Then the Chemically prepared [Co(I)(CN)<sub>5</sub>]<sup>4-</sup> in presence of 10 M KOH at different concentrations were analyzed by UV-Visible and potentiometric titration method and compared. Finally, the chemically prepared different concentration of Co(I) do monitored using selected electrode under the inert atmosphere by flow sensor cell. The resulted calibration plot used to derive the concentration of [Co(I)(CN)<sub>5</sub>]<sup>4-</sup>.
( Perumal Silambarasan ),문일식 한국공업화학회 2019 한국공업화학회 연구논문 초록집 Vol.2019 No.0
To overcome the off-line potentiometric titrations for electron mediator’s quantification, in-situ determination has been attempted. Here in, we have initiated to monitor the electrochemically prepared mediator [Co(I)(CN)5]4- by in-situ flow sensor cell coupled with paired electrolysis cell. First, cyclic voltammetry peak current for a standard redox couple Fe(II)/Fe(III) with different concentration ratios was used in the flow sensor cell to check the developed method. Then the Chemically prepared [Co(I)(CN)5]4- in presence of 10 M KOH at different concentrations were analyzed by UV-Visible and potentiometric titration method and compared. Finally, the chemically prepared different concentration of Co(I) do monitored using selected electrode under the inert atmosphere by flow sensor cell. The concentration of [Co(I)(CN)5]4- was derived from the calibration plot.
( Perumal Silambarasan ),( G. Muthuraman ),문일식 한국공업화학회 2018 한국공업화학회 연구논문 초록집 Vol.2018 No.0
In-situ macro electrochemical sensors at high concentrated electrolyte is still at initla stage. The present work aims to develop a suitable electrode to monitor electrogenerated [Co(I)(CN)<sub>5</sub>]<sup>4-</sup> in 10 M KOH solution using a in-situ flow sensor cell. First, suitable potential window for each electrode was derived using cyclic voltammetry under flow condition (solution slow rate between 0.5 to 3.0 L/min). Then suitable scan rate under the flow condition was identified using the selected electrode (Pt, carbon, Cu, Ag). The current at limiting current region or optimum peak region was selected for electrogenerated [Co(I)(CN)<sub>5</sub>]<sup>4-</sup> in 10 M KOH solution at suitable electrode. The electrochemically generated Co(I)(CN)5]4- by using potentiometric titration at different electrolysis time was used to make calibration plot that was used to correlate with current value measure using suitable electrode at different electrolysis time.
( Perumal Silambarasan ),( Govindan Muthuraman ),문일식 한국공업화학회 2019 한국공업화학회 연구논문 초록집 Vol.2019 No.1
Very recently, an in-situ determination of electron mediators’ quantification was developed by potentiometric sensor method. Here in, a rationalization of potentiometric sensor by RDE (rotating disc electrode) and flow cell methods were optimized. First, electrochemical generation of [Co(I)(CN)5]4- in 10 M KOH solution was done by Nafion324 membrane divided electrochemical cell. The electrogenerated solution monitored by current and potential using RDE and flow cell with different RPM (rotation per minute) and flow rate by cyclic voltammetry (CV) method. By comparing the peak potential and peak current change, validation of a suitable method was derived for potentiometric sensor in determination of electrogenerated electron mediator in solution.
( Perumal Silambarasan ),( G. Muthuraman ),문일식 한국공업화학회 2019 한국공업화학회 연구논문 초록집 Vol.2019 No.1
Our recent publication unfolded an in-line determination of homogeneous electron mediator but, validation by a standard hydrodynamic method is still deserved. In the present investigation, a comparative analysis by RDE (rotating disc electrode) and flow cell methods were optimized in development of on-line potentiometric sensor for homogeneous electron mediator generation. First, [Co(I)(CN)<sub>5</sub>]<sup>4-</sup> (Co(I)) was electrochemically generated in 10 M KOH solution by Nafion324 membrane divided electrochemical cell. The electrogenerated solution monitored by current and potential using RDE and flow cell with different RPM (rotation per minute) and flow rate by cyclic voltammetry (CV) method. By comparing the peak potential and peak current change, validation of a suitable method was derived for potentiometric sensor in determination of homogeneous electrogenerated electron mediator.
( Perumal Silambarasan ),( G. Muthuraman ),문일식 한국공업화학회 2019 한국공업화학회 연구논문 초록집 Vol.2019 No.0
Instead of only electrolyte in one half-cell in detection gas sensors, addition of mediator precursor can be an added advantageous to reduce the over potential. In the present investigation, 0.1 M CoSO<sub>4</sub> in 5 M H<sub>2</sub>SO<sub>4</sub> or 0.05 M [Ni(CN)<sub>4</sub>]<sup>2-</sup> in 10 M KOH as electrolyte in one half-cell were used with Ag-Ni or Ag-Co metal ions coated Nafion324 membrane electrode divided cell for detection of air pollutants. Based on the cyclic voltammetry and linear sweep voltammetry analyses with and without CoSO<sub>4</sub> and [Ni(CN)<sub>4</sub>]<sup>2-</sup>, the gas phase redox peak was fixed for detection of selected gas pollutants. Then sense a selected air pollutants by amperometric method at different suitable applied voltage. The current with different feed concentration were compared with in-situ FTIR gas analyzer concentration and derived calibration plot.
( Perumal Silambarasan ),( G. Muthuraman ),문일식 한국공업화학회 2018 한국공업화학회 연구논문 초록집 Vol.2018 No.0
Besides electrochemical sensor development for neutral and less sup-porting electrolyte concentrations, an electrochemical sensors for high concentrated supporting electrolyte medium is worth to discover due to unavailability. Here in, we have initiated to monitor the electroche-mically prepared mediator [N(I)(CN)<sub>4</sub>]<sup>3-</sup> by in-situ flow sensor cell coupled with paired electrolysis cell. First, cyclic voltammetry peak current for a standard redox couple Fe(II)/Fe(III) with different concen-tration ratios was used in the flow sensor cell to check the developed method. Then the Chemically prepared [Ni(I)(CN)<sub>4</sub>]<sup>3-</sup> in presence of 10 M KOH at different concentrations were analyzed by UV-Visible and potentiometric titration method and compared. Finally, the chemically prepared different concentration of NI(I) do monitored using selected electrode under the inert atmosphere by flow sensor cell. The resulted calibration plot used to derive the concentration of [Ni(I)(CN)<sub>4</sub>]<sup>3-</sup>.
( Perumal Silambarasan ),( G. Muthuraman ),문일식 한국공업화학회 2019 한국공업화학회 연구논문 초록집 Vol.2019 No.0
In the present investigation, Ag and Ag-Ni or Ag-Co metal ions coated Nafioni324 membrane electrode divided cell was developed and compared in amperometric detection of air pollutants. Ag and Ag-Ni or Ag-Co were chemically coated on the Nafion324 membrane and used in filter press technique to make a cell with one side having 0.1 M KOH electrolyte and gas phase cathodic half-cell. Based on the cyclic voltammetry and linear sweep voltammetry analyses, the gas phase redox peak was fixed for detection of selected gas pollutants. Then sense a selected air pollutants by amperometric method at different suitable applied voltage. The current with different feed concentration were compared with in-situ FTIR gas analyzer concentration and derived calibration plot.