Renewable Copper and Silver Amalgam Film Electrodes of Prolonged Application for the Determination of Elemental Sulfur Using Stripping Voltammetry

Abstract

New, renewable copper (Hg(Cu)FE) and silver (Hg(Ag)FE) based amalgam film electrodes applied for the determination of elemental sulfur using differential pulse cathodic stripping voltammetry are presented. With surface areas adjustable from 1 to 12 mm 2 , both electrodes are characterized by very good surface reproducibility ( 2%) and long-term stability (a few thousand measurement cycles). The mechanical refreshing of the amalgam film takes about 1 -2 seconds. The effects of various factors such as instrumental parameters and the supporting electrolyte composition were optimized. Interferences from sulfides are easily removed by the addition of acid, and bubbling with argon, for Hg(Ag)FE. In the case of Hg(Cu)FE, sulfides did not interfere. The calibration graph is linear within the studied range from 16 ng L À1 to 4.8 mg L À1 for Hg(Cu)FE, and up to 6.4 mg L À1 for Hg(Ag)FE (t acc ¼ 15 s). The correlation coefficients for the two electrodes were at least 0.997. The detection limits for a low concentration of S(0) and t acc ¼ 60 s are as low as 14 ng L À1 for Hg(Cu)FE and 4 ng L À1 for Hg(Ag)FE. The proposed method was successfully applied and validated by studying the recovery of S(0) from spiked river water.

Renewable silver amalgam film electrodes in electrochemical stripping analysis—a review

“…An interesting example of the application of the Hg(Ag)FE-c was the elaboration of a protocol of the CSV quantification of elemental sulfur in water [47] and petrol or diesel fuel [48]. In the latter case, the DP-CSV determination of S(0) was performed in a mixture of methanol, ethanol, and H 2 SO 4 after a short preconcentration of the analyte at 0.150 V. The elaborated procedure allowed S(0) concentrations as low as 1.3 nM (0.04 μg l −1 ) to be determined for a preconcentration time of DPV differential pulse voltammetry, SWV square wave voltammetry, NPV normal pulse voltammetry, CC-SCP constant current stripping chronopotentiometry, DMG dimethylglyoxime, DTPA diethylenetriaminepentaacetic acid, MES morpholinoethanesulfonic a The lowest concentration of the linear range is missing.…”

Adsorptive Stripping Determination of Scandium(III) with Mordant Blue 9 on Silver Amalgam Film Electrode

“…The principle of working and first proposal of a construction of the (Hg(Ag)FE) was described in [10]. The (Hg(Ag)FE) electrode was successfully applied for the determination of Pb, Zn, Cd, Cu, Cr, Co, Ni, elemental S, Mn, Mo, Se, U, Pd, Ga [10][11][12][13][14][15][16][17][18][19][20].…”

Study on simultaneous measurements of trace gallium(III) and germanium(IV) by adsorptive stripping voltammetry using mercury film electrode

“…The principle of working and first proposal of a construction of the Hg(Ag)FE was described in [34]. Next, the construction of the electrode has been developed and described in [35]. The simple construction of the applied electrode allows the mercury film to be refreshed before each measurement.…”

“…The Hg(Ag)FE electrode was successfully applied for the determination of Pb, Zn, Cd, Cu, Cr, Co, Ni, elemental S, Mn, Mo, Se, U, Pd, Ga, Sc [34][35][36][37][38][39][40][41][42][43][44][45].…”