Determination of ultra-trace amounts of silver in water by differential pulse anodic stripping voltammetry using a new modified carbon paste electrode

Abstract

A highly sensitive and selective new procedure for the determination of silver in aqueous media was developed using a modified carbon paste electrode (MCPE) by differential pulse anodic stripping voltammetry (DPASV). The modified electrode was based on the incorporation of 2-hydroxybenzaldehyde benzoylhydrazone (2-HBBH) in the carbon paste electrode. Silver ions were preconcentrated on the modified electrode at open-circuit by complexation with the ligand and reduced to zero valent at a potential of 0V, and followed by the reoxidation of adsorbed ions onto the electrode by scanning the potential in a positive direction. The oxidation peak of Ag(I) was observed at 0.2V (versus Ag/AgCl). The analysis of Ag(I) was carried out in a cell containing the sample solution (20mL) buffered by 0.1molL(-1) K2HPO4/NaOH at pH 5.5 in aqueous solution and nitric acid (pH 1) in real water samples. The optimum conditions for the analysis of silver include a reduction potential of 0V and a pulse amplitude of 100mV, among others. The optimum carbon paste composition was found to be 14.1% (w/w) 2-HBBH, 56.2% (w/w) graphite powder and 29.7% (w/w) paraffin oil. Differential pulse anodic stripping voltammetric response was used as the analytical signal. Under the selected conditions, the voltammetric signal was proportional to the Ag(I) concentration in the range of 0.001-100μgL(-1) with favorable limits of detection and quantification of 1.1ngL(-1) and 3.7ngL(-1) after 3min of accumulation time, respectively. By increasing the accumulation time to 10min, detection and quantification limits can be further improved up to 0.1ngL(-1) and 0.34ngL(-1), respectively. In addition, the results showed a highly reproducible procedure showing a relative standard deviation of 1.5% for 12 replicate measurements. Many coexisting metal ions were investigated and very few interferences were found on the determination of Ag(I). The proposed method was validated using certified reference estuarine waters (SLEW-3) with a relative error of -1.3% and applied to the determination of silver ions in three river water samples collected from Guadalquivir river (relative errors of +3.4%, +1.5% and -0.7%). Moreover, the method was successfully applied to the speciation analysis of total silver, free silver ions and silver nanoparticles in aqueous solutions. The results were in good agreement with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).

Detection and Determination of Released Ions in the Presence of Nanoparticles: Selectivity or Strategy?

“…However, due to the lack of literature addressing this problem, it is difficult to establish a proper comparison. The results of the validation were in agreement with what has been published for methods determining silver in other systems (other working electrodes or modified electrodes) . In this work, Ag + was properly identified and the achievement of a single signal was possible.…”

Sensitive determination of trace Cd(ii) and Pb(ii) in soil by an improved stripping voltammetry method using two differentin situplated bismuth-film electrodes based on a novel electrochemical measurement system

“…6 . By increasing the accumulation time for the second deposition step to 350 s, the detection limit, dened as DL ¼ 3Sb/m, 54 where Sb is the standard deviation of the blank (n ¼ 5) and m is the slope of the calibration curve, was found to be 0.02 mg L…”

Construction of modified carbon paste electrode by a new pantazene ligand for ultra-trace determination of ion silver in real samples

“…Maximum contaminant level for total silver in drinking water, the US Environmental Protection Agency (EPA) fixed it as 0.1 mg/L -1 . It is also reported that the concentration of silver in water higher than 0.17 μg/L -1 is toxic to fish and microorganism [4,5]. The measurement and identification of ultra-trace levels in drinking water, water sources near factories and industries that released their waste into the rivers is very important [6].…”

“…The rapid methods involving bulk optode based on an ionophore [17], high sensitive and selective optical sensor [18], optical recognition [19] have used too. But electrochemical method is one of the most desirable methods for determination of silver because of its low cost, high sensitivity and simple preparation [5,20]. Cyclic voltammetry (CV), is very frequently used because it offers a wealth of experimental information and insights into both the kinetic and thermodynamic details of many chemical systems [21].…”