Deposition of trace metals on solid electrodes:  experimental verification of limits of electrochemical preconcentration

Ciszewski, Aleksander; Fish, Judith R.; Maliński, Tadeusz; Sioda, Roman E.

doi:10.1021/ac00183a015

Cited by 23 publications

(7 citation statements)

References 28 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The deviations might be due to the higher impact of measurement errors on accurate determination of small stripping peak heights and continuous nebulization signals or simply due to instrumental drift (no internal standard used). However, it has been shown by theory and actual measurements that below a certain species-dependent concentration level, the rates for electrodeposition and redissolution begin to compete. ,, If this happens, a decrease in % DE will be observed. Our previous ASV-ICP-MS work with Tl showed no indication that % DE decreased with decreasing analyte concentration, at least down to a few hundred picograms per liter.…”

Section: Resultsmentioning

confidence: 99%

Anodic Stripping Voltammetry Coupled On-Line with Inductively Coupled Plasma Mass Spectrometry: Optimization of a Thin-Layer Flow Cell System for Analyte Signal Enhancement

1997

View full text Add to dashboard Cite

Parameters affecting analyte signal enhancement in anodic stripping voltammetry-inductively coupled plasma mass spectrometry (ASV-ICP-MS), using a thin-layer ASV cell and microconcentric nebulization (MCN), have been examined. Silver was used as a test analyte and was deposited at a glassy carbon working electrode. The MCN allowed use of solution flow rates that were beneficial to optimum electrolytic performance of the thin-layer cell. High analyte deposition efficiencies obtained with the thin-layer cell, combined with minimal sample consumption of the MCN, allowed substantial signal enhancement (>400 times higher than continuous nebulization level) to be obtained with 2-3 mL of sample and deposition times of less than 30 min. Signal enhancement was strongly influenced by the opposing effect of flow rate on the electrolytic deposition efficiency (deposition efficiency decreases with increasing flow rate) and on the quantity of analyte delivered to the cell (analyte mass throughput increases with increasing flow rate). Excellent linearity for stripping peak heights was demonstrated for a wide range of analyte deposition times and for peak heights and peak areas (r > 0.999) over a wide concentration range (25 ng/L-20 μg/L). Precision was good (RSD typically <3% for n = 3-6) except for a high Ag blank contributed to by corrosion of the counter electrode and by Ag diffusion from the reference electrode into the cell. Details of the flow manifold and ASV cells are discussed, along with relevant performance characteristics of the MCN.

show abstract

Section: Resultsmentioning

confidence: 99%

Anodic Stripping Voltammetry Coupled On-Line with Inductively Coupled Plasma Mass Spectrometry: Optimization of a Thin-Layer Flow Cell System for Analyte Signal Enhancement

1997

View full text Add to dashboard Cite

show abstract

“…The electrode was then mounted onto the rotating shaft and cleaned by spinning it for 5 min in 1:1 HN03 to strip off any trace impurities. The electrochemical cell containing 40.0 mL of seawater sample and 4 mL of pH 4.6 acetate buffer was mounted and the sample bubbled for 20 min with nitrogen gas before the potential was applied so as to reduce the extent of oxidative dissolution of the deposit by dissolved oxygen (21). The electrolysis was allowed to proceed with simultaneous nitrogen bubbling for the times specified in Table I.…”

Section: Methodsmentioning

confidence: 99%

“…However, the difficulty of quantitative calibration has plagued this technique because the deposition is not quantitative for all elements at a given potential and the fraction deposited for a given element is not always reproducible between analyses at different concentrations (9). It has also been shown that the electrolytic preconcentration ratio frequently decreases as sample concentration decreases, due to oxidation by solution constituents (20,21). EDXRF and ICP-MS, with their multielement capability, are amenable to the use of an internal standard to solve these problems.…”

Section: Introductionmentioning

confidence: 99%

Multielement trace metal determination by electrodeposition, scanning electron microscopic x-ray fluorescence, and inductively coupled plasma-mass spectrometry

Chong¹,

Norton²,

Anderson³

1990

Anal. Chem.

View full text Add to dashboard Cite

Multielement analysis of multicomponent metallic electrodeposits Is described, based on scanning electron microscopy with energy dispersive X-ray fluorescence [EDXRF] detection, followed by dissolution and Inductively coupled plasma mass spectrometry [ICP-MS] detection. Application of the method Is described for determination of trace elements in seawater, including Zn, Mn, Co, Cu, Cr, Ni, Fe, Cd, Pb, and Hg. These elements are simultaneously electrodeposKed onto a niobium wire working electrode at -1.40 V vs an Ag/AgCI reference and subjected to EDXRF analysis. Internal standardization is practical for quantitative calibration at the 1 ppm analyte concentration level In an analyte:internal standard concentration ratio range of 0.02-50. Detection limits for EDXRF range from 1.9 ppb for Fe to 50 ppb for Cd. The deposit is dissolved for subsequent ICP-MS determination. Significant reduction in ICP-MS matrix interferences by Na, Ca, Mg, K, and Cl ions is achieved by deposition at potentials more positive than their very negative reduction potentials. Measurement of elemental isotope ratios is achieved with 0-8 % relative error. ICP-MS detection limits for all elements except Zn and Fe are superior to those of EDXRF. Mn, Ni, Cd, Pb, and Hg can easily be determined in the range of 13-86 parts per trillion with ICP-MS.

show abstract

“…Currently, many techniques are used for separation and preconcentration of trace elements, including liquid‐liquid ( Iberhan and Wisniewski, 2003 ; Mcleod et al, 1981 ) and solid‐phase ( Alexandrova and Arpadjan, 1995 ; Anthemidis and Martavaltzoglou, 2006 ; Impellitteri, 2004 ) extractions, co‐precipitation ( Hiraide et al, 1995 ; Sun and Yang, 1999 ; Zhang et al, 2004 ), and electrochemical deposition ( Ciszewski et al, 1989 ; Dai and Compton, 2006 ). Among them, solid‐phase extraction has found an increasing application because of its higher preconcentration factor, simple procedure, and combination with different analytical techniques, such as AAS and ICP‐AES.…”

Section: Introductionmentioning

confidence: 99%

Preconcentration of Trace Arsenite and Arsenate with Titanium Dioxide Nanoparticles and Subsequent Determination by Silver Diethyldithiocarbamate Spectrophotometric Method

Xiao¹,

Ling²,

Sun³

et al. 2007

Water Environment Research

View full text Add to dashboard Cite

A novel method of preconcentration of trace arsenite and arsenate by using titanium dioxide nanoparticles as adsorbent was described. The concentrations of preconcentrated arsenite and arsenate were determined by a silver diethyldithiocarbamate spectrophotometric method without desorption. Batch adsorption experiments were carried out as a function of the pH, contact time, amount of titanium dioxide nanoparticles, and solution volume. In the pH range 5 to 6, adsorption rates of arsenite and arsenate were higher than 98%. The calibration coefficient was 0.9991, and the linear range was 0 to 100 μg/L. The developed method was precise, with the relative standard deviation <5% at concentration level of 10 μg/L, with a detection limit (3σ, n = 6) of 0.44 μg/L. The accuracy of the method for total arsenic was validated by standard reference materials (SRM 3103a) (National Institute of Standards and Technology, Gaithersburg, Maryland). The method was also applied to the analysis of arsenite and arsenate in natural water samples to verify the accuracy. The recovery values remained in a narrow range, from 95 to 103%.

show abstract

Deposition of trace metals on solid electrodes: experimental verification of limits of electrochemical preconcentration

Cited by 23 publications

References 28 publications

Anodic Stripping Voltammetry Coupled On-Line with Inductively Coupled Plasma Mass Spectrometry: Optimization of a Thin-Layer Flow Cell System for Analyte Signal Enhancement

Anodic Stripping Voltammetry Coupled On-Line with Inductively Coupled Plasma Mass Spectrometry: Optimization of a Thin-Layer Flow Cell System for Analyte Signal Enhancement

Multielement trace metal determination by electrodeposition, scanning electron microscopic x-ray fluorescence, and inductively coupled plasma-mass spectrometry

Preconcentration of Trace Arsenite and Arsenate with Titanium Dioxide Nanoparticles and Subsequent Determination by Silver Diethyldithiocarbamate Spectrophotometric Method

Contact Info

Product

Resources

About