RESUMEN
A non-enzymatic direct electrochemical glycerol detection method at a commercial boron-doped diamond (BDD) electrode in 0.1 M NaOH supporting electrolyte was developed. All the used electrochemical techniques proved useful features for the oxidation and direct amperometric determination of glycerol at a BDD electrode in 0.1 M NaOH aqueous solution. It was found that the direct electrooxidation of glycerol on the BDD electrode requires both adsorbed glycerol and hydroxyls at the electrode surface. Also, the sp(2) carbon did not allow enhancement of the glycerol oxidation process. The electronalytical sensitivity for the determination of glycerol at the BDD electrode ranged from 0.040 to 0.226 µA mM(-1) as a function of the technique used. The highest electroanalytical sensitivity for the determination of glycerol at the BDD electrode was reached in batch system amperometric quantification under stirring conditions. Performed recovery studies indicated that it is possible to determine glycerol in real samples, and the proposed batch system analysis-based methodology can be a valuable tool for practical glycerol analysis.
Asunto(s)
Boro/química , Diamante , Electroquímica/métodos , Electrodos , Glicerol/análisisRESUMEN
Cyclic voltammetry (CV) and chronoamperometry (CA) have been used to sense and determine simultaneously L-ascorbic acid (AA) and acetaminophen (AC) at a boron-doped diamond electrode (BDDE) in a Britton-Robinson buffer solution. The calibration plots of anodic current peak versus concentration obtained from CV and CA data for both investigated compounds in single and di-component solutions over the concentration range 0.01 mM - 0.1 mM proved to be linear, with very good correlation parameters. Sensitivity values and RSD of 2-3% were obtained for various situations, involving both individual and simultaneous presence of AA and AC. The chronoamperometric technique associated with standard addition in sequential one step and/or two successive and continuous chronoamperograms at two characteristic potential levels represented a feasible option for the simultaneous determination of AA and AC in real sample systems such as pharmaceutical formulations. The average values indicated by the supplier were confirmed to a very close approximation from chronoamperomgrams by using several additions with the application of suitable current correction factors.
RESUMEN
TAA is a harmful, presumptive pollutant in tap waters and waste waters. Several alternatives have been tested as new possibilities for the anodic determination of TAA in aqueous solutions, simulated waste waters and tap water. The electrochemical behaviour of thioacetamide (TAA) was investigated at a boron-doped diamond (BDD) electrode both in unbuffered 0.1 M Na2SO4 and buffered solutions as supporting electrolytes. The anodic oxidation of TAA showed well-defined limiting currents or current peaks and a good linearity of the amperometric signal vs. concentration plots. The analytical parameters of sensitivity, RSD and LOD, obtained under various experimental conditions, suggest the suitability of the BDD electrode for electroanalytical purposes. Low fouling effects, good reproducibility and stability, as well as the sharpness of the amperometric signals in both unbuffered/ buffered acidic or neutral media, highly superior to those obtained using a glassy carbon (GC) electrode, recommend the unmodified BDD electrode as a promising potential amperometric sensor for environmental applications, regarding the direct anodic determination of TAA in aqueous media.
RESUMEN
In this paper, the electrochemical behaviour of several parabens preservatives, i.e. esters of p-hydroxybenzoic acid, methyl-, ethyl- and propyl-4-hydroxybenzoates as methyl-, ethyl- and propyl-parabens (MB, EB, and PB), has been investigated at a commercial boron-doped diamond electrode (BDDE), especially in the anodic potential range, in both hydro-alcoholic and aqueous media. The cyclic voltammetric and chronoamperometric measurements yielded calibration plots with very good linearity (R2 between 0.990 and 0.998) and high sensitivity, useful for detection and analytical applications. The determination of the characteristics of individual compounds, of an "overall paraben index", the assessment of the stability and the saturation solubility in water, and the amperometric sensing and determination in double distilled, tap and river water matrix of the relatively slightly soluble investigated parabens have been carried out using electrochemical alternative. Estimated water solubility was correlated with the octanol-water partition coefficient. Several ideas regarding stability and persistence of the presumptive eco-toxic investigated preservatives in the environment or water systems have been adjacently discussed.
RESUMEN
In this paper, a modified expanded graphite composite electrode based on natural zeolitic volcanic tuff modified with silver (EG-Ag-Z-Epoxy) was developed. Cyclic voltammetry measurements revealed a reasonably fast electron transfer and a good stability of the electrode in 0.1 M NaOH supporting electrolyte. This modified electrode exhibited moderate electrocatalytic effect towards urea oxidation, allowing its determination in aqueous solution. The linear dependence of the current versus urea concentration was reached using square-wave voltammetry in the concentrations range of urea between 0.2 to 1.4 mM, with a relatively low limit of detection of 0.05 mM. A moderate enhancement of electroanalytical sensitivity for the determination of urea at EG-Ag-Z-Epoxy electrode was reached by applying a chemical preconcentration step prior to voltammetric/amperometric quantification.
RESUMEN
Electrodes based on carbon, i.e., expanded graphite (20%, wt.)-epoxy composite(20EG-Epoxy) and expanded graphite (20%, wt.)-polystyrene composite (20EG-PS) havebeen prepared, characterized using scanning electron microscopy (SEM) and cyclicvoltammetry (CV), and tested as anodic sensors. The electrodes exhibited good mechanicalresistance and low electrical resistances. Scan rate dependent cyclic voltammetry responsesat 20EG-Epoxy and 20EG-PS composite electrodes, which were exemplified for thiourea(TU), a toxic sulphur organic compound selected as testing target analyte in 0.1 M Na2SO4 supporting electrolyte, were investigated. The obtained voltammetric data were inaccordance with those for a random array of microelectrodes. The voltammetric andchronoamperometric detection results of TU in tap water samples, without a supplementaryaddition of supporting electrolyte, at 20EG-Epoxy electrode proved its use for directanalysis of environmental samples.
RESUMEN
In this work a new electrochemical sensor based on an Ag-doped zeolite-expanded graphite-epoxy composite electrode (AgZEGE) was evaluated as a novel alternative for the simultaneous quantitative determination of nitrate and nitrite in aqueous solutions. Cyclic voltammetry was used to characterize the electrochemical behavior of the electrode in the presence of individual or mixtures of nitrate and nitrite anions in 0.1M Na(2)SO(4) supporting electrolyte. Linear dependences of current versus nitrate and nitrite concentrations were obtained for the concentration ranges of 1-10mM for nitrate and 0.1-1mM for nitrite using cyclic voltammetry (CV), chronoamperometry (CA), and multiple-pulsed amperometry (MPA) procedures. The comparative assessment of the electrochemical behavior of the individual anions and mixtures of anions on this modified electrode allowed determining the working conditions for the simultaneous detection of the nitrite and nitrate anions. Applying MPA allowed enhancement of the sensitivity for direct and indirect nitrate detection and also for nitrite detection. The proposed sensor was applied in tap water samples spiked with known nitrate and nitrite concentrations and the results were in agreement with those obtained by a comparative spectrophotometric method. This work demonstrates that using multiple-pulse amperometry with the Ag-doped zeolite-expanded graphite-epoxy composite electrode provides a real opportunity for the simultaneous detection of nitrite and nitrate in aqueous solutions.