Eduardo Pinillla Gil

Publications

• 3.29

  Impact points

  Determination of trace and major elemental profiles in street dust samples by fast miniaturized ultrasonic probe extraction and ICP-MS.

  Ma Rosario Palomo Marín, Eduardo Pinilla Gil, Lorenzo Calvo Blázquez, José Luis Capelo-Martínez

  Talanta. 05/2011; 84(3):840-5.

  A simple, fast and miniaturized ultrasonic probe assisted protocol for acid extraction of trace and major elements from street dust samples, prior to final determination by ICP-MS, has been optimized and validated by standard reference materials and applied during an urban air quality monitoring cam... [more] A simple, fast and miniaturized ultrasonic probe assisted protocol for acid extraction of trace and major elements from street dust samples, prior to final determination by ICP-MS, has been optimized and validated by standard reference materials and applied during an urban air quality monitoring campaign. 15 mg samples were treated for 3 min with 1 mL concentrated HNO(3)-HCl (1:3, v/v) extracting solution, by a 1mm diameter titanium sonotrode connected to a 200 W and 24 kHz ultrasonic device at 80% amplitude. After centrifugation, the extracts were assayed by ICP-MS with good recoveries for the certified elements. Statistical analysis of real sample results by cluster analysis allowed the correct grouping of the samples according to the influence of traffic and construction/demolition activities. Correlation of street dust and PM10 elemental profiles showed the potential applicability of the proposed analytical protocol as a simple and effective way for urban air quality monitoring.
• 4.31

  Impact points

  Determination of mercury in ambient water samples by anodic stripping voltammetry on screen-printed gold electrodes.

  E Bernalte, C Marín Sánchez, E Pinilla Gil

  Analytica chimica acta. 03/2011; 689(1):60-4.

  The applicability of commercial screen-printed gold electrodes (SPGEs) for the determination of Hg(II) in ambient water samples by square wave anodic stripping voltammetry has been demonstrated. Electrode conditioning procedures, chemical and instrumental variables have been optimized to develop a r... [more] The applicability of commercial screen-printed gold electrodes (SPGEs) for the determination of Hg(II) in ambient water samples by square wave anodic stripping voltammetry has been demonstrated. Electrode conditioning procedures, chemical and instrumental variables have been optimized to develop a reliable method capable of measuring dissolved mercury in the low ng mL(-1) range (detection limit 1.1 ng mL(-1)), useful for pollution monitoring or screening purposes. The proposed method was tested with the NIST 1641d Mercury in Water Standard Reference Material (recoveries 90.0-110%) and the NCS ZC 76303 Mercury in Water Certified Reference Material (recoveries 82.5-90.6%). Waste water samples from industrial origin and fortified rain water samples were assayed for mercury by the proposed method and by a reference ICP-MS method, with good agreement. Screen printing technology thus opens a useful way for the construction of reliable electrochemical sensors for decentralized or even field Hg(II) testing.
• 3.14

  Impact points

  Impact of Santiago de Chile urban atmospheric pollution on anthropogenic trace elements enrichment in snow precipitation at Cerro Colorado, Central Andes

  F. Cereceda-Balic, M.R. Palomo-Marín, E. Bernalte, V. Vidal, J. Christie, X. Fadic, J.L. Guevara, C. Miro, E Pinilla Gil

  Atmospheric Environment. 01/2011;

  Seasonal snow precipitation in the Andes mountain range is evaluated as an environmental indicator of the composition of atmospheric emissions in Santiago de Chile metropolitan area, by measuring a set of representative trace elements in snow samples by ICP-MS. Three late winter sampling campaigns (... [more] Seasonal snow precipitation in the Andes mountain range is evaluated as an environmental indicator of the composition of atmospheric emissions in Santiago de Chile metropolitan area, by measuring a set of representative trace elements in snow samples by ICP-MS. Three late winter sampling campaigns (2003, 2008 and 2009) were conducted in three sampling areas around Cerro Colorado, a Central Andes mountain range sector NE of Santiago (36 km). Nevados de Chillán, a sector in The Andes located about 500 km south from the metropolitan area, was selected as a reference area. The experimental results at Cerro Colorado and Nevados de Chillán were compared with previously published data of fresh snow from remote and urban background sites. High snow concentrations of a range of anthropogenic marker elements were found at Cerro Colorado, probably derived from Santiago urban aerosol transport and deposition combined with the effect of mining and smelting activities in the area, whereas Nevados de Chillán levels roughly correspond to urban background areas. Enhanced concentrations in surface snow respect to deeper samples are discussed. Significant differences found between the 2003, 2008 and 2009 anthropogenic source markers profiles at Cerro Colorado sampling points were correlated with changes in emission sources at the city. The preliminary results obtained in this study, the first of this kind in the southern hemisphere, show promising use of snow precipitation in the Central Andes as a suitable matrix for receptor model studies aimed at identifying and quantifying pollution sources in Santiago de Chile.

• Determination of Lead in Ambient Aerosol Samples by Anodic Stripping Voltammetry on a Bismuth Film Electrode

  M.R. Palomo Marín, E. Pinilla Gil, L. Calvo Blázquez

  Electroanalysis. 01/2011; 23(1):215.

  Cd and Pb determination in ambient aerosol samples based on SWASV at a Bi film glassy carbon electrode is described. Extremely acid solutions resulting from sample digestion were directly assayed, with sufficient detection limits for testing the fulfilment of air quality regulations. Accuracy was te... [more] Cd and Pb determination in ambient aerosol samples based on SWASV at a Bi film glassy carbon electrode is described. Extremely acid solutions resulting from sample digestion were directly assayed, with sufficient detection limits for testing the fulfilment of air quality regulations. Accuracy was tested on NIST Standard Reference Materials and real aerosol samples, with good recoveries for Pb comparable to ICP-MS results. Cd was not detected, probably due to the combined effects of low Cd and high interfering Zn and Cu contents. The proposed method provides an attractive alternative to ICP-MS with potential applicability for decentralized analysis.

• Gold nanoparticles-modified screen-printed carbon electrodes for anodic stripping voltammetric determination of mercury in ambient water samples

  E. Bernalte, C. Marín Sánchez, E. Pinilla Gil

  Sensors and Actuators B. 01/2011;

  We present here a simple, fast and cheap procedure for the determination of Hg(II) by square wave anodic stripping voltammetry (SWASV) at a commercial gold nanoparticles-modified screen-printed carbon electrodes (AuNPs-SPCEs), as a tool for environmental waters monitoring. The advantages of electrod... [more] We present here a simple, fast and cheap procedure for the determination of Hg(II) by square wave anodic stripping voltammetry (SWASV) at a commercial gold nanoparticles-modified screen-printed carbon electrodes (AuNPs-SPCEs), as a tool for environmental waters monitoring. The advantages of electrode nanostructuration are exploited, e.g. no stirring for the deposition step is needed. The surface of the gold nanostructured screen-printed carbon electrodes was characterized using SEM, XPS and electrochemical methods. All experimental variables involved in the voltammetric stripping method were optimized to develop a reliable method capable of measuring dissolved mercury in the low ng/mL range. The proposed method was tested with the NIST 1641d Mercury in Water Standard Reference Material with good agreement. The applicability of the AuNPs-SPCEs for Hg(II) determination in real ambient water samples, namely rain water, river water and industrial waste water, without any sample pretreatment, was successfully demonstrated.
• 2.63

  Impact points

  Performance of a bismuth rotating disk electrode (BiRDE) for heavy metal analysis: Determination of lead in environmental samples

  María de la Gala Morales, Mª Rosario Palomo Marín, Lorenzo Calvo Blázquez, Eduardo Pinilla Gil

  Electroanalysis. 01/2011;

• Presence of plutonium isotopes, 239Pu and 240Pu, in soils from Chile

  E. Chamizo, M. García-León, J.I. Peruchena, F. Cereceda, V. Vidal, E. Pinilla, C. Miró

  Nuclear Instruments and Methods in Physics Research B. 01/2011; 269:3163.
• 3.29

  Impact points

  Modification of carbon screen-printed electrodes by adsorption of chemically synthesized Bi nanoparticles for the voltammetric stripping detection of Zn(II), Cd(II) and Pb(II).

  Ma Angeles Granado Rico, Mara Olivares-Marín, Eduardo Pinilla Gil

  Talanta. 12/2009; 80(2):631-5.

  A simple procedure for the chemical synthesis of bismuth nanoparticles and subsequent adsorption on commercial screen-printed carbon electrodes offer reliable quantitation of trace zinc, cadmium and lead by anodic stripping square-wave voltammetry in nondeareated water samples. The influence of two ... [more] A simple procedure for the chemical synthesis of bismuth nanoparticles and subsequent adsorption on commercial screen-printed carbon electrodes offer reliable quantitation of trace zinc, cadmium and lead by anodic stripping square-wave voltammetry in nondeareated water samples. The influence of two hydrodynamic configurations (convective cell and flow cell) and the effect of various experimental variables upon the stripping signals at the bismuth-coated sensor are explored. The square-wave peak current signal is linear over the low ng mL(-1) range (120 s deposition), with detections limits ranging from 0.9 to 4.9 ng mL(-1) and good precision. Applicability to waste water certified reference material and drinking water samples is demonstrated. The attractive behaviour of the new disposable Bi nanoparticles modified carbon strip electrodes, coupled with the negligible toxicity of bismuth, hold great promise for decentralized heavy metal testing in environmental and industrial effluents waters.

• A Novel Cell Design for the Improved Stripping Voltammetric Detection of Zn(II), Cd(II), and Pb(II) on Commercial Screen-Printed Strips by Bismuth Codeposition in Stirred Solutions

  M Angeles Granado Rico, Mara Olivares-Marin, Eduardo Pinilla Gil

  Electroanalysis. 12/2008; 20:2608.

  A novel electrochemical cell design is proposed to allow fast, reproducible and highly efficient convective transport of dissolved substances to screen-printed electrochemical three-electrode strips mounted on miniaturized plastic vessels, with the goal of improving detection limits in disposable el... [more] A novel electrochemical cell design is proposed to allow fast, reproducible and highly efficient convective transport of dissolved substances to screen-printed electrochemical three-electrode strips mounted on miniaturized plastic vessels, with the goal of improving detection limits in disposable electrochemical stripping field sensors. The experimental configuration has been tested for accumulation of the selected heavy metals ions Zn(II), Cd(II), and Pb(II), codeposited with bismuth ions on a carbon disk screen-printed working electrode before detection by square wave anodic stripping voltammetry. Chemical and instrumental variables of the proposed device and associate electrochemical method were optimized. Selected parameters gave detection limits in the low ng mL�1 range with moderate deposition time (120 s). Practical applicability was tested on certified water and real samples (tap water and waste water), with acceptable results, suggesting potential usefulness for field environmental monitoring of heavy metals.
• 3.29

  Impact points

  Optimization and validation of a capillary electrophoresis methodology for inorganic anions in atmospheric aerosol samples.

  Silvia Talaván García, Ma Isabel Acedo Valenzuela, Eduardo Pinilla Gil

  Talanta. 06/2008; 75(3):748-52.

  Optimization and validation of a method for the determination of inorganic anions, such as chloride, nitrate, sulphate, fluoride and phosphate, in atmospheric particulate matter is described. Ultrasonic extraction followed by CE, using CTAB as EOF modifier, has been established for this separation u... [more] Optimization and validation of a method for the determination of inorganic anions, such as chloride, nitrate, sulphate, fluoride and phosphate, in atmospheric particulate matter is described. Ultrasonic extraction followed by CE, using CTAB as EOF modifier, has been established for this separation using chromate as visualization reagent for the indirect UV/vis detection. Optimization of the experimental chemical conditions (pH, surfactant concentration, chromate concentration and acetonitrile concentration) and instrumental parameters (temperature, applied voltage and injection time) is described. Linear calibrations plots are obtained for the five ions, with detection limits in the high ng/mL range. A standard reference material, SRM 1648 Urban Particulate Matter, has been used to validate the proposed method. Satisfactory reproducibility and acceptable agreement to the matter atmospheric samples has been found (recoveries ranging from 86 to 96%). Application to real particulate matter atmospheric samples, collected on high volume samplers from the air quality surveillance network of Extremadura, southwest Spain, is shown.
• 3.14

  Impact points

  Spatial and temporal variations in airborne particulate matter (PM10 and PM2.5) across Spain 1999-2005

  X. Querol, A. Alastuey, T. Moreno, M.M. Viana, S. Castillo, J. Pey, S. Rodríguez, B. Artiñano, P. Salvador, S. Garcia Dos Santos, M.D. Herce Garraleta, R. Fernandez Patier, S. Moreno, M.C. Minguillón, E. Monfort, R. Palomo-Marín, E. Pinilla-Gil, E. Cueva

  Atmospheric Environment. 01/2008; 42:3964.
• 3.43

  Impact points

  Antimony distribution and mobility in topsoils and plants (Cytisus striatus, Cistus ladanifer and Dittrichia viscosa) from polluted Sb-mining areas in Extremadura (Spain).

  A Murciego Murciego, A. García Sánchez, M A Rodríguez González, E Pinilla Gil, C Toro Gordillo, J Cabezas Fernández, T Buyolo Triguero

  Environmental pollution (Barking, Essex : 1987). 02/2007; 145(1):15-21.

  A study about topsoil antimony distribution and mobility from the soils to the biomass has been afforded in three abandoned Sb mining areas located at Extremadura. Physico-chemical characteristics of the soils and total antimony levels were measured in soils and autochthonous plant species (Cytisus ... [more] A study about topsoil antimony distribution and mobility from the soils to the biomass has been afforded in three abandoned Sb mining areas located at Extremadura. Physico-chemical characteristics of the soils and total antimony levels were measured in soils and autochthonous plant species (Cytisus striatus, Cistus ladanifer and Dittrichia viscosa). Comparison with corresponding values in reference areas isolated from the mining activities is discussed. Antimony mobility in the soils was estimated by measuring the water extractable fraction; low results were obtained for the three soil areas, with no statistical differences. Plant ability to accumulate antimony was estimated by use of plant accumulation coefficients (PAC). Seasonal (spring vs. autumn) effects on the antimony content in the plant species. Cytisus striatus from Mari Rosa mine presented antimony excluder characteristics, whereas Dittrichia viscosa specimens growing in San Antonio mine showed a significant antimony bioaccumulation.

• Monitoring of Zn(II) and Cd(II) adsorption on activated carbon from aqueous multicomponent solutions by differential pulse polarography (DPP)

  R. Pardo-Botello, E. Pinilla-Gil, C. Fernandez-Gonzalez, V. Gomez Serrano

  International Journal of Environmental and Analytical Chemisstry. 06/2005; 85:1051.

  The adsorption process of Zn(II) and Cd(II) from aqueous solution has been investigated from both kinetic and equilibrium standpoints, using differential pulse polarography (DPP) on a mercury dropping electrode as the analytical technique. With such an aim, adsorption experiments were performed usin... [more] The adsorption process of Zn(II) and Cd(II) from aqueous solution has been investigated from both kinetic and equilibrium standpoints, using differential pulse polarography (DPP) on a mercury dropping electrode as the analytical technique. With such an aim, adsorption experiments were performed using not only a single metal ion–Zn(II) or Cd(II) solution but also a multi-component ion metal–Zn(II), Cd(II) and Hg(II) solution. The influence of the pH change in the multi-component ion metal solution on the adsorption of Zn(II) and Cd(II) was also studied. The adsorption processes is relatively fast for Zn(II) and Cd(II). The presence of two foreign ions in the solution slightly speeds up the adsorption process for Zn(II) and significantly slows it down for Cd(II). The adsorption isotherms are similarly shaped for Zn(II) and Cd(II). The addition of the foreign ions has a more unfavourable effect on the adsorption for Cd(II) than for Zn(II). At pH 2, neither Zn(II) nor Cd(II) is adsorbed practically on the carbon. The voltammetric approach has proved to be a fast and efficient method that, at the same time, enables one to monitor the adsorption of Zn(II) and Cd(II) with potential on-line application, which could be useful in waste-water treatment.
• 3.02

  Impact points

  Adsorption kinetics of zinc in multicomponent ionic systems.

  R Pardo-Botello, C Fernández-González, E Pinilla-Gil, E M Cuerda-Correa, V Gómez-Serrano

  Journal of colloid and interface science. 10/2004; 277(2):292-8.

  Using commercial activated carbon as an adsorbent, the kinetics of adsorption of zinc from multicomponent ionic systems having cadmium and mercury has been studied and reported. The variables investigated have been the chemical nature, ionic strength, and pH of the adsorptive (Zn2+) solution. The ad... [more] Using commercial activated carbon as an adsorbent, the kinetics of adsorption of zinc from multicomponent ionic systems having cadmium and mercury has been studied and reported. The variables investigated have been the chemical nature, ionic strength, and pH of the adsorptive (Zn2+) solution. The adsorption of Zn2+ is speeded up by the presence of Cd2+ and Hg2+ ions provided that the concentration of these two ions is high as compared to the concentration of Zn2+. When the ionic strength of the solution in relative terms is high (i.e., > 3 x 10(-4) M), however, the adsorption of Zn2+ decelerates. Also, the adsorption process is greatly accelerated at pH 12, whereas at pH 2 it does not occur at all.

• Potentiometric stripping analysis (PSA) for monitoring of antimony in samples of vegetation from a mining area.

  M C Toro Gordillo, E Pinilla Gil, M A Rodríguez González, A Murciego Murciego, P Ostapczuk

  Fresenius' journal of analytical chemistry. 07/2001; 370(4):434-7.

  A potentiometric stripping analysis (PSA) method has been developed and checked for the fast and reliable determination of antimony in vegetation samples of Cistus ladanifer from a mining area in Badajoz, Southwest Spain. The method, modified from previous PSA methods for Sb in environmental samples... [more] A potentiometric stripping analysis (PSA) method has been developed and checked for the fast and reliable determination of antimony in vegetation samples of Cistus ladanifer from a mining area in Badajoz, Southwest Spain. The method, modified from previous PSA methods for Sb in environmental samples, is based on dry ashing of the homogenized leaves, dissolution in hydrochloric acid, and PSA analysis on a mercury film plated on to a glassy carbon disk electrode. The influence of experimental variables such as the deposition potential, the deposition time, the signal stability and the calibration parameters, has been investigated. The method has been compared with an independent technique (instrumental neutron activation analysis) by analysis of standards and reference materials and comparison of the results. As a result of automation of the PSA equipment, the proposed method enables unattended analysis of 20 digested samples in a total time of 2 h, thus providing a useful tool for Sb monitoring of a large number of samples.

• Determination of arsenic species by field amplified injection capillary electrophoresis after modification of the sample solution with methanol

  E. Pinilla Gil, P. Ostapczuk, H. Emons

  Analytica Chimica Acta. 06/1999; 389:9.

  Organic solvent modi®cation is investigated as a simple and effective way to decrease the conductivity of liquid samples containing anionic As species, making them suitable for ®eld ampli®ed sample stacking capillary electrophoresis (CE) measurements with direct UV detection. Experimental variables ... [more] Organic solvent modi®cation is investigated as a simple and effective way to decrease the conductivity of liquid samples containing anionic As species, making them suitable for ®eld ampli®ed sample stacking capillary electrophoresis (CE) measurements with direct UV detection. Experimental variables that in¯uence the procedure, as buffer pH, stacking and running potential, are described for methanol, selected as the optimum sample modi®er. The in¯uence of modifying the CE buffer with methanol on the resolution is also discussed. Results of stacking with and without removing the sample matrix from the capillary (with and without polarity switching after the stacking stage) are reported. The optimized method permits the determination of As(III) (arsenite), free As(V) (arsenate), and dimethylarsinate (DMA), in the range from 0.5 to 20 mg/l, with detection limits around 0.3 mg/l. For other As(V) compound of human origin, phenylarsonate (PAA), and p-aminobenzenearsonate (PABA), the power of detection is higher due to their higher extinction coef®cients. The linear range extends from 20 to 1000 mg/l, with a detection limit of 11 mg/l (PAA) and 16 mg/l (PABA). # 1999 Elsevier Science B.V. All rights reserved.

• Evaluation of the influence of physical activity on the plasma concentrations of several trace metals.

  I Rodríguez Tuya, E Pinilla Gil, M Maynar Mariño, R M García-Moncó Carra, A Sánchez Misiego

  European journal of applied physiology and occupational physiology. 01/1996; 73(3-4):299-303.

  Our study was carried out with the aim of evaluating the influence that the degree of physical activity may have on plasma concentrations of essential and toxic elements. Copper and zinc, elements of known importance in basic cellular processes, have been analysed as essential, and cadmium and lead ... [more] Our study was carried out with the aim of evaluating the influence that the degree of physical activity may have on plasma concentrations of essential and toxic elements. Copper and zinc, elements of known importance in basic cellular processes, have been analysed as essential, and cadmium and lead as toxic for the body in abnormal doses. The study was performed on a total population of 50 healthy individuals, 34 of them professional sportsmen and the rest who undertook moderate physical activity (control group), all of them living in a polluted environment (Madrid, Spain). Sampling was conducted at the beginning of the season (October). Electro-analytical techniques of proved reliability and accuracy were used for the determination of the metals. The results were related to data obtained using graphite furnace atomic absorption spectrophotometry and by use of biological reference materials. We found significantly higher zinc plasma concentrations in the sportsmen involved in anaerobic-type training (judo, fencing) compared to those undertaking aerobic activities (endurance, cycling) (P < 0.05). The values in both cases were higher than those found in the control group. Our study showed an increase of plasma copper concentrations in professional sportsmen, especially in those performing anaerobic activities, compared to those subjects undertaking moderate activity (control group) (P < 0.05). In summary, our results showed that there were no deficiencies of copper and zinc in the athletes studied at the beginning of the season. The levels were higher than those of the control population. As for the toxic metals, cadmium and lead, we observed lower levels in the athletes than in the control group (cadmium P < 0.005, lead P < 0.05). These results may indicate the existence of possible elimination systems for these metals in athletes, when they are training in a polluted environment.
• 4.31

  Impact points

  Potentiometric stripping determination of mercury(II), selenium(IV), copper(II) and lead(II) at a gold film electrode in water samples

  E. Pinilla Gil, P. Ostapczuk

  Analytica Chimica Acta. 01/1995; 293:55.
• 4.31

  Impact points

  Determination of copper in human plasma by stripping potentiometry on a mercury film electrode in ethylenediamine medium

  E. Pinilla Gil, R.M. García-Moncó Carra, A. Sánchez Misiego

  Analytica Chimica Acta. 01/1995; 315:69.
• 6.26

  Impact points

  Competitive heterogeneous enzyme immunoassay for theophylline by flow-injection analysis with electrochemical detection of p-aminophenol.

  E P Gil, H T Tang, H B Halsall, W R Heineman, A S Misiego

  Clinical chemistry. 05/1990; 36(4):662-5.

  A competitive enzyme-linked immunoabsorbent assay based on the flow-injection amperometric detection of p-aminophenol has been investigated with use of the materials and general procedure of a commercial kit for the determination of theophylline in human serum. The antibody is immobilized on glass b... [more] A competitive enzyme-linked immunoabsorbent assay based on the flow-injection amperometric detection of p-aminophenol has been investigated with use of the materials and general procedure of a commercial kit for the determination of theophylline in human serum. The antibody is immobilized on glass beads, and the enzyme label is alkaline phosphatase (EC 3.1.3.1). The high currents generated during the electrochemical detection allowed a rapid (35 min) and simple determination of theophylline throughout its therapeutic range (10-20 mg/L) and also in the subtherapeutic range (detection limit of about 80 micrograms/L).