RESUMEN
This paper represents the results of a case study investigating the development of a novel, simple, cost-effective, solventless and sensitive chromatographic method for the determination of volatile pesticides in aqueous samples by an electrothermally prepared pencil graphite (PG). In this study, PG were conditioned by passing a suitable direct current to activate PG by Joule effect. Conditioned PG was used for the extraction of Chlorpyrifos (CP), which is used as case study. The method was also found successful in the determination of CP in real water samples, providing acceptable recovery values (82-111%).
Asunto(s)
Cloropirifos , Grafito , Residuos de Plaguicidas , Plaguicidas , Cloropirifos/análisis , Residuos de Plaguicidas/análisis , Plaguicidas/análisis , Agua/análisisRESUMEN
This report comprises the novel usage of polythiophene - ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett-Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box-Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002-0.667ng mL(-1). Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.
Asunto(s)
Silicatos de Aluminio/química , Bebidas/análisis , Contaminación de Alimentos/análisis , Líquidos Iónicos/química , Plaguicidas/aislamiento & purificación , Polímeros/química , Microextracción en Fase Sólida/métodos , Tiofenos/química , Arcilla , Diseño de Equipo , Límite de Detección , Plaguicidas/análisis , Microextracción en Fase Sólida/instrumentaciónRESUMEN
The behaviour of the copper complexes of glycyl-L-histidyl-glycine (GHG) was investigated using cyclic voltammetry and differential pulse voltammetry after their adsorptive accumulation on the surface of a hanging mercury drop electrode (HMDE). The nature of the observed cathodic and anodic peaks was established and optimum conditions were found for the differential pulse cathodic stripping voltammetric detemination of GHG at the 1 x 10(-8)M concentration level using adsorptive accumulation at -0.20 V vs. Ag/AgCl reference electrode and the cathodic stripping peak around -0.4 V (pH 8.3). This peak corresponds to the reduction of the Cu(I)-GHG complex formed at the HMDE surface as an intermediate in the reduction of Cu(II)-GHG to Cu(O)amalgam.
RESUMEN
Aside from its excellent mechanical properties, spider silk (SS) would offer an active surface for heavy metal interaction due to its rich protein structure. The present study describes the potential use of natural (SS) as a sorbent of heavy metals from aqueous solutions. Single and multi-species biosorption experiments of heavy metals by natural SS were conducted using batch and column experiments. The biosorption kinetics, in general, was found to follow the second-order rate expression, and the experimental equilibrium biosorption data fitted reasonably well to Freundlich isotherm. From the Freundlich isotherm, the biosorption capacities of Cu(II) and Pb(II) ions onto SS were found as 0.20 and 0.007 mmol g⻹, respectively. The results showed a decrease in the extent of metal ion uptake with lowering the pH.
Asunto(s)
Cobre/química , Hierro/química , Seda/química , Eliminación de Residuos Líquidos/métodos , Contaminantes Químicos del Agua/química , Purificación del Agua/métodos , Adsorción , Cinética , Modelos QuímicosRESUMEN
A biosensor for specific determination of hydrogen peroxide was developed by using homogenized artichoke (Cynara scolymus L.) tissue in combination with a dissolved oxygen probe and applied in determination of hydrogen peroxide in milk samples. Artichoke tissue, which has catalase activity, was immobilized with gelatine by means of glutaraldehyde and fixed on a pretreated teflon membrane. The electrode response was maximum when 0.05 M phosphate buffer was used at pH 7.0 and at 30 degrees C. Upon addition of hydrogen peroxide, the electrode gives a linear response in a concentration range of 5.0-50 x 10(-5) M with a response time of 3 min. The method was also applied to the determination of hydrogen peroxide in milk samples.