Voltammetric analysis of luminescent markers in gunshot residues.

Currently, SEM-EDS is used to detect gunshot residue (GSR) from the presence of Ba, Pb, and Sb in the sample. However, the development of new nontoxic ammunition (NTA) has prevented conventional metals from being found. In this work, we aim to determine the presence of an inorganic luminescent chemical marker based on rare earth in gunshot residues using the technique of squarewave voltammetry (SWV). After firing, the luminescent complex [(Eu2 Zr)(btc)3 (Hbtc)0.5 .6H2 O], which is used as a chemical marker, can be detected under a UV lamp. An aqueous solution with 0.1 mol L-1 KCl as supporting electrolyte can be easily collected on carbon paste electrode surfaces for SWV analysis A = 100 mV, f = 10 Hz, and step potential of 5 mV are required. The luminescent marker incorporated into the carbon paste electrode showed two anodic peak currents in the region of 0.4 V (vs Ag/AgCl) and at 0.75 V (vs Ag/AgCl) and also a cathodic one in 0.4 V (vs Ag/AgCl). SEM-EDS was able to analyze the same voltammetric results for conventional and nontoxic ammunition containing the luminescent marker. Therefore, voltammetry and SEM-EDS are valid for detecting the new residue marker in GSR. Despite this, the electrochemical method is still more advantageous because of its low cost and lack of expensive equipment and supplies in forensic laboratories.

Electrochemical Sensors Containing Schiff Bases and their Transition Metal Complexes to Detect Analytes of Forensic, Pharmaceutical and Environmental Interest. A Review.

Schiff bases and their transition metal complexes are inexpensive and easy to synthesize. These compounds display several structural and electronic features that allow their application in numerous research fields. Over the last three decades, electroanalytical scientists of various areas have developed electrochemical sensors from many compounds. The present review discusses the applicability of Schiff bases, their transition metal complexes and new materials containing these compounds as electrode modifiers in sensors to detect analytes of forensic, pharmaceutical and environmental interest. In forensic sciences, Schiff bases are mainly used to analyze illicit drugs: chemical reactions involving Schiff bases can help to elucidate illicit drug production and to determine analytes in seized samples. In the environmental area, given that most methodologies provide Limit of Detection (LOD) values below the values recommended by regulatory agencies, Schiff bases constitute a promising strategy. As for pharmaceutical applications, Schiff bases represent an approach for analysis of complex biological samples containing low levels of the target analytes in the presence of a large quantity of interfering compounds. This review will show that new highly specific materials can be synthesized based on Schiff bases and applied in the pharmaceutical industry, toxicological studies, electrocatalysis and biosensors. Most literature papers have reported on Schiff bases combined with carbon paste to give a chemically modified electrode that is easy and inexpensive to produce and which displays specific and selective sensing capacity for different applications.

Voltammetric determination of cocaine in confiscated samples using a carbon paste electrode modified with different [UO2(X-MeOsalen)(H2O)] · H2O complexes.

A fast and non-destructive voltammetric method to detect cocaine in confiscated samples based on carbon paste electrode modified with methoxy-substituted N,N'-ethylene-bis(salcylideneiminato)uranyl(VI)complexes, [UO2(X-MeOSalen)(H2O)] · H2O, where X corresponds to the positions 3, 4 or 5 of the methoxy group on the aromatic ring, is described. The electrochemical behavior of the modified electrode and the electrochemical detection of cocaine were investigated using cyclic voltammetry. Using 0.1 mol · L(-1) KCl as supporting-electrolyte, a concentration-dependent, well-defined peak current for cocaine at 0.62 V, with an amperometric sensitivity of 6.25 × 104 µA · mol · L(-1) for cocaine concentrations ranging between 1.0 × 10(-7) and 1.3 × 10(-6) mol · L-1 was obtained. Chemical interference studies using lidocaine and procaine were performed. The position of the methoxy group affects the results, with the 3-methoxy derivative being the most sensitive.

Voltammetric determination of Δ9-THC in glassy carbon electrode: An important contribution to forensic electroanalysis.

A new voltammetric method for the determination of Δ(9)-tetrahydrocannabinol (Δ(9)-THC) is described. The voltammetric experiments were accomplished in N-N dimethylformamide/water (9:1, v/v), using tetrabutylammonium tetrafluoroborate (TBATFB) 0.1mol/L as supporting electrolyte and a glassy carbon disk electrode as the working electrode. The anodic peak current was observed at 0.0V (vs. Ag/AgCl) after a 30s pre-concentration step under an applied potential of -1.2V (vs. Ag/AgCl). A linear dependence of Δ(9)-THC detection was obtained in the concentration range 2.4-11.3ng/mL, with a linear correlation coefficient of 0.999 and a detection limit of 0.34ng/mL. The voltammetric method was used to measure the content of Δ(9)-THC in samples (hemp and hashish) confiscated by the police. The elimination of chemical interferences from the samples was promptly achieved through prior purification using the TLC technique, by employing methanol/water (4:1, v/v) as the mobile phase. The results showed excellent correlation with results attained by HPLC.

A simple and fast method for the production and characterization of methylic and ethylic biodiesels from tucum oil via an alkaline route.

A simple, fast, and complete route for the production of methylic and ethylic biodiesel from tucum oil is described. Aliquots of the oil obtained directly from pressed tucum (pulp and almonds) were treated with potassium methoxide or ethoxide at 40°C for 40 min. The biodiesel form was removed from the reactor and washed with 0.1 M HCl aqueous solution. A simple distillation at 100°C was carried out in order to remove water and alcohol species from the biodiesel. The oxidative stability index was obtained for the tucum oil as well as the methylic and ethylic biodiesel at 6.13, 2.90, and 2.80 h, for storage times higher than 8 days. Quality control of the original oil and of the methylic and ethylic biodiesels, such as the amount of glycerin produced during the transesterification process, was accomplished by the TLC, GC-MS, and FT-IR techniques. The results obtained in this study indicate a potential biofuel production by simple treatment of tucum, an important Amazonian fruit.

Simultaneous determination of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry using a glassy carbon-mercury-film electrode.

A new, versatile, and simple method for quantitative analysis of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry is described. These metals can be quantified by direct dissolution of fuel ethanol in water and subsequent voltammetric measurement after the accumulation step. A maximum limit of 20% ( v/ v) ethanol in water solution was obtained for voltammetric measurements without loss of sensitivity for metal species. Chemical and operational optimum conditions were analyzed in this study; the values obtained were pH 2.9, a 4.7-microm thickness mercury film, a 1,000-rpm rotation frequency of the working electrode, and a 600-s pre-concentration time. Voltammetric measurements were obtained using linear scan (LSV), differential pulse (DPV), and square wave (SWV) modes and detection limits were in the range 10(-9)-10(-8) mol L(-1) for these metal species. The proposed method was compared with a traditional analytical technique, flame atomic absorption spectrometry (FAAS), for quantification of these metal species in commercial fuel ethanol samples.

Voltammetric determination of fenbendazole in veterinarian formulations.

A versatile voltammetric method for quantitative determination of fenbendazole (FBZ) in commercial tablets has been proposed, where direct dissolution of tablets is carried out in 0.1 mol l(-1) tetrabutylamoniun tetrafluorborate containing dimethylformamide solutions. Linear sweep (LSV), square wave (SWV) and differential pulse (DPV) voltammetry techniques were applied to study FBZ at a glassy carbon electrode, exhibiting a well defined irreversible oxidation peak at 1.15 V vs. SCE. This methodology allows a precise quantitative determination of FBZ presenting detection limits of 5.2 x 10(-5) (LSV), 5.0 x 10(-6) (DPV) and 5.0 x 10(-5) mol l(-1) (SWV).