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1.
Talanta ; 178: 400-409, 2018 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-29136840

RESUMO

We examined the feasibility of using handheld mid-infrared (MIR) Fourier-Transform infrared (FT-IR) instrumentation for detecting and analysing cyanide (CN) contamination in field contaminated soils. Cyanide spiking experiments were first carried out, in the laboratory, to test the sensitivity of infrared Fourier transform (DRIFT) spectrometry to ferro- and ferricyanide compounds across a range of reference soils and minerals. Both benchtop and handheld diffuse reflectance infrared spectrometers were tested. Excellent results were obtained for the reference soils and minerals, with the MIR outperforming the near-infrared (NIR) range. Spectral peaks characteristic of the -C≡N group were observed near 2062 and 2118cm-1 in the MIR region for the ferro- and ferricyanide compounds spiked into soils/minerals, respectively. In the NIR region such peaks were observed near 4134 and 4220cm-1. Cyanide-contaminated samples were then collected in the field and analyzed with the two spectrometers to further test the applicability of the DRIFT technique for soils containing aged CN residues. The prediction of total CN in dry and ground contaminated soils using the handheld MIR instrument resulted in a coefficient of determination (R2) of 0.88-0.98 and root mean square error of the cross-validation (RMSE) of 21-49mgkg-1 for a CN range of 0-611mgkg-1. A major peak was observed in the MIR at about 2092cm-1 which was attributed to "Prussian Blue" (Fe4[Fe(CN)6]3·xH2O). These results demonstrate the potential of handheld DRIFT instrumentation as a promising alternative to the standard laboratory method to predict CN concentrations in contaminated field soils.


Assuntos
Cianetos/análise , Poluentes do Solo/análise , Solo/química , Espectroscopia de Infravermelho com Transformada de Fourier/instrumentação , Cianetos/química , Ferricianetos/análise , Ferricianetos/química , Poluentes do Solo/química
2.
Sensors (Basel) ; 15(8): 18887-900, 2015 Jul 31.
Artigo em Inglês | MEDLINE | ID: mdl-26263997

RESUMO

The development of portable sensors that can be used outside the lab is an active area of research in the electroanalytical field. A major focus of such research is the development of low-cost electrodes for use in these sensors. Current electrodes, such as glassy-carbon electrodes (GCEs), are costly and require time-consuming preparation. Alternatives have been proposed, including mechanical pencil-lead electrodes (MPEs). However, MPEs themselves possess numerous drawbacks, particularly structural fragility. In this paper, we present a novel pencil-graphite electrode (PGE) fabricated from a regular HB#2 pencil. This PGE is a simple, disposable, extremely low-cost alternative to GCEs ($0.30 per PGE, vs. $190 + per GCE), and possesses the structural stability that MPEs lack. PGEs were characterized by square-wave voltammetry of ferricyanide, gallic acid, uric acid, dopamine, and several foodstuffs. In all cases, PGEs demonstrated sensitivities comparable or superior to those of the GCE and MPE (LOD = 5.62 × 10(-4) M PGE, 4.80 × 10(-4) M GCE, 2.93 × 10(-4) M MPE). Signal areas and peak heights were typically four to ten times larger for the PGE relative to the GCE.


Assuntos
Antioxidantes/análise , Custos e Análise de Custo , Técnicas Eletroquímicas/economia , Técnicas Eletroquímicas/métodos , Grafite/química , Grafite/economia , Madeira/química , Carbono/química , Eletrodos/economia , Ferricianetos/análise , Frutas/química , Ácido Gálico/análise , Vidro/química , Chumbo/química , Padrões de Referência , Reprodutibilidade dos Testes , Verduras/química
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