Inorganic antimony speciation using tungsten coil atom trap and hydride generation atomic absorption spectrometry

Download
2010
Akay, Pınar
Antimony is a toxic element which is mostly found in two oxidation states (III and V) in environmental, biological and geological samples. Antimony may form various inorganic and organic compounds that exhibit differences in analytical behavior, toxicity and mobility; inorganic compounds of antimony are more toxic than organic forms and toxicity of Sb(III) has been shown to be 10 times higher than that of Sb(V). Therefore selective determination of Sb(III) and Sb(V) is required in environmental and biological samples. Hydride generation atomic absorption spectrometry is a sensitive, fast and economical technique for the determination of antimony at trace level. A possible non-chromatographic method for antimony speciation is hydride generation atomic absorption spectrometry that is based on the relatively slow kinetics of hydride formation from Sb(V). In this study, continuous flow hydride generation method for the determination of antimony was developed and hydride generation conditions were optimized. Analyte solution was prepared in 0.050 mol/L HCl and 1.2% (w/v) NaBH4 stabilized in 0.30% (w/v) NaOH was used as a reductant solution. Inorganic antimony speciation conditions were determined by continuous flow HGAAS system. For the pre-reduction of Sb(V) to Sb(III), 8.0% (w/v) potassium iodide (KI) and 0.10% (w/v) ascorbic acid were used. Further speciation study was also carried out using Ir coated W-coil Atom Trap Hydride Generation Atomic Absorption Spectrometry. Tungsten coil atom trap was used to enhance the sensitivity. Tungsten coil surface was treated with Ir and totally 250 μg 1000 mg/L Ir stock solution was used for coating of tungsten coil. LOD and LOQ values were calculated as 152 pg/mL and 508 pg/mL according to 120 seconds trapping. 128 and 37 fold enhancement were obtained for 120 seconds collection with respect to W-coil-ETAAS and ETAAS, respectively.

Suggestions

Asymmetric synthesis of chiral camphor fused pyridine type novel organocatalysts
Küçükdişli, Murat; Tanyeli, Cihangir; Department of Chemistry (2009)
Chiral pyridines as organocatalysts have been used in asymmetric organic synthesis in recent years. The asymmetric synthesis of camphor fused pyridine type novel organocatalysts were perfomed starting from cheap and easily available natural (+)-camphor. Using camphor fused pyridine skeleton, six organocatalysts 29, 32, 33, 38, 40, and 41were successfully synthesized. The first four nucleophilic and Lewis base catalysts 29, 32, and 33 are different P-oxides and P,N-dioxides which were tested in allylation of...
Multicomponent ion exchange on clinoptilolite
Bayraktaroğlu, Kerem; Yücel, Hayrettin; Department of Chemical Engineering (2006)
Zeolites are crystalline, hydrated aluminosilicate minerals that are characterized by their ability to exchange some of their constituent cations with cations in aqueous solutions, without a major change in their crystalline structure. Clinoptilolite is the most abundant ype of zeolite and it has received extensive attention due to its favorable selectivity for mmonium and certain heavy metal cations. The aim of this study is to investigate the binary and ternary (multicomponent) ion xchange behavior of sod...
Voltammetric methods of reboxetine analysis and the mechanism of its electrode reactions
Altunöz Erdoğan, Deniz; Erk, Nevin; Kilic, Esma (Walter de Gruyter GmbH, 2013-05-01)
Reboxetine (RBX) electrochemical redox behavior at hanging mercury drop (HMDE) and glassy carbon electrodes (GCE) was studied in various pH Britton-Robinson universal buffers using cyclic voltammetry and square-wave voltammetry. RBX was reduced at the HMDE and oxidized at the GCE with reversible adsorption controlled and irreversible diffusion controlled processes respectively. The anodic peak is due to the amine and the cathodic peak may correspond to oxygen protonation. An oxidation reaction mechanism is ...
Darzens reaction of substituted alfa-bromo acetophenones with acyl phosphonates
Pirkin, Eser; Demir, Ayhan Sıtkı; Department of Chemistry (2008)
Phosphorous containing small cycles are very important building blocks in organic and medicinal chemistry. Many of their derivatives, especially cyclopropyl- and 1,2- epoxypropylphosphonates, have attracted great attention due to the broad spectrum of their biological properties including antiviral, anticancer, antibiotic, antibacterial, pesticidal, insecticidal and enzyme inhibitory activities. The Darzens condensation is one of the most potential methodologies for the preperation of α,β-epoxy carbonyl com...
Tellurium speciation using hydride generation atomic absorption spectrometry and in-situ graphite cuvette trapping
Yıldırım, Emrah; Ataman, Osman Yavuz; Department of Chemistry (2009)
In recent years speciation analysis is becoming more important as it is known that each chemical form of an element behaves differently in biological and environmental media. Since abundance of tellurium in earth crust is extremely low, very sensitive and accurate methods are needed to determine the concentration of tellurium. Hydride generation atomic absorption is a sensitive, fast and economical technique applied for the determination of tellurium. Speciation of tellurium can be achieved by making use of...
Citation Formats
P. Akay, “Inorganic antimony speciation using tungsten coil atom trap and hydride generation atomic absorption spectrometry,” M.S. - Master of Science, Middle East Technical University, 2010.