Hydride generation and preconcentration of bismuth on a single-drop followed by determination using electrothermal atomic absorption spectrometry

Download

index.pdf

Date

2015

Author

Dügencili, Başak

Metadata

Show full item record

Item Usage Stats

148
views

54
downloads

A novel method for determination of bismuth is proposed where the analyte is converted to its hydride form, BiH3, followed by head space preconcentration on a single aqueous drop; final detection was done using electrothermal atomic absorption spectrometry (ETAAS). The preconcentration step was named as headspace single-drop microextraction (HS-SDME). Experimental parameters for hydride generation using both continuous flow and batch technique, ETAAS and finally HS-SDME were optimized. For HS-SDME, Pd, Ni, Au or Pt was used as matrix modifiers (MMs) with a concentration of 5.0 mg/L. In hydride generation, sample was prepared in 1.0 mol/L HCl, reductant was 1.0 mL of 0.5% (w/v) NaBH4 stabilized in 0.2% (w/v) NaOH. 3.0 µL of 10.0 µL of selected MM in 1.0% HNO3 was exposed to analyte vapors in head-space mode. Au was selected as the best MM where the detection limit was found to be 0.005 ng/mL using a sample of 5.0 mL. vi Nonspectral interference effects for some species were studied. Regarding the hydride forming species, the effects of As(III), Se(IV), Sb(III), Sn(IV), Te(VI) and Pb(II) were investigated. In the presence of As(III), Se(IV) and Sb(III), the analyte signal was suppressed when interferant/analyte mass ratio was as high as 1000; Sn(IV), Te(VI) and Pb(II) did not have any significant interference effect using the same conditions. Among the transition elements, Co, Cu and Zn seemed to have a suppressing effect while Cr, Mn and Fe had a much lower effect. Regarding the effects of some ubiquitous ions, Ca2+and Mg2+ had no significant effect while Al3+ , Na+ and PO43- had higher effect on analyte signal. The developed method was applied to tap water, bottled water and mineral water samples; it was observed that standard additions would be needed for desired accuracy. Using NIST 1643e “Trace elements in water” standard reference material, satisfactory accuracy was obtained.

Subject Keywords

Bismuth., Absorption., Hydrides., Atomic absorption spectroscopy.

URI

http://etd.lib.metu.edu.tr/upload/12619321/index.pdf
https://hdl.handle.net/11511/25116

Collections

Graduate School of Natural and Applied Sciences, Thesis

Suggestions

OpenMETU
Core

In situ atom trapping of Bi on W-coated slotted quartz tube flame atomic absorption spectrometry and interference studies KILINÇ, ERSİN; BAKIRDERE, Sezgin; AYDIN, FIRAT; Ataman, Osman Yavuz (2013-11-01) Analytical performances of metal coated slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) and slotted quartz tube in situ atom trapping flame atomic absorption spectrometry (SQT-AT-FAAS) systems were evaluated for determination of Bi. Non-volatile elements such as Mo, Zr, W and Ta were tried as coating materials. It was observed that W-coated SQT gave the best sensitivity for the determination of Bi for SQT-FAAS and SQT-AT-FMS. The parameters for W-coated SQT-FAAS and W-coated SQT-AT-FAAS ...
Electrothermal atomic absorption spectrometric determination of gold by vapor formation and in situ trapping in graphite tubes Ertaş, Gülay; Ataman, Osman Yavuz (2004-10-01) Gold was determined in ore samples following generation, separation, collection on a graphite cuvette inner wall, and atomization of its volatile species formed by combining an acidified sample solution with an aqueous sodium tetrahydroborate solution at room temperature. A detection limit of 2.6 mug L-1 (3sigma) was obtained with a 5.0 mL sample volume. Precision of replicate measurements was typically 10% RSD. The overall efficiency of the volatile species generation, transport, and trapping process was 0...
Enantioselective direct aldol reactions promoted by phosphine oxide aziridinyl phosphonate organocatalysts Doğan, Özdemir (2015-12-15) A series of phosphine oxide based chiral Lewis bases were screened as organocatalysts for silicon tetrachloride mediated direct asymmetric aldol reactions between cyclohexanone and various aromatic aldehydes. One of the phosphine oxide-aziridinyl phosphonate POAP-A Lewis bases formed the aldol products in up to 75% yield and with 65% ee.
Dielectric and Thermal Effects on the Optical Properties of Natural Dyes: A Case Study on Solvated Cyanin Malcıoğlu, Osman Barış; Gebauer, Ralph; Varsano, Daniele; Baroni, Stefano (2011-10-05) The optical properties of the flavylium state of the cyanin dye are simulated numerically by combining Car-Parrinello molecular dynamics and linear-response time-dependent density functional theory calculations. The spectrum of the dye calculated in the gas phase is characterized by two peaks in the yellow and in the blue (green and violet), using a GGA-PBE (hybrid-B3LYP) DFT functional, which would bring about a greenish (bright orange) color incompatible with the dark purple hue observed in nature. Descri...
Synthesis of ferrocenyl quinones and ferrocenyl based burning rate catalysts Açıkalın, Serdar; Zora, Metin; Department of Chemistry (2003) Recently, considerable interest has been devoted to the synthesis of new ferrocene derivatives since properly functionalized ferrocene derivatives could be potential antitumor substances. For this purpose, we have investigated the synthesis of ferrocenyl quinones starting from squaric acid. Thermolysis of ferrocenylsubstituted cyclobutenones, which have been prepared from ferrocenyl cyclobutenediones and alkenyllithiums, affords hydroquinones, which furnish, upon oxidation, ferrocenyl quinones. Ferrocenyl c...

Citation Formats

B. Dügencili, “Hydride generation and preconcentration of bismuth on a single-drop followed by determination using electrothermal atomic absorption spectrometry,” M.S. - Master of Science, Middle East Technical University, 2015.