On-line preconcentration of vapor forming elements on resistively heated w-coil prior to their determination by atomiz absorption spectrometry

Download
2004
Cankur, Oktay
Vapor generation in atomic spectrometry is a well established technique for the determination of elements that can be volatilized by chemical reactions. In-situ trapping in graphite furnaces is nowadays one of the most popular methods to increase the sensitivity. In this study, resistively heated W-coil was used as an online trap for preconcentration and revolatilization of volatile species of Bi, Cd and Pb. The collected analyte species were revolatilized rapidly and sent to a quartz Ttube atomizer for AAS measurement. Although the nature of revolatilized species of Bi and Pb are not clear, they are probably molecular since they can be transported at least 45 cm without any significant decrease in the peak height values. However, cadmium is revolatilized from the trap surface as atoms. The experimental parameters were optimized for the highest vapor generation, trapping and revolatilization efficiencies. The concentration limits of detection calculated by the 3 of blank solution were found to be 0.0027, 0.0040 and 0.015 ng/mL for Bi (18 mL), Cd (4.2 mL) and Pb (2 mL), respectively; enhancement factors in the sensitivity were 130, 31 and 20, respectively. These values are comparable with those obtained by in-situ trapping in graphite furnaces or even ICP-MS found in the literature or better. Sensitivity can be improved further for Bi and Cd using larger sample volumes, but purification of blank is required for Pb. Certified standard reference materials were analyzed for the assessment of accuracy of developed method.

Suggestions

Determination of germanium at trace levels by chloride generation atomic absorption spectrometry
Kaya, Murat; Volkan, Mürvet; Department of Chemistry (2004)
Trace amounts of germanium is determined by flame atomic absorption spectrometry by utilizing the vaporization of germanium tetrachloride. Using a continuous flow reactor, sample solution is mixed with concentrated hydrochloric acid and heated to 80ð C to form volatile germanium tetrachloride which can be subsequently sent to N2O-C2H2 flame AAS. The necessary conditions for the volatilization of germanium tetrachloride are investigated in detail and the applicability of the method for the determination of t...
Determination of silver by chemical vapour generation and atomic absoption spectrometry
Öztürk, Çağla Pınar; Ataman, Osman Yavuz; Department of Chemistry (2004)
A method for determination of silver has been developed based on chemical vapour generation atomic absorption spectrometry (CVGAAS). Volatile species of silver in acidified medium were generated by the reduction of sodium tetrahydroborate; these species were sent to a flame-heated quartz tube atomizer (QTA) following isolation by using a gas-liquid separator. Flow injection (FI) was used for sample introduction. Optimization of parameters such as; concentrations of acid and NaBH4 concentration, flow rates o...
Preparation and characterization of surface enhanced raman scattering substrate through electro deposition of silver-pedot film on ito glass surface
Doğan, Üzeyir; Volkan, Mürvet; Department of Chemistry (2011)
Detection of chemicals is a vital part of chemistry. For this reason, many detection systems are developed by scientists and every detection system has its own advantages. Raman spectroscopy is one of these detection systems having many advantages. However, this technique suffers from low signal intensity disadvantage. By developing a well prepared substrate, this problem can be easily solved; moreover, even single molecule detection can be possible. In this study, a novel surface enhanced Raman scattering ...
Optimization of ETV-ICP(TOF)MS and transient signal profiles for reducing isobaric interferences
Ertaş, Gülay (Royal Society of Chemistry (RSC), 2005-01-01)
One of the advantages of the ETV sample introduction is the ability to temporally separate analyte elements in complex mixtures by differences in their vaporization temperatures within the ETV for ICPMS. However, the broadening of the transient peaks in the transport tubing often obscures this temporal resolution. This study shows that decreasing the transport tubing diameter produces little broadening beyond that produced during aerosol production in the ETV. Maintaining such narrow peaks through the trans...
Hydrogen sulfide determination by solid surface luminescence
Eroglu, AE; Volkan, Mürvet; Bayramh, E; Ataman, Osman Yavuz; Mark, HB (1996-07-01)
In the analytical system suggested, atmospheric hydrogen sulfide reacts with the surface of a filter paper treated with aqueous cadmium chloride and yields a luminescent species whose intensity can be correlated with the analyte concentration in ambient air. It was shown that the luminescent species are CdS solid particles which were formed in a well defined size. The paper luminescence was also tried on polymeric surfaces; polyethyleneoxide, polyvinyl alcohol, ethylcellulose and carboxymethylcellulose were...
Citation Formats
O. Cankur, “On-line preconcentration of vapor forming elements on resistively heated w-coil prior to their determination by atomiz absorption spectrometry,” Ph.D. - Doctoral Program, Middle East Technical University, 2004.