Preconcentration of volatile elements on quartz surface prior to determination by atomic spectrometry

Korkmaz, Deniz
Hydride generation technique is frequently used for the detection of elements as As, Se, Sb, Sn, Bi, Ge, Te and Pb that form volatile hydrides in solution using a reductant. In this study, a novel quartz trap for on-line preconcentration of volatile analyte species was designed. Pb, Sb and Cd were selected as analyte elements and chemical vapour generation technique was employed for generation of their volatile species in flow systems. The trapping medium was formed by external heating of either the inlet arm of the quartz tube atomizer or a separate cylindirical quartz tube. Generated analyte species were trapped on quartz surface heated to the collection temperature and the collected species were revolatilized when the trap was heated further to releasing temperature and hydrogen gas was introduced in the trapping medium. The conventional quartz T-tube and multiple microflame quartz tube were employed as atomizers. The influence of relevant experimental parameters on the generation, collection and revolatilization efficiencies was investigated. Optimum conditions, performance characteristics of the trap and analytical figures of merit are presented. Experimental design was used for optimizations in some cases. Standard reference materials were analyzed to assess the accuracy of the proposed method. For a collection period of 1.0 minute for Pb, 2.0 minutes for Sb and 3.0 minutes for Cd, 3s limit of detections, in pg ml-1, were 19, 3.9 and 1.8, respectively. In cases of Sb and Cd, the limits of detections obtained are the same as the best attained with in-situ trapping in graphite furnaces.


Determination of Arsenobetaine in Fish Tissue by Species Specific Isotope Dilution LC-LTQ-Orbitrap-MS and Standard Addition LC-ICPMS
Yang, Lu; Ding, Jianfu; Maxwell, Paulette; McCooeye, Margaret; Windust, Anthony; Ouerdane, Laurent; Bakirdere, Sezgin; Willie, Scott; Mester, Zoltan (American Chemical Society (ACS), 2011-05-01)
An accurate and precise method for the determination of arsenobetaine (AsB, (CH(3))(3)(+)AsCH(2)COO(-)) in fish samples using exact matching species specific isotope dilution (ID) liquid chromatography LTQ:Orbitrap mass spectrometry (LC-LTQ-Orbitrap-MS) and standard addition LC inductively coupled plasma mass spectrometry (LC-ICPMS) is described. Samples were extracted by sonication for 30 min with high purity deionized water. An in-house synthesized (13)C enriched AsB spike was used for species specific ID...
Volkan, Mürvet; Ataman, Osman Yavuz (1987-10-01)
Silica modified by the addition of mercapto chelating groups has been developed for the pre-concentration of trace metals from natural waters. This material removes cadmium, copper, lead and zinc from aqueous solution and can be employed for the pre-concentration of these metals by both column and batch techniques. Under column and batch conditions recoveries larger than 95% were common. For batch extractions of cadmium, zinc, copper and lead from sea water, recoveries of 91 ± 5, 98 ± 4, 97 ± 4 and 96 ± 5%,...
Use of multi-walled carbon nanotubes in matrix solid phase dispersion extraction combined with gas chromatography
Njie, Njaw; Aygün, Rüveyde Sezer; Department of Chemistry (2008)
The use of Multi-Walled Carbon Nanotubes (MWCNT) as solid sorbent in Matrix Solid-Phase Dispersion (MSPD) extraction and preconcentration method was presented to determine some commonly used organophosphorus insecticides/OPIs in honey samples using a Gas Chromatography Flame Ionization Detector (GC-FID). OPIs are poisonous compounds used to kill insects and rodents by affecting their nervous system. The limit of detections obtained after MSPD extraction were 7.0 ng/g for Malathion, Malaoxon and Fenitrothion...
Electrochhemical hydride generation and tungsten trap atomic absorption spectrometry for determination of antimony
Yıldıran, Ahmet; Ataman, Osman Yavuz; Department of Chemistry (2008)
Electrochemical hydride generation is an alternative technique to the chemical hydride generation by NaBH4 which is widely used for atomic spectrometric determination of volatile elements such as As, Bi, Ge, Pb, Sb, Se, Sn and Te. The aim of this research has been to develop an analytical technique at the level of ng/L for determination of antimony by using a simple and inexpensive AA spectrometer and the other parts that can be built in any laboratory. Carbon rod and platinum foil were used as cathode and ...
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...
Citation Formats
D. Korkmaz, “Preconcentration of volatile elements on quartz surface prior to determination by atomic spectrometry,” Ph.D. - Doctoral Program, Middle East Technical University, 2004.