Development of novel analytical methods for selenium, gold, silver and indium determination using volatile compound generation, atom trapping and atomic absorption spectrometry

Download
2011
Arslan, Yasin
A novel analytical technique was developed where gaseous hydrogen selenide formed by sodium tetrahydroborate reduction is transported to and trapped on a resistively heated gold-coated W-coil atom trap for in situ preconcentration. The atom trap is held at 165 ºC during the collection stage and is heated up to 675 ºC for revolatilization; analyte species formed are transported to an externally heated quartz T-tube where the atomization takes place and the transient signal is obtained. For gold, a high volume gas liquid separator (HVGLS) was designed to improve the detection limit of Au down to the ng mL-1 levels. In this apparatus, analyte and reductant solutions are collected in a limited volume and volatile analyte species are formed. After separation of the volatile analyte species from liquid phase, the entire analyte vapor is sent to an atomizer. A W-coil trap was used to further decrease the detection limit. The enhancement factor for the characteristic concentration was found to be 10.7 when compared to HG-AAS performance without W-coil trap by using peak height values. Furthermore, the generation of analytically useful volatile form of Au has been studied. The flow injection generation was performed in a dedicated generator consisting of a special mixing apparatus and gas-liquid separator design. The on-line atomization in the quartz tube multiatomizer for atomic absorption (AAS) detection has been employed as the convenient atomization/detection mean. 198Au, 199Au radioactive indicator of high specific activity together with AAS measurements was used to track quantitatively the transfer of analyte in the course of generation and transport to the atomizer. In-situ trapping in GF for AAS was explored as an alternative to the on-line atomization. Transmission electron microscopy measurements proved the presence of Au nanoparticles of diameter of approximately 10 nm and smaller transported from the generator by the flow of carrier Ar. For silver, three types of GLS which are U-shaped, cylindrical and high volume gas liquid separators (HVGLS) were used to compare the sensitivities of these GLSs during Ag determination. The DL (3s) values were found as 29 ng mL-1, 0.4 ng mL-1 and 0.05 ng mL-1 for U-shaped GLS, cylindrical GLS with W-coil trap and HVGLS with W-coil trap, respectively. For indium, two types of GLS which are cylindrical and HVGLS with W-coil trap were used. The LOD and characteristic concentration were found as 148 and 317 ng mL-1 with cylindrical shape GLS. HVGLS with W-coil trap was used to improve sensitivity. In this case, LOD and characteristic concentration were found to be 0.46 and 0.98 ng mL-1, respectively. Moreover, to increase the reactivity between indium and reductant solutions, Ru(acac)3 catalyst was used. In this case, LOD and characteristic concentration were found to be 0.13 and 0.23 ng mL-1, respectively. In the case of using this catalyst, sensitivity was enhanced around 1378 fold with respect to cylindrical GLS.

Suggestions

Evaluation of adsorbents with passive sampling and their analytical methods to determine volatile organic compounds emitted from vehicular exhaust
CİVAN, MİHRİBAN; Tuncel, Süleyman Gürdal (2012-04-01)
In order to accurate and precise determination of Volatile Organic Compounds (VOCs) from vehicular emissions were developed method including a) adsorption of VOCs on different adsorbents followed by thermal desorption and gas chromatography (GC) with flame ionization detector (FID) quantification, b) validation of the sampling and analytical method. The adsorption efficiency of Tenax and Chromosorb 106 adsorbents were eveluated for 104 VOCs to select of adequate sorbent for passive sampling. Since most of t...
Evaluation of adsorbents with passive sampling and their analytical methods to determine volatile organic compunds emitted from vehicular exhaust
Civan, Mihriban; Tuncel, Süleyman Gürdal (2012-09-01)
In order to accurate and precise determination of Volatile Organic Compounds (VOCs) from vehicular emissions were developed method including a) adsorption of VOCs on different adsorbents followed by thermal desorption and gas chromatography (GC) with flame ionization detector (FID) quantification, b) validation of the sampling and analytical method. The adsorption efficiency of Tenax and Chromosorb 106 adsorbents were eveluated for 104 VOCs to select of adequate sorbent for passive sampling. Since most of t...
Epoxidation reactions of small alkenes on catalytic surfaces
Kurnaz, Emine; Önal, Işık; Department of Chemical Engineering (2011)
Propylene epoxidation reaction was investigated on catalytic surfaces of chlorinated copper(I) oxide and ruthenium(IV) oxide using periodic density functional theory (DFT). Cu2O(001) and (110) surface of RuO2 was selected to generate chlorinated surfaces to be used in the study. Besides epoxidation, other reactions that compete with epoxidation were also studied such as formations of allyl-radical, acrolein, acetone on chlorinated Cu2O(001) and formations of propionaldehyde, allyl-radical and acetone on chl...
Novel conversion of thiols into disulfides, via S-nitrosothiol intermediates using trichloronitromethane
Demir, Ayhan Sıtkı; Igdir, AC; Mahasneh, AS (1999-10-15)
An efficient oxidative coupling of thiols to give disulfides via thionitrite (S-nitrosothiol) intermediate is described using trichloronitromethane as an efficient reagent in organic solvents and water. Cysteine and glutathione are converted into the corresponding disulfides in water in high yields.
A novel analytical system involving hydride generation and gold-coated W-coil trapping atomic absorption spectrometry for selenium determination at ng l(-1) level
Kula, I.; Arslan, Y.; Bakirdere, S.; Ataman, Osman Yavuz (2008-08-01)
A novel analytical technique was developed where gaseous hydrogen selenide formed by sodium tetra hydrobora te reduction is transported to and trapped on a resistively heated gold-coated W-coil atom trap for in situ preconcentration. Gold coating on W-coil was prepared by using an organic solution of Au. The atom trap is held at 165 degrees C during the collection stage and is heated up to 675 degrees C for revolatilization; analyte species formed are transported to an externally heated quartz T-tube where ...
Citation Formats
Y. Arslan, “Development of novel analytical methods for selenium, gold, silver and indium determination using volatile compound generation, atom trapping and atomic absorption spectrometry,” Ph.D. - Doctoral Program, Middle East Technical University, 2011.