Separation and quantitation of some platinum group metals by rp-hplc

Alshana, Usama
In this study, a reversed-phase high performance liquid chromatography (RP-HPLC) method has been developed to separate and determine Pt and Pd after formation of their chelates with N,N-diethyl-N'-benzoylthiourea (DEBT). With the aim of reducing the number of steps in treating the samples, the method developed does not require the elimination of excess chelating reagent before the analysis of metal chelates. The different physical and chemical parameters affecting separation were examined in details. The whole analysis was completed on a C18 column in 16 min at 280 nm, with the mobile phase of acetonitrile-methanol-water (80:10:10, v:v:v) containing 0.20 mol l-1 pH 5.0 acetate buffer at a flow rate of 0.8 ml min-1. Detection limits of the method, based on 3s, were found as 14.2 ug l-1 for Pd and 0.77 mg l-1 for Pt using a 20-ul sample loop. Reproducibility of the method for ten repeated measurements was found as 2.36 % for 0.60 mg l-1 Pd and 2.58 % for 10.0 mg l-1 Pt as % RSD. The proposed method is a rapid, simple and highly selective method for the simultaneous determination of Pt and Pd by HPLC without the need for any interference elimination process.


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...
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 of PLZT thin films by chemical solution deposition and their characterization
Kaplan, Burkan; Özenbaş, Ahmet Macit; Department of Metallurgical and Materials Engineering (2005)
In this study, La3+ was substituted into lead zirconate titanate (PZT) system by Pb1-xLax(ZryTi1-y)1-x/4O3 nominal stochiometry and it was processed via chemical solution deposition on (111)-Pt/Ti/SiO2/Si-(100) substrate.PLZT solutions were prepared by mixing two solutions, one of which was obtained by dissolving lead acetate and lanthanum acetate hydrate in 2 methoxyethanol at high temperature. This solution was then mixed with the second solution containing zirconium propoxide and titanium isopropoxide. 4...
Deposition of a Sorbent into a Recession on a Solid Support To Provide a New, Mechanically Robust Solid-Phase Microextraction Device
Poole, Justen J.; Grandy, Jonathan J.; Yu, Miao; Boyacı, Ezel; Gomez-Rios, German A.; Reyes-Garces, Nathaly; Bojko, Barbara; Heide, Harmen Vander; Pawliszyn, Janusz (American Chemical Society (ACS), 2017-08-01)
To date, solid-phase microextraction (SPME) fibers used for in vivo bioanalysis can be too fragile and flexible, which limits suitability for direct tissue sampling. As a result, these devices often require a sheathing needle to prepuncture robust sample matrixes and protect the extraction phase from mechanical damage. To address this limitation, a new SPME device is herein presented which incorporates an extraction phase recessed into the body of a solid needle. This device requires no additional support o...
Preconcentration of volatile elements on quartz surface prior to determination by atomic spectrometry
Korkmaz, Deniz; Ataman, Osman Yavuz; Department of Chemistry (2004)
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 a...
Citation Formats
U. Alshana, “Separation and quantitation of some platinum group metals by rp-hplc,” M.S. - Master of Science, Middle East Technical University, 2004.