Determination of thallium is important due to its toxic effects on the environment and human health. Extremely low abundance of thallium in earth crust requires very sensitive and accurate methods for determination of this element. Although volatile compound generation is a sensitive, fast and economical method, thallium determination by this method has not been sufficiently investigated in literature, because of the fact that the formation of volatile forms of this element is a difficult task.
A continuous flow volatile compound generation system was developed and parameters that affect the analytical signal were optimized. Sample solutions were acidified with 0.5 mol/L HNO3 and prepared in 0.0005% (v/v) rhodamine B and 1.0 mg/L Pd while 0.5% (m/v) NaBH4 stabilized in 0.5% (m/v) NaOH was used as reductant. Fast decomposition and unstability of thallium volatile species affected system performance negatively.
Flow injection volatile compound generation studies were carried out with a special system. After optimizations, LOD and LOQ values were calculated as 12 ng/mL and 40 ng/mL according to peak height values in HNO3 medium. Similarly, in HCl medium LOD and LOQ values were calculated as 14 ng/mL and 45 ng/mL. Addition of Te and Pd to the sample solution containing co-enhancement reagent rhodamine B improved volatile compound generation efficiency in peak height by 3.6 and 9.3, respectively. Type of the acid used was affected peak heights and peak shapes of Tl+ and Tl3+ volatile species and HNO3 medium gave better results.
By changing the location of introduction for Ar gas, the sources of memory effects and reasons of peak broadening were investigated. Most of the memory effects were coming from the gas-liquid separator (GLS) or before the GLS, as well as T-tube atomizer.
Nature and behavior of Tl volatile species were also investigated and it was found that Tl and also Pd were generated in the form of nanoparticles. Transmission electron microscopic (TEM) measurements prove the presence of Tl nanoparticles in the analyte species transported to the atomizer by the effect of carrier Ar gas.
| Identifer | oai:union.ndltd.org:METU/oai:etd.lib.metu.edu.tr:http://etd.lib.metu.edu.tr/upload/12613728/index.pdf |
| Date | 01 October 2011 |
| Creators | Ataman, Seval |
| Contributors | Ataman, Osman Yavuz |
| Publisher | METU |
| Source Sets | Middle East Technical Univ. |
| Language | English |
| Detected Language | English |
| Type | M.S. Thesis |
| Format | text/pdf |
| Rights | To liberate the content for public access |
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