Date

2010

Author

Özcan Gurbetçioğlu, G. Pelin

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Flame atomic absorption spectroscopy (FAAS) is a common technique for detecting metals and metalloids in environmental, biological and metallurgical samples. Although it is a rather old technique, it is still very reliable, simple to use and inexpensive. The technique can be used to determine the concentration of over 70 different metals in a solution. However, it has detection limits at mg/L levels. Some atom trapping methods have been developed to reach the detection limits of ng/mL levels. Slotted quartz tube (SQT) is one of these atom trapping methods. It is an important technique, since it is easy to use, applicable in all laboratories, commercially available and economical. This thesis consists of development of a sensitive method for cadmium with the help of SQT atom trap. In this study, it was used for two different purposes. One was for keeping the analyte atoms more in the light path; in other words, for increasing the residence times of analyte atoms in the measurement zone. This first application was provided a 2.9 times enhancement with respect to conventional FAAS. Second application was for trapping the analyte on the surface of the SQT, in other words, for performing on-line preconcentration of cadmium in SQT. In the presence of a lean flame, analyte samples were trapped and collected for a few minutes at a low suction rate. After finishing the collection period, analyte atoms were revolatilized with the help of a small volume of (10-50 µL) methyl isobutyl ketone (MIBK) and a rapid atomization occurred. This introduction also altered the flame composition momentarily and analyte atoms were released from the surface of the SQT. Application of this method enhanced the sensitivity 2065 times with respect to conventional FAAS. Another approach to this type of atom trapping has been investigated also in this study, which was coating of SQT with some metals having low volatility. Therefore, some transition metals were coated to the surface of SQT and among them zirconium was selected as the best coating material as having the most sensitivity enhancement factor. That is why, rest of the study was performed with the Zr coated SQT. The enhancement was 3368 as compared with FAAS. Cd determination with this method provides LOD value of 8 pg/mL and Co value of 19 pg/mL. In order to see the effect of some other type of elements or ions on determination of cadmium, interference study was done.

Subject Keywords

Chemistry., QD Analytical Chemistry 71-142.

URI

http://etd.lib.metu.edu.tr/upload/12612212/index.pdf
https://hdl.handle.net/11511/19790

Collections

Graduate School of Natural and Applied Sciences, Thesis