Trace Element Analysis of Selenium Mahmoud Shahat Ahmed Soliman

139 Pages·2013·2.93 MB·English

Banha University
Faculty of Science
Chemistry department

Trace Element Analysis of Selenium

A Thesis submitted

By

Mahmoud Shahat Ahmed Soliman

(B. Sc. Chemistry)

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Supervisors

Prof. Dr. Ass. Prof. Dr.
Abd El-Fattah Ibrahim Helal Sayed Ahmed Abd El-Aziz Shama

Former Vice Chairman of Ass. Prof. of Analytical chemistry
Atomic Energy Authority Faculty of Science
Banha University

Late Prof. Dr.
Nagwa Faheem Zahran
Former Vice Chairman of Atomic Energy Authority

2010
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(cid:10)ـــ(cid:11)(cid:12)(cid:13)(cid:14)(cid:4)(cid:7)او (cid:16)ـــ(cid:5)(cid:6)(cid:7)ا (cid:10)(cid:14)(cid:17)(cid:7)
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١
٢

٣

٤

/ / (cid:7)(cid:23)(cid:24)(cid:9)(cid:4)(cid:25)(cid:8)ا (cid:20)(cid:21)ر(cid:9)(cid:22)

Acknowledgements

Acknowledgements

First of all, thanks to ALLAH, who enabled me to face and
overcome all problems throughout this work and by the grace of whom
the progress and success was possible.

I would like to express my gratitude and appreciation to Professor Dr.
Abd El-Fattah I. Helal, Former Vice Chairman of Atomic Energy Authority,
and Professor Dr. Nagwa F. Zahran, Former Vice Chairman of Atomic
Energy Authority, for their great efforts for suggesting and supervising this
work and also for their valuable guidance and illuminating discussions.

I would like to express my gratitude and appreciation to Ass. Prof. Dr.
Sayed Ahmed Abd Elaziz Shama, Ass. Prof. of Analytical chemistry,
Faculty of Science, Banha University, for his support during the work,
encouragement, sponsorship and effective supervision along the work.

I would like to express my deep thanks to Dr. Ramadan Mohammed
Abd Elwahed, Central Laboratory for Elemental and Isotopic Analysis,
Nuclear Research Center, Atomic Energy Authority, for his great help during
the execution of this work.

Many thanks to my colleagues and co-workers in the Central
Laboratory for Elemental and Isotopic Analysis, Nuclear Research Center,
Atomic Energy Authority, for their generous helps.

Special thanks to my parent and my Wife for their encouragement,
support and their efforts to me.
LIST OF TABLES

LIST OF TABLES

Table Title Page
(1-1) Some inorganic and organic species of selenium compounds. 3
(2-1) Properties of common flames 32
(2-2) Literate citation on interferences by other hydride-forming 45
elements in the determination of selenium in a QTA. The
tolerance limit is defined as the reduction of the absorbance
(peak height) by 10% in the presence of the interferent.
(3-1) The power-setting program 58
(3-2) The operating parameters for the HG-AAS. 60
(4-1) 74
Major and minor elements concentration (%) in toenail
samples using XRF and EDX spectrometers.
(4-2) Sample Location 76
(4-3) 77
digestion program for toenails samples in the microwave
system

(4-4) 80
Trace elements concentrations in mg/L in underground water
samples.
(4-5) Trace Elements concentration in (mg/L) in soil samples. 81
(4–6) 86
Distribution Coefficients for different elements in different
samples
(4-7) 89
Trace Elements concentration in (mg/L) in Toenails samples.
LIST OF TABLES
(4-8) Analytical figures of merit for Se(IV) determination 92
(4-9) Concentration in (ng/mL) of Different Selenium Species in 93
Different Samples
(4-10) 98
Concentration of selenium (mg/L) in different toenails
samples using INAA (Solid samples) and AAS (liquid
samples)
LIST OF FIGURES

LIST OF FIGURES

Figure Title Page
(2-1) Interpretation of microwave heating program. 21
(2-2) Ratios of ni / nt as a function of the temperatures in K for 25
some elements.
(2-3) 26
Simplified drawing of a basic flame atomic absorption
system
(2-4) Schematic diagram of a hollow- cathode lamp 27
(2-5) Classification of interferences in the hydride-generation 39
technique according to Dedina
(2-6) Schematic of ICP torch. 47
(2-7) Schematic of a Fassel type torch. 47
(2-8) Magnetic Sector analyzer 49
(2-9) Electrostatic analyzer 50
(2-10) The double focusing mass spectrometry. 50
(2-11) Flow diagram for two types of neutron activation methods. 53
(2-12) A well-type scintillation counter. 54
(3-1) Schematic of laboratory microwave unit. 58
(3-2) 61
System and optical Diagram of AAS
(3-3) Nebulizer, mixing chamber and burner. 63