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Determination of Concentration of Heavy Elements in Ghubaysh (Guiera Senegalensis) using X-Ray Technique Rahma Ibrahim Altaybe Ibrahim Postgraduate Diploma in Physics, University of Gezira (2017) B. Sc. Education in Physics and Mathematics, University of Gezira (2014) A Dissertation Submitted to the University of Gezira in Partial Fulfillment of the Requirements for the Award of the Degree of Master of Science in Physics Department of Electronics Engineering Faculty of Engineering and Technology May/ 2021
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Page 1: Rahma Ibrahim Altaybe Ibrahim.pdf

Determination of Concentration of Heavy Elements in

Ghubaysh (Guiera Senegalensis) using X-Ray Technique

Rahma Ibrahim Altaybe Ibrahim

Postgraduate Diploma in Physics, University of Gezira (2017)

B. Sc. Education in Physics and Mathematics, University of Gezira

(2014)

A Dissertation

Submitted to the University of Gezira in Partial Fulfillment of the

Requirements for the Award of the Degree of Master of Science

in

Physics

Department of Electronics Engineering

Faculty of Engineering and Technology

May/ 2021

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ii

Determination of Concentration of Heavy Elements in

Ghubaysh (Guiera Senegalensis) using X-Ray Technique

Rahma Ibrahim Altaybe Ibrahim

Supervision Committee:

Name Position Signature

Dr. Hasabalrasoul Gesmallah Ismail Main supervisor ……………

Prof. Mubarak Dirar Abdullah Co-supervisor ……….…...

Date: May / 2021

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Determination of Concentration of Heavy Elements in

Ghubaysh (Guiera Senegalensis) using X-Ray Technique

Rahma Ibrahim Altaybe Ibrahim

Examination Committee:

Name Position Signature

Dr. Hasabalrasoul Gesmallah Ismail Chairperson ….………..

Dr. Hashim Mohammed Ali Altaieb External Examiner ….………..

Dr. Mortada Mohammed Abdulwahab Internal Examiner .…………..

Date of Examination: 02 /05 / 2021

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iv

Declaration

I hereby declare that this dissertation is my own original work, and

wherever contributions of others are involved. Every effort is made to

indicate this clearly with references and acknowledgment. The result

embodied in this dissertation has not submitted to any other University or

Academic Institution for the award of any scientific degree.

Name : Rahma Ibrahim Altaybe Ibrahim

Signature : ……………………..

Place and Date: El-Hasahisa locality, Gazira State, Sudan

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Dedication

I dedicate my research to:

To my dear Parents Alia AL Safi and Ibrahim Mamon Alhlbawe

To my the spirit of my grandmother, Amna Tidjani

To my dear Uncle M-Haron, Amera, Salwa Zobedi and Azza

To my brothers Nasr Alden, Jmal and Mohammed

To my sisters Alaa, Mawda and Isra Amir

To The people of Abu Zabad, especially El- Tijani Abu family ,

EL-Deif family, Al-siddig Kram, tem work electricity and alhaj

Adm

To everyone who taught me a letter or developed a value inside me

My friends and specially… Israa - Ghada – Roaa - Sara - Riham - Ikram -

Shula - Ahd - Aya - Islam – Shaima – Amena - Hoeam – Doaa – Zohl –

And – Soaad - Rawia and Hiba

To Classmates in various stages, and I specialize in batch "32" in

Mathematics Physics - Faculty of Education, Rafaa - University

of Gezira

To colleagues (Education El- hasahiesa) and specially... Postgraduate Studies Office Dr. Salwa, Dr. Abo maali, Fawzia,

Dr. Abdurazig, Dr. Azza, Dr. M-Bakhet, alrisala and zahra.

The researcher

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Acknowledgements First and foremost, praises and thanks to the God,

the Almighty, for His showers of blessings throughout my

research work to complete the research successfully.

and may the blessings and peace of Allah be upon the most

honored of messengers our master Muhammad and upon all his

family and companions, It is therefore my greatest pleasure to

express my gratitude to them all in this acknowledgement, First

of all, I would like to convey my deepest gratitude to my

supervisors: Dr. Hasabalrasoul Gesmallah Ismail Hamza and

Prof. Mubarak Dirar Abd-alla Yagoub for their generous

guidance, encouragement and support from the start until the end

of my study. My warm gratitude goes to, an engineer: Mohamed

Abdullah Mohamed Noraldeen in Sudan petroleum technical

center (ptc), Special thanks to all the senior staff, Department of

Electronics Engineering and Department of Physics and

Mathematics at Gezira University, and all the teachers' they

taught us all these years.

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Determination of Concentration of Heavy Elements in Ghubaysh

(Guiera Senegalensis) using X-Ray Technique

Rahma Ibrahim Altaybe Ibrahim

Abstract

The X-ray technique is considered one of the most widespread and useful

methods for the determination of presence and quantity of the elements in a given

substance Ghubaysh (Guiera senegalensis) is a flowering plant genus in the family

Combretaceae. is the only species in the genus, found in Tropical Africa in dry areas

from Senegal to Sudan, It is used in folk medicine in the areas of its presence. The aim

of this study is to determine the elements contained in the leaves Ghubaysh and to be

suitable for therapeutic uses in the areas of its presence, using the fluorinated X-ray as

one of the spectrum analysis (X-Met 5000). Collect 10 samples of Ghubaysh (Guiera

senegalensis) bushes from three areas in West Kordofan (Zaklouna, northwest of the

Abu Zabad station transmutation power electricityand Um drouta) in Abu Zabad City.

Measurements were made Ten Ghubaysh samples by using the X-MET5000 device at a

five (5) seconds intervals. The results of reveal that there was a great variation in the

concentration of the studied elements (Fe, W, Cr, Ni, Cu, Zn, Pb, Mn, Mo, V, Ti, Co,

Nb) in the study areas. the highest concentration was that of iron (Fe). It ranges between

(0.45 mg/g) in Zaklouna and (86.21 mg/g) in Um drouta, depending on the nature of the

geographical location and the human activities spread throughout the study area. While

there was no concentration recorded for the elements in six samples in three areas

studied there elements was (Pb, Zn, Ti, Co, Nb). In there are other four samples studied

areas, the highest concentration was that of lead (Pb) Which ranges between (1.25

mg/g) in Zaklouna and (0.08 mg/g) in Um drouta, And the concentration of Zinc (Zn)

ranged between (0.43 mg/g) in Zaklouna and (0.01 mg/g) in Um drouta, The

concentration of Titanium (Ti) was (0.11 mg/g), and that of Cobalt (Co) was (0.90

mg/g), and that of Niobium (Nb) was (0.25 mg/g), The study confirms that the plant

has not degree of toxicity and it is safe to be used medicinally. This study recommends

that further studies be made spectrophotometeorically to confirm the safe use of plant.

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تقنية األشعة بإستخدام (Guiera Senegalensis)تركيز العناصر الثقيلة في الغبيش تحديد

السينية.

رحوة إبراهين الطيب إبراهين

هلخص الدراسة

ذعرثش ذمح األشعح انسح احذج ي أكصش انطشق ارشاسا فائذج نرحذذ ظد كح

ثاخ انغثش ثاخ ي عائهح انكيثشراخ انع انحذ ف انعاصش ف يادج يعح،

، سرخذو ف انعس، انظد ف إفشما االسرائح ف اناطك انعافح ي انسغال إن انسدا

ثاخ . ذفد انذساسح نهرعشف عه انعاصش انظدج ف أساق طة انشعث ف ياطك ذاظذان

فهسج كأحذ طشق ذحهم رتاسرخذاو األشعح انسح ان انعالظح نالسرخذاياخكا صانحح انغثش

( siu0e G0e0s a0eGuGعاخ ي شعشاخ انغثش ) 10ذى ظع ، (X-0005 5000انطف )

أو دسذح( ، ي شالز ياطك ف الح غشب كشدفا )صلهح، شال غشب يحطح كشتاء أت صتذ

ف لد خسح XMET5000تذح أت صتذ. ذى إظشاء انماساخ نعشش عاخ تاسرخذاو ظاص

ف كم يشج. ذصهد انذساسح إن عذج رائط أا: ذثاا كثشا ف ذشكض انعاصش ظدشا

ف ياطك (Fe،W ،Cr ،Ni ،Cu ،Zn ،Pb، Mn ،Mo، V ،Ti ،Co ،Nbنذسسح )ا

يم/ض( ف صلها 0.45يا ت ) ذشكض( تهغ Feحس كا أعه ذشكض نعصش انحذذ ) ،انذساسح

رنك حسة طثعح انلع انعغشاف انفعاناخ انثششح انرششج ف أو دسذ، يم/ض( 16.21 )

، تا نى كأاع األشعاس انراظذج ف انشع تعذا ع انهشاخ انذساسحعه طل يطمح

ف ف سرح عاخ تا سعها ( Zn ،Pb ،Ti ،Co ،Nbسعم انعاص أ ذشكض نعاصش )

ف صلها ( يم/ض1.25)( ف انذ يا ت pbأعه ذشكض نعصش انشصاص )كا أستعح ياطك

ف صلها ( يم/ض0.43)( ف انذ يا ت Zn، انضك )ف أو دسذ ض(يم/0.01 )

( كا Coيم/ض(، انكتاند )0.11كا ) (Ti، ذشكض انرراو )يم/ض( ف أو دسذ0.01)

ؤكذ أ انثاخ نس ن دسظح سح أ يم/ض(، يا 0.25كا ) (Nb) انتويم/ض(، 5..0)

نهثاذاخ انطف انضئ يماسع تانكشفذص انذساسح . طثا اسرخذاييضاس عذ

نرشتح ظزس ساق انطمح نرحذذ انضاس انفائذ، دساسح انعاصش انصمهح انظدج ف ذهك

يماسح ت انرشاكض نرحذذ أا أفذ نالسرخذاو. تزس انثاخ يع عم

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Table of Contents

No Subject Page

1 Declaration IV

2 Dedication V

3 Acknowledgment VI

4 Abstract English VII

5 Abstract Arabic VIII

6 Table of Contents IX

7 List of Tables XII

8 List of Figures XIII

CHAPTER ONE: Introduction

1.1 Overview 1

1.2 Research Problem 2

1.3 Aim of the Work 2

1.4 Materials and Method 2

1.5 Lay out of Thesis 3

CHAPTER TWO: Literature Review

2.1 Introduction 4

2.2 Physics of X-Rays 4

2.3 Generation and Properties of X-Rays 5

2.4 Electromagnetic Radiation 5

2.5 Properties of X-Rays 8

2.6 X-Rays and White Radiation 9

2.7 The Origin of X-Rays 10

2.8 X-ray Sources 11

2.9 Type of X-ray 13

2.10 Soft X-rays 13

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2.11 Hard X-rays 13

2.12 X-ray wavelength and energy scales 14

2.13 Theory of absorption of X-Rays and X-ray Emission Spectroscopy 14

2.14 The Continuous Spectrum 16

2.15 Discrete Spectrum 17

2.16 X - Ray machine and its uses 17

2.17 Digital X-Ray 18

2.18 Uses of the X – Ray 19

2.19 X-ray absorption spectroscopy (XAS) 19

2.20 X-Ray Detection 20

2.21 History of X-Ray Fluorescence 20

2.22 X-Ray Fluorescence 21

2.23 Guiera senegalensis (Ghubaysh) plant 21

2.23.1 Family 21

2.23.2 Local Names 21

2.23.3 Description 22

2.23.4 Ecology 22

2.24 Elements of Interest 22

2.25 The Individual Elements 22

2.25.1 Iron (Fe) 22

2.25.2 Lead (Pb) 24

2.25.3 Manganese (Mn) 27

2.25.4 Chromium (Cr) 29

2.25.5 Nickel (Ni) 32

2.25.6 Zinc (Zn) 34

2.25.7 Molybdenum (Mo) 35

2.25.8 Copper (Cu) 36

2.25.9 Tungsten (W) 36

2.25.10 Vanadium (V) 37

2.25.11 Titanium (Ti) 37

2.25.12 Cobalt (Co) 37

2.25.13 Niobium (Nb) 38

2.26 Previous studies: 38

2.26.1 Ethno botanical survey and phytochemical studies of Guiera senegalensis Lam.

In mubi local Government of Adamawa State

38

2.26.2 Guiera senegalensis (Gs) is a well-known traditional medicinal plant in Africa 39

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2.26.3 Introduction: Guiera senegalensis J. F. Gmel 39

2.26.4 Phytochemical and pharmacological study of roots and leaves of Guiera

senegalensis J.F. Gmel (Combretaceae)

40

CHAPTER THREE: Materials and Methods

3.1 Introduction 41

3.2 Material 41

3.3 Study area 42

3.3.1 Description of the study area 42

3.3.2 Location map of the Study 42

3.4 The method of work 42

3.4.1 The first step 42

3.4.2 The second step: X-MET5000 43

3.5 Description X-MET5000 43

3.5.1 High Speed on-site Measurement 45

3.5.2 Rugged and Reliable tool for analysis 45

3.5.3 High Performance 45

3.6 Sample Preparation 46

CHAPTER FOUR: Results and Discussion

4.1 Introduction 47

4.2 Results 47

4.3 Discussion 57

CHAPTER FIVE: Conclusions and Recommendations

5.1 Conclusion 59

5.2 Recommendations 60

References 61

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List of Tables

No Table Page

2.1 Energy and names of various wavelength range 7

4.2.1 The concentration of elements in the sample (A1) 47

4.2.2 The concentration of elements in the sample (A2) 48

4.2.3 The concentration of elements in the sample (A3) 49

4.2.4 The concentration of elements in the sample (A4) 50

4.2.5 The concentration of elements in the sample (A5) 51

4.2.6 The concentration of elements in the sample (A6) 52

4.2.7 The concentration of elements in the sample (A7) 53

4.2.8 The concentration of elements in the sample (A8) 54

4.2.9 The concentration of elements in the sample (A9) 55

4.2.10 The concentration of elements in the sample (A10) 56

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List of Figures

No Figures Page

2.1 The electromagnetic spectrum. The boundaries between regions are arbitrary, since

no sharp upper or lower limits can be assigned. (B.D. Cullity S.R. Stock, 2014)

6

2.2 Schematic diagram of a sealed crystallographic X-ray tube. The target anode is

provided with a means of rotation, so as to aid the dissipation of heat generated by

the electron impact on the target and to prolong the life of the target

9

2.3 Variation of intensity with wavelength for an X-ray tube, for three different

operating voltages; as V increases, the maximum wavelength in the continuous

spectrum moves to shorter wavelengths

10

2.4 A pictorial representation of X-ray using a generic atom and generic energy levels.

This picture uses the Bohr model of atomic structure and is not to scale.

11

2.5 Principle of the X-ray tube 12

2.6 Variation with wavelength of the linear absorption coefficient m for nickel; the

discontinuity at approximately 1.4886 A ° corresponds with the L absorption edge

of the element

16

3.1 Guiera senegalensis in Abu Zabad locality of Western Kordufan, Sudan. 41

3.2 Location map of the study area 42

3.3 The leaves and then dried at room temperature for a few days to ensure complete

dryness and stored in plastic boxes illustrated in Abu Zabad City

42

3.4 X-MET5000 45

3.5 Color touch screen display visible 45

3.6 Element ranges of X- Met 5000 and X- Met 5100

(Oxford instrument, 2009

46

3.7 X-MET5000 46

4.1 The concentration of the sample (A1) 47

4.2 The concentration of the sample (A2) 48

4.3 The concentration of the sample (A3) 49

4.4 The concentration of the sample (A4) 50

4.5 The concentration of the sample (A5) 51

4.6 The concentration of the sample (A6) 52

4.7 The concentration of the sample (A7) 53

4.8 The concentration of the sample (A8) 54

4.9 The concentration of the sample (A9) 55

4.10 The concentration of the sample (A10) 56

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CHAPTER ONE CHAPTER ONE

INTRODUCTION

1.1 Overview

Plants are the backbone of all life on earth and essential resource for human

well-being. Through photosynthesis, plant provide all the food we eat which comes to

us either directly or indirectly, air (oxygen) is brought by plants, as a byproduct of

photosynthesis(Abubaker et al,2000). Several traditional medicinal plants, including

Guiera senegalensis (Gs), a shrub that grows well in sub-Saharan Africa and Sudan

(Hill, 1952), have been candidates for research because of their perceived medicinal

properties. Evaluation of compounds such as, tannins, alkaloids, flavonoids saponins,

terpenoids and phenols have been used as a method of screening of medicinal plants

(Sule and Mohammed, 2006). Guiera Senegalensis has been used in Western

Kourdofan of Sudan and elsewhere in traditional medicine as a cure for infections and

wounds (Alshafei et al, 2016; El-Gazali et al, 1994) In the Sudan, Guiera Senegalensis

is locally known as Ghubaysh of which the leaves extract and the roots powder are used

for treatment of a variety and diseases and wounds, respectively. In a companion paper

(El-Gazali et al, 1994). Guiera Senegalensis, very well known in its native area,

generally occurs as a shrub that can grow to a height of 3 to 5 m according to habitat. Its

stem presents numerous knots that send out branches. The ash-grey stem and branches

have fibrous or pubescent bark and bear opposing, short petiolated oval leaves,

sometimes mucronate, sometimes even cordate at their base, about 2 to 4 cm long by 1

to 2 cm wide. These grey-green leaves, darker on their upper surface, display black

spots on their lower surface and are slightly downy on both sides. These features lend

the plant an overall silver green colour that is conspicuous in brush land (Silva et

al,2008). Flowering occurs almost throughout the year, when it is leafy. Often blooms

twice a year, during the dry season and the rainy season. Each flower has a calcinal tube

ovoid, welded to the ovary. This tube is topped by a bellflower blade with 5 teeth

screened black and persistent points to fruiting. The stamens are 10 on two rows of 5,

all inserted on the calyx. The ovary has a single box containing 4 to 6 eggs (Koumaré ,

1986).

X-rays with energies ranging from about 100 eV to 10MeV are classified as

electromagnetic waves, which are only different from the radio waves, light, and

gamma rays in wavelength and energy. X-rays show wave nature with wavelength

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ranging from about 10 to 10-3

nm. According to the quantum theory, the

electromagnetic wave can be treated as particles called photons or light quanta. The

essential characteristics of photons such as energy, momentum, e tc.( Yoshio Waseda et

al,2011)

The heavy elements and there isotopes are mainly produced by thes process and

ther process and to less extent by the p-process. They trace back the chemical evolution

of the galaxy, thus they represent alink to the lowred shift universe (Mounib, 2018).

1.2 Research problem

Recently chemical drugs are known to have severe side effects. Several bacteria and

other organizims that cause human diseases, show resistance to chemical drugs. This

requires knowing the effective ingredients of natural herbs. One of them is guier

senegalensis.

Highlighting the importance of Sudanese plants in general and those of western

Sudan, especially Guiera Senegalensis (Ghubaysh) plant needs very sensitive new

techniques.

1.3 Aim of the Work

This study aims at using the fluorinated X-ray as one of the spectrum analysis to

measure concentration of heavy elements in Guiera senegalensis (Ghubaysh) natural

plants used in the Traditional medicine in the western Sudan.

To determination of characteristics that could be a reference to the researchers and

showing the importance of this plant to be used in a wider range around the world

and heavy elements of extract of Guiera Senegalensis, using the fluorinated X-ray as

one of the spectrum analysis (X-Meet 5000).

These elements obtained show the effective ingredients that exist in this herb and

comparing it to the permissible and internationally agreed limits.

1.4 Materials and Method

Collect 10 samples of Guiera senegalensis (Ghubaysh) bushes from three areas in West

Kordofan (Zaklouna, northwest of the Abu Dhabid power station and Um drouta ) in

Abu Zabad locality. Some samples of the plant.

Measurements were made for leaves Guiera Senegalensis (Ghubaysh) samples in the

X-ray spectrometer by using the X-MET5000.

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1.5 Lay out of thesis

This is research include five chapters. Chapter one is the introduction, while chapter two

is the background and literature review while chapter three is concerned with material

and methods. Chapter four is devoted for results and discussion and chapter five is

conclusion and recommendation.

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CHAPTER TWO

LITERATURE REVIEW

2.1 Introduction

This chapter consists of the theoretical background of Physics of X-Rays, the

X-Ray Fluorescence, Guiera senegalensis (Ghubaysh) plant, the Elements of Interest

and previous studies.

2.2 Physics of X-Rays

The discovery of X-rays by Wilhelm Röntgen in 1885 opened a whole new field

of research that quickly sparked numerous applications that nowadays are indispensable

in many fields like medical diagnostics, industrial quality control or security. X-rays

penetrate matter much better than visible light and can be used to get an image of the

inside of samples without the need for mechanical slicing or opening. For the most part,

today’s imaging systems use the same experimental setup that Röntgen used in his

laboratory: a source, based on accelerated electrons hitting a target, emits X-rays which

then travel through the sample and are detected in a plane downstream. Image contrast

is created by the absorption of photons in the sample and the resulting local intensity

decrease on the detector. This yields excellent results when large differences in

absorption coefficients are present in the sample, like bones in soft tissue. When little

absorption is present, e.g. in very thin structures or material composed of light elements,

the achieved contrast is limited. Materials with similar absorption coefficients are

hardly distinguished in X-ray radiography; this is a major drawback especially in

medical imaging, because the tissue that forms the inner organs, muscles and body fat is

mainly composed of light elements and there is little difference in the absorption

coefficients of different tissue types. This limitation can be overcome when using not

the absorption, but the phase shift that X-rays undergo inside the sample. Both

properties are described by the complex refractive index , where δ describes

the phase shift and β the absorption. For light materials, δ can be three orders of

magnitude larger than β, which means that a strong phase signal can be present even in

cases of very faint absorption. (Ismail 2019; Frieder Johannes Koch, 2017)

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2.3 Generation and Properties of X-Rays

X-rays are an electromagnetic radiation of short wavelength, and can be

produced by the sudden deceleration of rapidly moving electrons at a target material. If

an electron falls through a potential difference of V volt, it acquires an energy eV

electron-volt (eV), where e is the charge on an electron. This energy may be expressed

as quanta of X-rays of wavelength λ, where each quantum is given by

eVhc (2.1)

h being the Planck constant and c the speed of light in vacuum. Substitution of

numerical values into (2.1) leads to

V4.12 (2.2)

Where V is measured in kilovolt and l is given in Angstrom units (A°). The wavelength

range of X-rays is approximately 0.1–100A°, but for the purposes of practical X-ray

crystallography, the range used is restricted to 0.7–2.5 A°.( Ismail 2019; Mark Ladd

Rex Palmer ,2013)

Since x-rays are produced whenever high-speed electrons collide with a metal

target, any x-ray tube must contain (a) a source of electrons, (b) a high accelerating

voltage, and (c) a metal target. Furthermore, since most of the kinetic energy of the

electrons is converted into heat in the target, the latter is almost always water cooled to

prevent its melting.

All x-ray tubes contain two electrodes, an anode (the metal target) maintained, with few

exceptions, at ground potential, and a cathode, maintained at a high negative potential,

normally of the order of 30,000 to 50,000 volts for diffraction work. X-ray tubes may be

divided into two basic types, according to the way in which electrons are provided: gas

tubes, in which electrons are produced by the ionization of a small quantity of gas

(residual air in a partly evacuated tube), and filament tubes, in which the source of

electrons is a hot filament. (Ismail 2019; B.D. Cullity S.R. Stock, 2014)

2.4 Electromagnetic Radiation

X-rays are electromagnetic radiation of exactly the same nature as light but of

very much shorter wavelength. The unit of measurement in the x-ray region is the

angstrom (Å), equal to 10-10 m, and x-rays used in diffraction have wavelengths lying

approximately in the range 0.5-2.5 Å, whereas the wavelength of visible light is of the

order of 6000 Å. X-rays therefore occupy the region between gamma and ultraviolet

rays in the complete electromagnetic spectrum(Fig2. 1). Other units sometimes used to

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measure x-ray wavelength are the X unit (XU) and the kilo X unit (kX = 1000 XU). The

kX unit, whose origin will be described in Sec. 3-7, is only slightly larger than the

angstrom. The approved SI unit for wavelengths in the x-ray region is the nanometer:

1 nanometer = 10-9 m = 10 Å.

This unit has not become popular in x-ray diffraction.

Figure :(2.1) The electromagnetic spectrum. The boundaries between regions are

arbitrary, since no sharp upper or lower limits can be assigned. (Cullity, Stock et

al, 2014)

Electromagnetic radiation, such as a beam of x-rays, carries energy, and the rate

of flow of this energy through unit area perpendicular to the direction of motion of the

wave is called the intensity I. The average value of the intensity is proportional to the

square of the amplitude of the wave, i.e., proportional to A2. In absolute units, intensity

is measured in joules/m2/sec, but this measurement is a difficult one and is seldom

carried out; most x-ray intensity measurements are made by counting the number of

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photons incident on a detector or by measuring the degree of blackening of

photographic film exposed to the x-ray beam. (Ismail 2019; Cullity et al,2014)

X rays are electromagnetic radiation. All X-rays represent a very energetic

portion of the electromagnetic spectrum and have short wavelengths of about 0.1 to 100

angstroms (Å). They are bounded by ultraviolet light at long wavelengths and gamma

rays at short wavelengths X-rays in the range from 50 to 100 Å are termed soft X-rays

because they have lower energies and are easily absorbed. (Ismail 2019; Moussa

Bounakhla &Mouni Tahri, 2000and Reinhold Schlotz et al,2006).

Table 2.1: Energy and names of various wavelength range.

Energy range (eV) Wave length range Name

<10-7

cm to km Radio Waves (short ,medium, long waves)

<10-3

m to cm Micro Wave

<10-3

m to mm Infra-Red

0.0017 - 0.0033 380 to 750nm Visible Light

0.033 - 0.1 10 to 380nm Ultra violet

0.11 - 100 0.01 to 12 nm X-rays

10 - 5000 0.0002 to 0.12nm Gamma Radiation

The range of interest for X-ray is approximately from 0.1 to 100 Å. Although,

angstroms are used throughout these notes, they are not accepted as SI unit.

Wavelengths should be expressed in nanometers (nm), which are 10-9

meters (1 Å = 10-

10 m), but most texts and articles on microprobe analysis retain the use of the angstroms.

Another commonly used unit is the micron, which more correctly should be termed

micrometer (μm); a micrometer is104 Å(Moussa Bounakhla &Mouni Tahri, 2000and

Reinhold Schlotz et al, 2006).

The relationship between the wavelength of electromagnetic radiation and its

corpuscular energy (E) is derived as follows. For all electromagnetic radiation:

E=hv (2.3)

Where:

h is the Planck constant ( sj.62.6 1024

).

ν is the frequency expressed in Hertz.

For all wavelengths,

/cv (2.4)

Where:

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8

c = speed of light ( sm /99782.2 108

).

λ= wavelength (Å).

Thus:

/98636.1/ 1024

hcE (2.5)

Where E is in Joule and λ in meters.

The conversion to angstroms and electron volts ( jouleeV 1019

602.11 ) yields the

Duane-Hunt equation:

)/(396.12)(0

AeVE (2.6)

Note the inversion relationship. Short wavelengths correspond to high energies

and long wavelengths to low energies. Energies for the range of X-ray wavelengths are

124 k eV (0.1Å) to 124 eV (100 Å). The magnitudes of X-ray energies suggested to

early workers that X-rays are produced from within an atom. Those produced from a

material consist of two distinct superimposed components: continuum (or white)

radiation, which has a continuous distribution of intensities over all wavelengths, and

characteristic radiation, which occurs as a peak of variable intensity at discrete

wavelengths (Moussa and Mouni 2000).

2.5 Properties of X-Rays

A general summary of the properties of X-rays is presented below:

Invisible;

Propagate with velocity of light (3.108 m/s).

Unaffected by electrical and magnetic fields;

Differentially absorbed in passing through matter of varying composition,

density and thickness;

Reflected, diffracted, refracted and polarized;

Capable of ionizing gases;

Capable of affecting electrical properties of solids and liquids;

Capable of blackening a photographic plate;

Able to liberate photoelectron. And recoils electrons;

Emitted in a continuous spectrum;

Emitted also with a line spectrum characteristic of the chemical element;

Found to have absorption spectra characteristic of the chemical element X-Rays

and White Radiation

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9

2.6 X-Rays and White Radiation

Except for synchrotron radiation, a widely used source of X-rays in conventional

crystallography laboratories is the sealed hot-cathode tube with a rotating anode,

illustrated diagrammatically. Electrons are emitted from a heated tungsten filament, the

cathode, and accelerated by a high voltage, 40 kV or more, towards a water-cooled

target anode, usually made of copper or molybdenum. A large proportion of the energy

reaching the target is dissipated as heat on account of multiple collisions within the

target material, but about 10% of it is converted usefully for X-ray crystallographic

purposes. In order to dissipate the heat rapidly and efficiently, the water-cooled anode is

rotated, as indicated in the diagram of Fig. 2.2.

Fig (2.2) Schematic diagram of a sealed crystallographic X-ray tube. The target

anode is provided with a means of rotation, so as to aid the dissipation of heat

generated by the electron impact on the target and to prolong the life of the target

As a consequence, a higher accelerating voltage can be applied to the tube,

which results in a more powerful X-ray source. If the energy eV is not too high, there

will be a continuous distribution of X-ray wavelengths, ―white‖ radiation, or

Bremsstrahlung (Ger. ¼ braking radiation), as shown in Fig. 2.3. With an increase in the

accelerating voltage V, the intensity of the radiation increases, and the maximum of the

curve moves to shorter wavelengths. (Ismail 2019, Mark Ladd • Rex Palmer et al,

2013)

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10

Fig (2.3) Variation of intensity with wavelength for an X-ray tube, for three

different operating voltages; as V increases, the maximum wavelength in the

continuous spectrum moves to shorter wavelengths, in accordance with (2.2)

2.7 The Origin of X-Rays

An electron can be ejected from its atomic orbital by the absorption of a light

wave (Photon) of sufficient energy. The energy of the photon (hν) must be greater than

the energy with which the electron is bound to the nucleus of the atom. When an inner

orbital electron is ejected from an atom, an electron from a higher energy level orbital

will transfer into the vacant lower energy orbital (Figure 2.4). During this transition a

photon may be emitted from the atom. To understand the processes in the atomic shell,

we must take a look at the Bohr's atomic model.

The energy of the emitted photon will be equal to the difference in energies

between the two orbitals occupied by the electron making the transition. Due to the fact

that the energy difference between two specific orbital shells, in a given element, is

always the same (i.e., characteristic of a particular element), the photon emitted when an

electron moves between these two levels will always have the same energy. Therefore,

by determining the energy (wavelength) of the X-ray light (photons) emitted by a

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11

particular element, it is possible to determine the identity of that element. (Moussa and

Mounia, 2008)

Figure (2.4): A pictorial representation of X-ray using a generic atom and generic

energy levels. This picture uses the Bohr model of atomic structure and is not to

scale.

2.8 X-ray sources

In most applications today, X-rays are produced using a principle very similar to

what Röntgen used for his experiments. Electrons emitted from a cathode in an

evacuated tube are accelerated in an electric field with a potential difference between a

few and hundreds of kilovolt, and directed to a target, usually made out of a metal such

as Copper, Molybdenum or Tungsten. Shows a schematic depiction of the principle.

Fig (2.5): Principle of the X-ray tube

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The accelerated electrons lose their kinetic energy mainly in two ways: Hitting electrons

in the target material and transferring momentum to them, and decelerating in the field

of an atomic nucleus. Both processes lead to the emission of X-rays. When an

accelerated electron liberates an electron from the inner shell of a target atom, this void

is filled with electrons from outer shells, and the energy difference between the two

states is either radiated as an X-ray photon or transferred to another electron which is

then liberated from the atom (Auger electrons). The difference of potential energies

between the states of an atom, and therefore the energy of the emitted photon, is

characteristic of the chemical element of the target. The second process, the deceleration

in the electric field of the nucleus, is mostly governed by the initial energy of the

electron. An accelerated or decelerated electric charge emits electromagnetic radiation

called Bremsstrahlung. The photon energy corresponds to the amount of energy lost; the

highest possible photon energy is therefore identical to the initial kinetic energy of the

electron. The spectrum created by this process is continuous; the X-ray emission from

these so-called tube sources is therefore polychromatic and highly dependent on the

target material and acceleration voltage.

The output of a tube source is a cone beam. Apart from the radiation produced in the

deceleration of electrons in the target material, a lot of heat is created, which limits the

output intensity of a tube source. Several approaches exist to overcome this problem, a

very important step forward was the introduction of the rotating anode principle, in

which a constant rotational movement of the anode distributes the heat load over a

larger area in the target and facilitates cooling. These rotating anode tubes allow much

higher output power; modern devices achieve around 100 kW with a source size of

about 1 mm², see e.g. reference.

High resolution X-ray imaging requires small source sizes, and electron focusing optics

are used in so-called micro focus tubes to narrow the impact zone on the target to a spot

of only a few micrometers in diameter. With decreasing focal spot size, the local heat

load increases, which in practice means that conventional micro focus tubes have a

limited output power. A more recent approach replaces the solid target material with a

liquid metal jet, which allows a substantial increase of the brilliance. Synchrotrons and

storage rings Synchrotrons are large particle accelerators that use a series of bending

and focusing magnets to put a charged particle on a closed trajectory. Radio frequency

electric fields are used to accelerate the particles, and upon gaining energy, the fields in

the bending magnets have to be ramped up synchronously (hence the name) in order to

keep the particle trajectory constant.(Frieder,2017)

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13

The change of direction in a magnetic field is an acceleration of the charged

particle and thus gives rise to the emission of electromagnetic radiation. With electrons

at relativistic speed, this effect provides the possibility to create intense X-ray beams

that are called synchrotron radiation. The ANKA (Ångströmquelle Karlsruhe)

synchrotron in Karlsruhe is an example for an accelerator specifically built to create

synchrotron radiation; other examples are the European Synchrotron Radiation Facility

(ESRF) in France, Spring-8 in Japan or the Advanced Photon Source in the USA. The

radiation used for experiments at these facilities is referred to as synchrotron radiation

for historical reasons, although it is usually not produced in a synchrotron, but in a

storage ring. Storage rings have a similar layout as synchrotrons, but operate at constant

energy and thus require acceleration of the particle to the final energy prior to injection,

which is usually done with a series of linear acceleration and a booster synchrotron.

(Ismail 2019 and Koch ,2017)

2.9 Type of X-ray

There are two types of X-rays, according to their photon energy. The photon energy is

given by the formula E = hν where E is the energy in Joules, h is Planck's constant and

ν is the frequency of the photon. The frequency of the photon (ν) can also be obtained

from the equation c = λν where c is the speed of light (~3.0 × 108 m/s) and λ is the

photon's wavelength. Because Planck's constant is small ( ~6.62 × 10-34

Joule-seconds),

it is typically more convenient to work in electron-Volts (eV) where one eV is about

1.602 × 10-19

Joule. For example, visible light photons with wavelengths between

700nm and 400nm have energies between 1.77 eV and 3.1 eV respectively (Mitr,

Sarah et al, 2012).

2.10 Soft X-rays

These x-rays are defined by having photon energies below 10keV. They have less

energy than the hard x-rays, therefore they have longer wavelength. Soft X-rays are

used in radiography to take pictures of bones and internal organs. Because of their lower

energy, they do not cause much damage to tissues, unless they are repeated too often

(Roobottom CA, et al, 2010).

2.11 Hard X-rays

Hard X-rays have photon energies above 10 KeVThey have shorter wavelength than the

soft x-rays. These X-rays are used in radiotherapy, a treatment for cancer. Due to their

higher energy, they destroy molecules within specific cells, thus destroying tissue.

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14

Another use for these X-rays is in airport security scanners to examine baggage (Hall

and Brenner et al, 2008).

2.12 X-ray wavelength and energy scales

The X-ray or Röntgen region of the electromagnetic spectrum starts at ca. 10 nm

and extends towards the shorter wavelengths. The energies of X-ray photons are of the

same order of magnitude as the binding levels of inner shell electrons (K, L, M …

levels) and therefore can be used to excite and/or probe these atomic levels. The

wavelength λ of an X-ray photon is inversely related to its energy E according to:

)(/24.1)( KeVEnm (2.7)

Where 1 eV is the kinetic energy of an electron that has been accelerated over a voltage

difference of 1 V (1eV = 1.602 10-19 J). Accordingly, the X-ray energy range starts at

100 eV and continues towards higher energies. X-ray analysis methods most commonly

employ radiation in the 1-50 keV (1 - 0.02 nm) range (G. Gauglitz.etal, 2003 and

Reinhold Schlotz et al ,2006).

2.13 Theory of absorption of X-Rays and X-ray Emission Spectroscopy

X-ray spectroscopic techniques such as X-ray photoelectron spectroscopy

(XPS), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), small

angle X-ray scattering (SAXS), X-ray emission spectroscopy (XES), and X-ray

absorption spectroscopy are available, each with different advantages and

disadvantages. The focus of this thesis will be onto XAS and the related XES as well as

onto combinations of those two, the resonant inelastic X-ray scattering (RIXS) and

variations thereof. To perform valuable X-ray spectroscopic experiments an intense and

tunable X-ray source is indispensable, which leads to the need for synchrotron radiation

sources that are by now available all over the world. The electrons inside the

synchrotron ring are forced to travel with constant velocity and on a circular trajectory

for what reason they emit X-rays. These X-rays are - depending on the synchrotron ring

- within the energy range from 0.1 to 100 keV, i.e. wavelength from 100 down to 0.1 Å,

almost covering the hole range of atomic core level binding energies and interatomic

distances, respectively. (Timna-Josua Kühn ,2011)

All materials absorb X-rays, and the transmitted intensity is attenuated according

to an exponential law:

)exp(0 tII (2.8)

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15

I0 and I are, respectively, the incident and transmitted intensities; m is the linear

absorption coefficient of the material, and t is the path length for X-rays through the

material.

Here, the proportional factor µ is called linear absorption coefficient, which is

dependent on the wavelength of X-rays, the physical state (gas, liquid, and solid) or

density of the substance, and its unit is usually inverse of distance. However, since the

linear absorption coefficient µ proportional to density, (µ /) becomes unique value of

the substance, independent upon the state of the substance. The quantity of (µ /) is

called the mass absorption coefficient and the specific values for characteristic X-rays

frequently-used are compiled. Equation (2.8) can be re-written as (2.9) in terms of the

mass absorption coefficient.

xII )(exp0 (2.9)

Mass absorption coefficient of the sample of interest containing two or more

elements can be estimated from (2.10) using the bulk density, and weight ratio of wj

for each element j. (Yoshio Waseda et al, 2011)

jj

jwww

12

2

1

1 ... (2.10)

The absorption of X-rays increases with the atomic numbers of the elements in

the absorbing material. The variation of m with wavelength is illustrated in Fig. 2.6,

which refers to elemental nickel. The absorption coefficient m of any material decreases

approximately as λ5/2

, so that as l falls, the energy of the radiation (hc/λ) becomes

greater and more penetrating. With continuing decrease in wavelength, a position is

reached where the energy of the radiation is sufficient to eject an electron from the L

energy level of an atom of the material. At this point, known as the absorption edge, or

resonance level, the value of µ is greatly enhanced. As the wavelength decreases

further, the absorption coefficient continues to fall off as before. In the case of nickel,

this particular L absorption edge occurs at a wavelength of 1.4886 A°. Absorption edges

are important in selecting the correct radiation for a particular application. For example,

copper X-radiation would be unsuitable for materials containing a high percentage of

iron. The K absorption edge for iron is 1.7433 A°, so that radiation of this wavelength

would be strongly absorbed by the iron moiety and subsequently re-emitted as the

characteristic K spectrum of iron.

In such a case, molybdenum radiation, λ(Kα) = 0.71073 A ° , would be a

satisfactory alternative. (Mark Ladd • Rex Palmer ,2013)

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Fig (2.6) Variation with wavelength of the linear absorption coefficient m for

nickel; the discontinuity at approximately 1.4886 A ° corresponds with the L

absorption edge of the element

2.14 The Continuous Spectrum

The largest number of electrons colliding with the target of the x-ray tube does

not experience head-on collision collisions with the target atoms. Rather, they are

involved in partial collisions resulting in the loss of a portion of the kinetic energy of

these electrons, resulting in a slow sluggish movement. The energy pulse of the X-ray

and the energy bond appear as heat. Kramer's Equation:

)( EEKZI mE (2.11)

Where IE is the density of photons with energy E, Z Atomic number of target material,

Em is the maximum energy of the electron, K static.

The maximum potential of the bremsstrahlung photon is the falling photon energy.

Kilo-electron Volt (KeV) is the equivalent of the applied voltage Kilovolts peak (KVp)

but the density of these photons is zero, as derived from the previous equation, i.e. IE =

0 when E = Em (Ismail 2019).

The unfiltered energy spectrum is clearly modified whenever photons experience self-

filtering (absorption from the target, tube wall glass or glass prelim window). The

Inherent Filter in the normal X-ray tube is often equivalent to about 0.5-1 mm of

aluminum. Filtering adds additional spectrum adjustments. This filtering affects low-

energy photons but has little impact on the high-energy photons of the spectrum.

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The purpose of this filter is to increase the number of high-energy photons by absorbing

low-energy photons. The higher the filter, the more powerful the beam will be, in the

sense that it reaches a higher medium energy and the penetration force increases. So

adding a filter is one way to improve the penetration capacity of the beam. Another way

is to increase the voltage exerted on the tube. Since the total density of the beam

decreases with increased filtration and increases with voltage, the choice between filter

and voltage applied to the tube must be balanced to obtain reasonable penetration

capacity and acceptable density (Ismail 2019).

The shape of the X-ray energy spectrum is only the result of the alternating voltage

exerted on the tube and the multiple interactions of the braking radiation through the

target material and the filter in the beam. Even if the x-ray tube's power increases with

constant voltage, the X-ray will remain heterogeneous in energy due to multiple braking

processes that produce different energies for the photons.

Because x-rays contain a spectral distribution of energy based on both voltage and

filtering, it is difficult to describe and characterize beam quality in terms of energy,

penetration capacity, or beam strength of Beam Hardening. But generally there are

several philosophies to find an average X-ray energy and can currently accept that they

are approximately two-thirds of the maximum energy or KVp (Aseel aleumr, et al,

2012).

2.15 Discrete Spectrum

A separate spectrum arises from individual interactions with the electron of the

atom, where the falling electron can remove another electron from its orbit. The atom of

one of its electrons can dispose of its energy by firing an X-ray photon by dropping an

electron from another orbit in the existing space (Abdalla Mohamed alzeer, et al,

2015).

2.16 X - Ray machine and its uses

The simplified principle of X-ray device in general. The main part of this device

is the x-ray tube, which is a glass tube, which is a thin metal thread that is heated by an

electric current, where cathode. This heat expels an electron from the surface of the

helipad. While the elevator is the positively charged .tungsten is a flat disk of tungsten

(Ismail 2019, mohammed saleh metwally, et al, 2015).

A high voltage difference between the elevator and the airstrip is applied. The

electrons extracted from the helipad move at a high speed towards the elevator. When

an electron strikes a tungsten atom on the elevator, it releases an electron with a low

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18

energy level from that atom. This electron replaces another electron of the same atom,

this process results in the release of excess energy in the shape of a high-energy photon,

an X-ray photon. Free electrons can generate photons without colliding atoms. The

nuclei of the atoms can attract the accelerated electrons as they cause the electrons to

slow down and change their paths. Thus, the electron emits at this surplus state its

energy in the form of x-ray photons.

The collision of the electrons in the elevator results in high heat, so a motor is used to

rotate the elevator and protect it from fusion (Mohammed saleh metwally, et al, 2015).

The internal structure of the x-ray tube is surrounded by a thick lead film that prevents

x-ray dispersion in different directions. This cover contains a small window that allows

the x-ray photons to emerge in a narrow package through a series of filters. Before

falling on the patient's body on the other side of the patient's body is an X-ray camera

which uses the same technology used in films. But the difference here is that those who

will incite chemical reactions on the film are X-rays and not visible light. In Digital X-

Ray the CDCD we will talk about later uses an electronic sense element instead of films

the regions of the film that have been exposed to large amounts of dark rays appear

between the areas that were less exposed to the rays. This explains why the bones

appear on the film white as they absorbed the falling rays and the rays reach the film

while the soft tissues appear black or gray because the radiation did not absorb and

therefore increased amounts of these rays to the film (Naveed Ahmed,2008).

2.17 Digital X-Ray

The Digital X-Ray is different from conventional x-ray systems with image

capture and processing. These devices do not contain conventional films but have an

electronic display section consisting mainly of a component called CCD or Charge

Couple Device .It is a matrix with a large number of light sensitive elements of about 30

microvolt and its accuracy reaches 1024X 1024 Pixel. The component element is

CCD.To convert the photovoltaic X-ray photons into an electrical signal. These photons

generate an electrical charge on each element of the matrix according to photon energy.

This signal is then manipulated by the computer to obtain an image displayed on the

monitor.

This component is the cornerstone of digital photography, whether it is by conventional

cameras or medical imaging the CCD element (Ismail 2019).

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2.18 Uses of the X - Ray

X-rays are widely used to make radiographic images of bones and internal

organs. Doctors benefit from radiotherapy in detecting anomalies and diseases, such as

broken bones or lung diseases, inside the patient's body. Dentists use x-rays to detect

empty spaces and teeth (Ismail 2019).

2.19 X-ray absorption spectroscopy (XAS)

XAS is a widely-used technique for determining the local geometric and

electronic structure of matter. It is applicable to any states of matter, i.e. solid, liquid or

gaseous, as no particular long range order is necessary. It is element-specific, since the

X-ray energy is tunable to an arbitrary edge of the element of interest. XAS is used in

very different scientific fields including molecular and condensed matter physics,

materials science and engineering, chemistry, earth science, and biology. The strong

sensitivity to first neighbors makes XAS the tool of choice, in particular, for

coordination chemistry and chemistry of catalysts and other nanostructures.

In a XAS experiment the X-ray energy is tuned by using a crystal

monochromatic through an edge of the element of interest of the to be investigated

material. These edges, arising from the ejection of deep bound core electrons, are

labelled K, L, M, etc., which corresponds to the principal quantum number n = 1, 2, 3,

... of the main electron shell. The respective knocked out electrons are labelled 1s,

2(s,p), 3(s,p,d), etc., whereas the second (azimuthal) quantum number (s, p, d, ...)

denotes the orbital angular momentum l = 1, 2, 3, ..., n − 1. To characterize the orbitals

and corresponding electrons completely, the magnetic quantum numbers ml = −l, ..., l

(projection of the orbital angular momentum) and ms = ±1/2 (projection of the intrinsic

angular momentum, the spin s) are needed. From the Pauli Exclusion Principle that

states that no two electrons within one atom can have the same set of quantum numbers

n, l, ml and ms it follows furthermore: Each main shell n can contain electrons.

l

m

n

l l

nl1

21

1

2122 (2.12)

However, in reality the angular momenta l and s are coupled due to the spin-orbit

interaction, so that another quantum number j (the total angular momentum) is adequate

to fully describe an electron state. It is the vectorial sum of l and s and can take the

following range of values: |l − s| ≤ j ≤ l + s, which results in 2 j + 1 electron states for

each j. Since the electron spin s has the fixed value 1/2, j can take the values, e.g., for n

= 1, 2. (Timna-Josua Kühn ,2011)

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2.20 X-Ray Detection

Once a sample has been excited to fluorescence, a detector is used to convert X-

rays into electronic signals which can be used to determine energy and intensity

(number of X-rays) emitted from the sample. There are two types of detectors

commonly used, the proportional counter used in WXRF and the semiconductor

detector. The former is rarely used in archaeological applications (Ismail 2019,

Lundblad et al. 2008).

2.21 History of X-Ray Fluorescence:

This chapter consists of theoretical background of history of X-ray fluorescence, basic

Principle of the X-ray fluorescence process and previous studies.

The history of X-ray fluorescence dates back to the accidental discovery of X-rays

in1895 by the German physicist Wilhelm Conrad Roentgen. While studying cathode

rays in a high-voltage, gaseous-discharge tube, Roentgen observed that even though the

experimental tube was encased in a black cardboard box the barium- platinocyanide

screen, which was lying adjacent to the experiment, emitted fluorescent light whenever

the tube was in operation.

Roentgen's discovery of X-rays and their possible use in analytical chemistry went

unnoticed until 1913. In 1913, H.G.J. Mosley showed the relationship between atomic

number (Z) and the reciprocal of the wavelength (1/λ) for each spectral series of

emission lines for each element. Today this relationship is expressed as:

2sZac (2.2.1)

Where:

a is a proportionality constant,

S is a constant dependent on a periodic series.

Although the earliest commercial XRF devices used simple air path conditions,

machines were soon developed utilizing helium or vacuum paths, permitting the

detection of lighter elements. In the 1960’s, XRF devices began to use lithium fluoride

crystals for diffraction and chromium or rhodium target X-ray tubes to excite longer

wavelengths. This development was quickly followed by that of multichannel

spectrometers for the simultaneous measurement of many elements. By the mid 60’s

computer controlled XRF devices were coming into use. In 1970, the lithium drifted

silicon detector (Si(Li)) was created, providing very high resolution and X-ray photon

separation without the use of an analyzing crystal.

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2.22 X-Ray Fluorescence

The working principle of XRF analysis is the measurement of wavelength or energy and

intensity of the characteristic X-ray photons emitted from the sample. This allows the

identification of the elements present in the analyte and the determination of their mass

or concentration. All the information for the analysis is stored in the measured

spectrum, which is a line spectrum with all characteristic lines superimposed above a

certain fluctuating background.

Other interaction processes, mainly the elastic and inelastic scattering of the primary

radiation on sample and substrate, induce the background.

X-Ray Fluorescence (XRF) is used to study the elemental composition of materials.

Generally the photons are absorbed by the material by photoelectric effect produces

vacancies in the inner electron shells of the atoms of material, followed bv the emission

of characteristic x-rays of the elements present. (Eric Lifshin, Oct, 1999).

Measurement of the spectrum of the emitted characteristic fluorescence radiation is

performed using wavelength-dispersive (WD) and energy-dispersive (ED))

spectrometers. In wavelength-dispersive X-ray fluorescence analysis (WDXRF). The

result is an intensity spectrum of the characteristic lines versus wavelength measured

with a Bragg single crystal as dispersion medium while counting the photons with a

Geiger Muller, a proportional or scintillation counter. In energy-dispersive X-ray

fluorescence analysis (EDXRF), a solid-state detector is used to count the photons,

simultaneously sorting them according to energy and storing the result in a multichannel

memory. The result is X-ray energy vs. intensity spectrum. The range of detectable

elements ranges from Be (Z = 4) for the light elements and goes up to U (Z = 92) on the

high atomic number Z side. (Gunter Gauglitz . et al. 2003).

The peaks in x-rays spectrum indicate what kind of chemical elements arc present,

while the number of counts (the area under the peaks) is related to the number of the

atoms in the sample, allowing the quantitative measurements to be made. Moreover, the

method gives information about the elements present in the sample irrespective of their

state of chemical combinations or the phases in which they exit (EricLifshin, Oct,

1999).

2.23 Guiera senegalensis (Ghubaysh) plant:

2.23.1 Family: Combretaceae.

2.23.2 Local Names: Arabic (Ghubaysh), latin (guiera senegalensis).

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2.23.3 Description: (Ghubaysh)is a shrub of savannah region of West and Central

Africa. Its leaves are commonly used in traditional medicine in gastrointestinal

disorders, respiratory infections and malaria. (Semi-)evergreen shrub up to (3–5) m tall,

with spindly bole or many branched; theparts covered with black dots; bark fibrous.

Leaves (almost) opposite, simple and entire; stipules absent; petiole 2–5 mm long,

short-hairy; ovate to orbicular, 3–5.5 cm × 2–3 cm, base rounded to almost cordate.

2.23.4 Ecology: (Ghubaysh) occurs in shrub savanna, tree savanna and fallow land,

from sea-level up to 1000 m altitude. (Ghubaysh) occurs on all types of soil but mainly

on dry sandy or degraded soils, sometimes in areas which are, temporarily, flooded.

(Wegdan, 2018)

2.24 Elements of Interest

The first step to setting up a XRF analysis is determining the elements of interest. If a

sample or rock type has never been analyzed for every conceivable element, the odds

are high that it contains something that we might not expect. Some samples come into a

laboratory as complete unknowns, such as obsidian artifacts from a region unfamiliar to

analysts in the lab. For example, many of the rhyolite centers that produced obsidian in

the Rift Valley in East Africa contain relatively high concentrations of Zn, much higher

than obsidian in the rest of the world (Negash and Shackley, 2006; Negash et al.,

2006).Zinc becomes one of the best discriminating elements in the region, particularly

those sources in Ethiopia and to a certain extent the Near East, but has little utility in

other regions.

If a sample is not well characterized, it is a good idea to perform a qualitative

examination of the material using three or more acquisition conditions, designed to

cover high, medium, and low energy ranges. Qualitative acquisition conditions will be

covered below. Alternatively, a multivariate statistical analysis such as principal

components analysis can isolate those elements of interest that are best discriminators in

the region (Glascock et al, 1998).

2.25 The Individual Elements:

2.25.1 Iron (Fe)

Iron has several vital functions in the body. It serves as a carrier of oxygen to the

tissues from the lungs by red blood cell hemoglobin, as a transport medium for electrons

within cells, and as an integrated part of important enzyme systems in various tissues.

The physiology of iron has been extensively reviewed Most of the iron in the body is

present in the erythrocytes as hemoglobin, a molecule composed of four units, each

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containing one heme group and one protein chain. The structure of hemoglobin allows it

to be fully loaded with oxygen in the lungs and partially unloaded in the tissues (e.g., in

the muscles). The iron-containing oxygen storage protein in the muscles, myoglobin, is

similar in structure to hemoglobin but has only one hemo unit and one globin chain.

Several iron-containing enzymes, the cytochromes, also have one hemo group and one

globin protein chain. These enzymes act as electron carriers within the cell and their

structures do not permit reversible loading and unloading of oxygen. Their role in the

oxidative metabolism is to transfer energy within the cell and specifically in the

mitochondria. Include the synthesis of steroid hormones and bile acids; detoxification of

foreign substances in the liver; and signal controlling in some neurotransmitters, such as

the dopamine and serotonin systems in the brain. Iron is reversibly stored within the

liver as ferritin and hemosiderin whereas it is transported between different

compartments in the body by the protein transferrin. The primary function of

hemoglobin (Hb) is to transport oxygen. Since oxygen is not very soluble in water (the

major constituent of blood), an oxygen transport protein must be used to allow oxygen

to be 'soluble'. Hemoglobin (Hb) is the oxygen transport protein used in the blood of

vertebrates. It is composed of 4 polypeptide chain, each of which contains one iron ion.

The iron is the site of oxygen binding; each iron can bind one O2molecule thus each

hemoglobin molecule is capable of binding a total to four (4) O2molecules. In humans,

the average hemoglobin concentration is 16 g/100 ml. This means that there are

approximately 150,500,000,000,000,000,000 hemoglobin molecules in 100 ml of whole

blood. How many possible binding sites for oxygen are contained in 100 ml of blood?

How many O2molecules can be carried by 100 ml of blood if the hemoglobin is

completely saturated (meaning every possible binding site is filled) with oxygen? It is

important that you remember that the purpose of Hb is to pick up oxygen at the lungs

and to deliver it to the tissues. (C.P.Gupta,2014)

Iron is the most abundant metal, and is be lived to be the tenth most abundant element

in the universe. Iron is a metal extracted from iron are, and is hardly ever found in the

free (elemental) state. Iron is the most used of all the metals, comprising 95 percent of

all the metal tonnage produced worldwide. Its combination of low cost and high

strength make it indispensable, especially in applications like automobiles. The hulls of

large ships, and structural components for buildings. Steel is the besk known alloy of

iron. Iron is essential to all organisms, except for a few bacteria. Iron binds avidly to

virtually all biomolecules so it will a there nonspecifically to cell membranes, nucleic

acids, proteins etc. iron distribution is heavily regulated in mammals. The iron absorbed

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from the duodenum binds to transferring, and carried by blood it reaches different it

cells. It is strongly advised not to let the chemical enter into the environment because it

persist in the environment. Excess iron in the body causes liver and kidney damage

(haemochromatosis) some iron compounds are suspected carcinogens, (Ismail 2019,

Greaney, 2005).

Effects on humans

Iron is an essential element in human nutrition. Estimates of the minimum daily

requirement for iron depend on age, sex, physiological status, and iron bioavailability

and range from about 10 to 50 mg/day (12).

The average lethal dose of iron is 200–250 mg/kg of body weight, but death has

occurred following the ingestion of doses as low as 40 mg/kg of body weight (6).

Autopsies have shown hemorrhagic necrosis and sloughing of areas of mucosa in the

stomach with extension into the sub mucosa. Chronic iron overload results primarily

from a genetic disorder (hemochromatosis) characterized by increased iron absorption

and from diseases that require frequent transfusions (10). Adults have often taken iron

supplements for extended periods without deleterious effects (10), and an intake of 0.4–

1 mg/kg of body weight per day is unlikely to cause adverse effects in healthy persons

(19). (World Health Organization, 2003)

2. 25.2 Lead (Pb)

Lead is a ubiquitous pollutant in the ecosystem. On a global scale the

combustion of alkyl lead additives in motor fuels accounts for the major part of all lead

emissions into the atmosphere, thus influencing all compartments of the environment.

This has been hypothesized from mass balance studies (1) and has been confirmed by

the changes in environmental lead levels subsequent to the reductions in worldwide use

of alkyl leads in petrol since the early 1980s. Point sources, such as primary or

secondary lead smelters, may create local pollution problems. The level of

contamination of the surrounding air and soil depends on the amount of lead emitted,

the height of the stack, the presence of fugitive sources, topography and other local

features. In addition, the refining and manufacture of lead-containing compounds and

goods and refuse incineration also give rise to lead emissions. Since coal, like many

minerals, rocks and sediments, usually contains low concentrations of lead, a number of

other industrial activities such as iron and steel production, copper smelting and coal

combustion must be regarded as additional sources of lead emissions into the

atmosphere. (WHO, 2001)

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Lead (Pb), with atomic number 82, atomic weight 207.19 and a specific gravity of

11.34, is a bluish or silvery-grey metal with a melting point of 327.5 °C and a boiling

point at atmospheric pressure of 1740 °C. It has four naturally occurring isotopes with

atomic weights 208, 206, 207 and 204 (in decreasing order of abundance). The isotopic

ratios may differ for different mineral sources, and this property has been exploited in

non-radioactive tracer studies to investigate environmental and metabolic pathways of

lead. Despite the fact that lead has four electrons on its valence shell, its typical

oxidation state is +2 rather than +4, since only two of the four electrons ionize easily.

Apart from nitrate, chlorate and, to a much lesser degree, chloride, most of the inorganic

salts of lead (II) have poor solubility in water. Stable organic lead compounds, such as

tetraethyl lead and tetraethyl lead, are formed by direct binding of lead to a carbon

atom. These compounds are colorless liquids with boiling points of 110 °C and 200 °C,

respectively. They are decomposed at boiling point as well as by ultraviolet light and

trace chemicals in air, such as halogens, acids and oxidizing agents. Owing to their use

as fuel additives for anti-knock purposes, they are sources of environmental lead

Nevertheless; their environmental impact has fallen during the past 15 years in most

industrialized countries owing to legislation aimed at reducing and replacing lead in

petrol. Sources Lead is a ubiquitous pollutant in the ecosystem. On a global scale the

combustion of alkyl lead additives in motor fuels accounts for the major part of all lead

emissions into the atmosphere, thus influencing all compartments of the environment.

This has been hypothesized from mass balance studies (1) and has been confirmed by

the changes in environmental lead levels subsequent to the reductions in worldwide use

of alkyl leads in petrol since the early 1980s. Point sources, such as primary or

secondary lead smelters, may create local pollution problems. The level of

contamination of the surrounding air and soil depends on the amount of lead emitted,

the height of the stack, the presence of fugitive sources, topography and other local

features. In addition, the refining and manufacture of lead-containing compounds and

goods and refuse incineration also give rise to lead emissions. Since coal, like many

minerals, rocks and sediments, usually contains low concentrations of lead, a number of

other industrial activities such as iron and steel production, copper smelting and coal

combustion must be regarded as additional sources of lead emissions into the

atmosphere. The presence of lead water-pipes in old houses can be an important source

of lead exposure for humans, particularly in areas with soft water. In certain areas, lead-

containing paint in old. (WHO Regional Office for Europe, Copenhagen, Denmark,

2001)

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Most of the studies looking for a possible link between lead exposure and cancer

have focused on workers with high levels of occupational (work-related) exposure to

inorganic lead. People with heavy workplace exposures to lead have been found to have

blood lead concentrations many times higher than the average blood lead concentration

in the general population. Several studies have looked for a link between exposure to

lead in the workplace (mainly among battery workers and smelter workers) and lung

cancer. Some of these studies have found a small increase in lung cancer risk. However,

most of these studies were limited in that they didn't take into account other factors that

might affect lung cancer risk, such as smoking or exposures to arsenic or other heavy

metals that typically also occur along with lead exposures in industrial settings. Some

studies looking at blood lead levels in the general population have also found a small

increased risk of lung cancer in people with higher lead levels. Several of these same

workplace studies also looked at stomach cancer risk. Most of the studies found an

increased risk of stomach cancer with higher lead exposure. Although it is unlikely

these results would be affected by smoking or arsenic exposure, the studies didn’t take

into account other factors that could also have affected stomach cancer risk. Studies

have also looked at possible links between workplace exposures to lead and other

cancers, including cancers of the brain, kidney, bladder, colon, and rectum. The results

of these studies have been mixed. Some studies have found links, while others have not.

The link between lead exposure and cancer is clearly a concern, and more research is

needed to better define the possible link between lead exposure and a number of

cancers. (Manju Mahurpawar ,2015)

Effects on humans

Toxicological effects

As far as long-term, low-level lead exposure is concerned, the following effects have to

be considered in relation to the general population:

1. Effects on haem biosynthesis;

2. Effects on the nervous system;

3. Effects on blood pressure and cardiovascular effects, and

4. Effects on kidney function.

The present discussion is, therefore, limited to these aspects of lead toxicity.

(WHO, 2001)

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2. 25.3 Manganese (Mn)

Manganese (Mn) is the twelfth most abundant element in the earth's crust and is

naturally present in rocks, soil, water, and food. Mn is an essential element for humans,

animals, and plants, and is required for growth, development, and maintenance of

health. There are inorganic and organic Mn compounds, with the inorganic forms

being the most common in the environment. Uses of Mn include:

(i) Iron and steel production;

(ii) Manufacture of dry cell batteries;

(iii) Production of potassium permanganate and other Mn chemicals;

(iv) Oxidant in the production of hydroquinone;

(v) Manufacture of glass;

(vi) Textile bleaching;

(vii) Oxidizing agent for electrode coating in welding rods;

(viii) Matches and fireworks;

(ix) Tanning of leather1.

Organic compounds of Mn are present in the fuel additive,

methylcyclopentadienyl manganese tricarbonyl (MMT), fungicides (e.g., mane band

mannose), and in contrast agents used in magnetic resonance imaging. Mn is naturally

present in food, with the highest concentrations typically found in nuts, cereals,

legumes, fruits, vegetables, grains, and tea - it is also present at low levels in drinking

water. Typical, daily intakes range from 2-9 mg/day for adults and approximately

3-5 per cent is absorbed from the gastrointestinal tract3. Absorption of Mn from the

diet occurs in the divalent and tetravalent state.

Manganese balance studies and excretion data indicate that low gastrointestinal

absorption and rapid elimination of Mn limits the toxicity of the Mn following the

ingestion of high doses. Chronic inhalation exposure to relatively high levels of

Mn has been associated with adverse neurological effects and a few studies have

reported the same following the ingestion of high levels or chronic exposure to

Mn in drinking water. Clinical Mn neurotoxicity has been reported in patients

receiving long-term parenteral nutrition and in patients with chronic liver dysfunction or

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renal failure, as a result of their inability to eliminate and clear Mn from the blood. The

primary anthropogenic sources of Mn in ambient air include emission of Mn from

industrial sources such as ferroalloy production plants, iron and steel foundries, power

plants, and coke ovens and entrainment of soils containing Mn. The background levels

of Mn in rural and urban areas without point sources of Mn range from about 0.005-

0.07 μg Mn/m3, while average ambient air levels of Mn near industrial sources

range from 0.13-0.3 μg Mn/m3,4,5. Exposure to Mn from the erosion of soil is the

most important natural source of Mn in the ambient air, but little data are available to

estimate the contribution of Mn in ambient air from this source. Higher inhalation

exposures may be experienced in occupational settings such as Mn mines,

foundries, smelters, and battery manufacturing facilities.( Ismail 2019)

Manganese (Mn) is an element widely distributed in the earth’s crust. It is

considered to be the twelfth most abundant element and the fifth most abundant metal.

Manganese does not occur naturally in a pure state; oxides, carbonates and silicates are

the most important manganese-containing minerals. The most common manganese

mineral is pyrolusite (MnO2), usually mined in sedimentary deposits by open-cast

techniques. Manganese occurs in most iron ores. Its content in coal ranges from 6 μg/g

to 100 μg/g; it is also present in crude oil, but at substantially lower concentrations.

Manganese is mainly used in metallurgical processes, as a deoxidizing and

desulfurizing additive and as an alloying constituent. It is also used in the production of

dry-cell batteries, in chemical manufacturing, in the manufacture of glass, in the leather

and textile industries, and as a fertilizer. Organic carbonyl compounds of manganese are

used as fuel-oil additives, smoke inhibitors and anti-knock additives in petrol.

Crustal manganese enters the atmosphere by a number of natural and anthropogenic

processes, which include the suspension of road dusts by vehicles and wind erosion and

the suspension of soils, particularly in agricultural, construction and quarrying activities.

The resulting mechanically generated aerosols consist primarily of coarse particles ≥ 2.5

μm mass median aerodynamic diameter (MMAD). (Who .2000)

Manganese is a very common compound that can be found everywhere on earth.

Manganese is one out of three toxic essential trace elements, which means that it is not

only necessary for humans to survive, but it is also toxic a thigh concentration.

Manganese effects occur mainly in the respiratory trace and in the brain. Manganese

compounds exist naturally in the environment as solids is the soils and small particles in

the water. Manganese particles in air are present in dust particles. These usually settle to

earth within a few days. Humans enhance manganese concentrations in the air by

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industrial activities and through burning fossil fuels. For animals manganese is an

essential compound of over thirty – six enzymes that are used for the carbohydrate,

protein and fat metabolism. In plant manganese ions are transported to the leaves after

uptake from soils. This causes disturbances in plant mechanisms. Manganese can cause

both toxicity and deficiency symptoms in plants. When the pH of the soil is low

manganese deficiencies are more common, (Ismail 2019, Greaney, 2005).

Effects on humans

Several epidemiological studies of workers have provided consistent evidence

indicating that neurotoxicity is associated with low-level occupational manganese

exposure. Conducted a cross-sectional study of neurobehavioral and other endpoints in

Belgian workers. A group of 92 male alkaline battery plant workers exposed to MnO2

dust were compared to a matched control group of 101 male workers without industrial

manganese exposure. The geometric mean occupational-lifetime integrated respirable

dust concentration was 793 μg manganese per m3·years (range: 40 – 4433). The

equivalent value for total dust was 3505 mg manganese per m3·years (range: 191–27

465). The monitored concentrations were considered representative of the usual

exposures of the workers because work practices had not changed during the preceding

15 years of the plant’s operation. Because the respirable fraction (5-μm MMAD) is

more representative of the toxicologically significant particles (i.e. the smaller inhaled

particles that deposit predominantly in the lower respiratory tract), the respirable dust

measurements were considered to be more accurate than total dust as an indicator of

exposure in relation to the observed health effects. The manganese-exposed workers

performed significantly worse than matched controls on several measures of

neurobehavioral function, particularly eye-hand coordination, hand steadiness and

visual reaction time. (Who .2000)

2. 25.4 Chromium (Cr)

Elemental chromium (Cr) was discovered in crocoite (PbCrO4) by

Vaquelin in 1798 (Barceloux, 1999). Carcinogenic effects of hexavalent Cr were

discovered towards the end of the 19th century, when nose tumours in workers handling

chromium pigments in Scotland were described. In the 1930s, case studies focusing on

lung cancer incidence in workers handling Cr were published and lung cancer was

recognized as an occupational disease in these workers in Germany during 1936

(Teleky, 1936). Since then, Cr has been studied especially as a mineral with toxic effect

on the organism. +

. (A. PECHOVA, L. PAVLATA, 2007)

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Chromium (Cr) is a grey, hard metal most commonly found in the

trivalent state in nature. Hexavalent (chromium (VI)) compounds are also

found in small quantities. Chromite (FeOCr2O3) is the only ore containing a

significant amount of chromium. The ore has not been found in the pure form; its

highest grade contains about 55% chromic oxide .In Europe, ferrochromium is

produced mainly in Finland, France, Italy, Norway, Sweden and former

Yugoslavia. Potassium chromate is produced mainly in Germany, Italy,

Switzerland and the United Kingdom. Sodium chromate and dichromate are

now among the most important chromium products, and are used chiefly

for manufacturing chromic acid, chromium pigments, in leather tanning and for

corrosion control. Chromium levels in soil vary according to area and the

degree of contamination from anthropogenic chromium sources. Tests on

soils have shown chromium concentrations ranging from 1 to 1000 mg/kg,

with an average concentration ranging from 14 to about 70 mg/kg .

Chromium(VI) in soil can be rapidly reduced to chromium(III) by organic

matter. As chromium is almost ubiquitous in nature, chromium in the air

may originate from wind erosion of shale's, clay and many other kinds of soil. In

countries where chromite is mined, production processes may constitute a major

source of airborne chromium. In Europe, endpoint production of chromium

compounds is probably the most important source of chromium in air.

Occurrence in air Information on concentrations of total and spectated chromium

in the atmosphere is limited. Measurements carried out above the North

Atlantic, north of latitude 30° north, several thousands of kilometers from

major land masses, showed concentrations of chromium of 0.07–1.1 ng/m3.

The concentrations above the South Pole were slightly lower. (WHO Regional Office

for Europe, Copenhagen, Denmark, 2001)

Methods for adequate analysis of Cr in biological material have not been

developed until recently. This is why there has been relatively little data on Cr content

in different body tissues and fluids. The blood concentrations of Cr reported in literature

have come down with the gradual improvement of instrumentation. Levels of chromium

ranging between 1 and 40 μg/l had been claimed until. 1978 was a turning point of a

kind since electro thermic atomic absorption spectrophotometry started to be used,

making Cr content analysis more accurate, which got reflected in the lower Cr

concentrations detected in biological samples. Claim that the concentrations are 0.035–

0.04 μg/l and 0.120–0.34 μg/l for the blood serum of a healthy population and full

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blood, respectively. There is a greater difference between full blood and blood serum

according to, who reported 0.058–0.388 μg/l of Cr in the blood serum of a healthy

population and 0.120–0.673 μg/l of Cr in full blood. Anderson et al. (1985) have found

the basal serum concentration of Cr in adults to be 0.13 ± 0.02 μg/l, followed by a

significant increase to 0.38 ± 0.02 μg/l after 3 months of Cr supplementation, but

despite this, they do not regard serum concentrations of Cr as a good indicator of the Cr

nutritional status. Concentrations of Cr in the blood of cattle with respect to the Cr

content in pasture plants in a region characterized by an increased Cr stress level’s

blood levels detected in this trial ranged from 9 to 92 μg/l, depending on the Cr content

in the plants. Found the Cr blood concentrations in dairy cows during the perinatal

period to be 3–5 μg/l while supplementation with 10 mg Cr per animal/day had no

effect on the Cr concentrations in blood.

The concentration of Cr in full blood is approximately 2–3 times higher than the

Cr concentration in plasma. Plasmatic Cr concentrations reflect the exposure to both

Cr3+

and Cr6+

while intracellular concentration reflects the exposure to Cr6+

, this is

because only Cr6+

has the capacity to penetrate into erythrocytes. The low concentration

of Cr in erythrocytes also testifies to the fact that the Cr6+

concentration has not

significantly surpassed the reduction capability of blood plasma for Cr6+

. (A.

PECHOVA, L. PAVLATA, 2007)

Effects on humans

Toxicological effects

Chrome ulcers, corrosive reactions on the nasal septum, acute irritative

dermatitis and allergic eczematous dermatitis have been recorded among subjects

exposed to chromium (VI) compounds (1,4). Ulcerations or perforations of the nasal

septum were reported in two-thirds of subjects following inhalation exposure to

chromium (VI) (as chromic acid) resulting from exposure at peak concentrations of

more than 20 μg/m3 (39). The data available in published reports do not suggest any

dose–response relationship between local exposure to chromium (VI) compounds and

the development of septal ulceration of the nose. Mancuso & Hueper (40) described a

spotty, moderately severe but not nodular pneumoconiosis in chromate workers.

(WHO, 2001)

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2. 25.5 Nickel (Ni)

Nickel is a metal that is widely distributed in the earth's crust (soil and rocks),

air and water. Nickel can combine with other elements including sulphur, chlorine and

oxygen to form water soluble and insoluble nickel compounds. Nickel compounds are

mostly crystals or powders at room temperature. Nickel is used to produce stainless

steel and other alloys. Nickel alloys are used in coins, jeweler, household appliances

and electrical equipment. Nickel compounds are also used in the production of nickel-

cadmium batteries.

Human activities including combustion of coal and oil, municipal incineration, steel and

other nickel alloy production and electroplating all release nickel into the environment.

Volcanoes and forest fires also release nickel into the environment. people may be

exposed to nickel by ingesting food that is contaminated with nickel or by

cigarette smoking. People may also be exposed to low levels of nickel by

inhaling air contaminated with nickel or by ingesting nickel contaminated water.

Skin contact with products that contain nickel (e.g. jewelry, stainless steel and coins)

can lead to trace amounts released from such products. Nickel contact

dermatitis was often seen in individuals who wore nickel containing jewelry in

the past, but stringent controls are now in place to ensure that this no longer a

significant route of exposure. Workers employed in industries that produce, process

or use nickel may be exposed to higher levels of nickel than the general population.

He presence of nickel in the environment does not always lead to exposure.

Clearly, in order for it to cause any adverse health affects you must come into contact

with it. You may be exposed by breathing, eating, or drinking the substance or by

skin contact. Following exposure to any chemical, the adverse health affects you may

encounter depend on several factors, including the amount to which you are

exposed (dose), the way you are exposed, the duration of exposure, the form of

the chemical and if you were exposed to any other chemicals. Inhalation of nickel

or nickel compounds for a short period of time may cause sore throat and hoarseness.

Ingestion of nickel compounds may cause nausea, vomiting, abdominal pain and

diarrhea. Skin exposure to nickel or its compounds can lead to skin irritation

and allergic contact dermatitis (an immunological reaction leading to skin

sensitization expressed as a reddening/rash on the skin). Nickel contact

dermatitis was often seen in individuals who wore nickel containing jewelry in the

past, but stringent controls are now in place to ensure that this is no longer a significant

route of exposure.( Ismail 2019, CRCE, PHE ,2009)

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Nickel is a compound that occurs in the environment only at very low levels.

Humans use nickel for many different applications. The most common application of

nickel is the use as an ingredient of steal and other metal products. It can be found in

common metal products such as jewelry. Foodstuffs naturally contain small amounts of

nickel. Chocolate and fats are known to contain severely high quantities. Nickel uptake

will boost when people eat large quantities of vegetables from polluted soils. Plants are

known to accumulate nickel and as a result the nickel uptake from vegetables will be

eminent. Smokers have a higher nickel uptake through their lungs. Finally, nickel can

be found in detergents. Humans may be exposed to nickel by breathing air, drinking

water, eating food or smoking cigarettes. Skin contact with nickel-contaminated soil or

water may also result in nickel exposure. In small quantities nickel is essential, but

when the uptake is too high it can be a danger to human health. An uptake of too large

quantities of nickel has the following consequences: Higher chances of development of

lung cancer, nose cancer, larynx cancer and prostate cancer Sickness and dizziness after

exposure to nickel gas Respiratory failure, Lung embolism, Birth defects, Asthma and

chronic bronchitis, Allergic reactions such as skin rashes, mainly from jewelry, Heart

disorders. Nickel fumes are respiratory irritants and may cause pneumonitis. Exposure

to nickel and its compounds may result in the development of a dermatitis known as

―nickel itch‖ in sensitized individuals. The first symptom is usually itching, which

occurs up to 7 days before skin eruption occurs. The primary skin eruption is

erythematous, or follicular, which may be followed by skin ulceration. Nickel

sensitivity, once acquired, appears to persist indefinitely. (Manju Mahurpawar ,2015)

The largest deposits of Ni are to be found in the oceanic manganese nodules,

which contain about I % Ni. The greatest part of the production of Ni is used in the steel

industry and for the production of alloys. Organ nickel compounds play an important

role in a number of polymerization processes. Physiologically Ni is one of the trace

elements; the human body contains about 10 mg. Little is known about the biological

role that Ni plays, but it appears to participate in carbohydrate metabolism; the

concentration in serum and urine is around 0.5 µg/L. Inhalable dusts or aerosols of Ni

metal or compounds, such as are produced during production and processing, are

classified as hazardous substances and are carcinogenic. Nickel is thus an important

element in the areas of toxicology and industrial hygiene. (Bcrnhard and

Michael,2005)

Nickel is a compound that occurs in the environment only at very low levels and is

essential in small dross but it can be dangerous when the maximum tolerable amounts

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are exceeded. This can cause various kinds of cancer on different sites within the bodies

of animals, mainly of those that live near refineries. The most common application of

nickel is an ingredient of steal and other metal products. Nickel is released into the air

by power plants and trash incinerators and will settle the ground or fall down after

reactions with precipitin. Is usually takes a long time for nickel to be removed from air

(Ismail 2019, Greaney,2005).

Effects on humans

Toxicological effects

Severe lung damage has been recorded following acute inhalation exposure to nickel

carbonyl. Reversible renal effects (in workers), allergic dermatitis (most prevalent in

women), and mucosal irritation and asthma (in workers) have been reported following

exposure to inorganic nickel compounds (5). Renal effects and dermatitis presumably

relate both to nickel uptake by both inhalation and ingestion, in addition to cutaneous

contact for dermatitis.Allergic skin reactions to nickel (dermatitis) have been

documented both in nickel workers and in the general population. However, the

significance of nickel as a cause of occupationally-induced skin reaction is decreasing.

In contrast, there is evidence that nickel is increasingly a major allergen in the general

population, especially in women. About 2% of males and 11% of females show a

positive skin reaction to patch testing with nickel sulfate. Ear-piercing considerably

increases the risk of nickel sensitization (34). (Who .2000)

2. 25.6 Zinc (Zn)

Zinc the periodic table of the elements, zinc can be found in group IIb, together

with the two toxic metals cadmium and mercury. Nevertheless, zinc is considered to be

relatively non-toxic to humans. This is reflected by a comparison of the LD50 of the

sulfate salts in rats. According to the Toxnet database of the U.S. National Library of

Medicine, the oral LD50 for zinc is close to 3 g/kg body weight, more than 10-fold

higher than cadmium and 50-fold higher than mercury. (Laura, Lothar and

Hajo,2010)

Zinc is found in a wide variety of foods. You can get recommended amounts of

zinc by eating a variety of foods including the following: Oysters, which are the best

source of zinc. Red meat, poultry, seafood such as crab and lobsters, and fortified

breakfast cereals, which are also good sources of zinc.• Beans, nuts, whole grains, and

dairy products, which provide some zinc.

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Zinc is present in almost all multivitamin/mineral dietary supplements. It is also

available alone or combined with calcium, magnesium or other ingredients in dietary

supplements. Dietary supplements can have several different forms of zinc including

zinc gluconate, zinc sulfate and zinc acetate. It is not clear whether one form is better

than the others.

Zinc is also found in some oral over-the-counter products, including those

labeled as homeopathic medications for colds. Use of nasal sprays and gels that contain

zinc has been associated with the loss of the sense of smell, in some cases long-lasting

or permanent. Currently, these safety concerns have not been found to be associated

with oral products containing zinc, such as cold lozenges.

Zinc is also present in some denture adhesive creams. Using large amounts of

these products, well beyond recommended levels, could lead to excessive zinc intake

and copper deficiency. This can cause neurological problems, including numbness and

weakness in the arms and legs. (National Institute of Health, 2016)

2. 25.7 Molybdenum (Mo)

Mo is an essential micronutrient, but the physiological requirement for this element is

relatively low. Plants take up Mo mainly as molybdate ions, and its absorption is

proportional to its concentration in the soil solution. Although there is no direct

evidence, there is a suggestion of the active uptake of Mo (Kabata and Pendias 2000)

General discretions is Physicochemical properties the physicochemical properties of

molybdenum are summarized below. Property Value Melting point 2610 °C Boiling

point 5560 °C Density 10.2 g/cm3Vapour pressure 0.133 kPa at 3102 °C Water

solubility Insoluble 1.2 Organoleptic properties Ammonium molybdate imparts a

slightly astringent taste to water at concentrations above about 10 mg of molybdenum

per litre. 1.3 Major uses Molybdenum is used in the manufacture of special steels, in

electrical contacts, spark plugs, X-ray tubes, filaments, screens and grids for radio

valves, and in the production of tungsten, glass-to-metal seals, non-ferrous alloys and

pigments. Molybdenum disulfide has unique properties as a lubricant additive.

Molybdenum compounds are used in agriculture either for the direct treatment of seeds

or in the formulation of fertilizers to prevent molybdenum deficiency (World Health

Organization 2011).

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2. 25.8 Copper (Cu)

Copper is a naturally occurring metal in soil that can also be introduced by human

activities. Mining activities, metal production, wood production, phosphate fertilizer

production and use of agrichemicals in horticultural soils are human – influenced

sources of copper in agricultural soils most copper compounds complexes strongly with

organic matter. Water – soluble species pose a threat to the environment.(Kabata and

Pendies, 2000).

Very extensive studies have been made on the forms and behavior of Cu in plants. All

findings described in a number of outstanding textbooks can be summarized as follows:

1. Cu is mainly complexed with organic compounds of low molecular weight and with

proteins.

2. Cu occurs in the compounds with no known functions as well as in enzymes having

vital functions in plant metabolism.

3.Cu plays a significant role in several physiological processes—photosynthesis,

respiration, carbohydrate distribution, N reduction and fixation, protein metabolism, and

cell wall metabolism.

4. Cu influences water permeability of xylem vessels and thus controls water

relationships.

5. Cu controls the production of DNA and RNA, and its deficiency greatly inhibits the

reproduction of plants (reduced seed production, pollen sterility).

6. Cu is involved in the mechanisms of disease resistance. This resistance of plants to

fungal diseases is likely to be related to an adequate Cu supply. There is also evidence

that plants with enriched Cu concentrations are susceptible to some diseases. These

phenomena may indicate that the role of Cu in disease resistance is an indirect one

(Kabata and Pendias, 2000)

2. 25.9 Tungsten (W)

Tungsten is a naturally occurring element that exists in the form of minerals, but

typically not as a pure metal (ATSDR 2005). The color of tungsten may range from

white for the pure metal to steel-gray for the metal with impurities (NIOSH 2016).

There are more than 20 known tungsten-bearing minerals (ATSDR 2005). Wolframite

([FeMn]WO4) and Scheelite (CaWO4) are two common, commercially-mined minerals

that contain tungsten (ATSDR 2005; Koutsospyros et al, 2006). Natural tungsten is

composed of five stable isotopes. There are 28 artificial radioactive isotopes, which

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37

have short half-lives ranging from less than a second to 121 days (ATSDR 2005; Audi

et al, 2003).

Tungsten in plants was either taken up by the plant or was attached to the plant as a

component of the soil. Although very limited data are available, exposure to tungsten

from air, drinking water, and food is expected to be insignificant. In certain workplaces,

you can be exposed to levels of tungsten in air that are higher than background levels

((NTIS), 2005).

2. 25.10 Vanadium (V)

The evidence that V is essential for the growth of higher plants is not yet conclusive,

while the essentiality of this element for alga species is unquestionable and V is known

to stimulate photosynthesis in these organisms(Kabata and Pendias, 2000)

Nutritional studies have shown that vanadium Its deficiency may result in growth

reduction, impairment of reproduction and disturbances in lipid metabolism. Vanadium

is also essential for soil nitrogen-fixing microorganisms. It may play a significant role in

human nutrition. Biochemical, physiological and pharmacological properties of

vanadium compounds have been reviewed. It has been suggested that vanadium may be

a regulatory agent for enzymatic activities in mammalian tissues. Vanadium is a potent

inhibitor of many enzymes, while it stimulates adenylate cyclase. It has been shown to

inhibit cholesterol biosynthesis and lower plasma cholesterol levels. Vanadium can also

directly influence glucose metabolism in vitro and may play a role in its regulation.

Lipid peroxidation of rat lung extracts, liver microsomes and mitochondria was induced

by sulfite and accelerated by the presence of vanadium compounds. Vanadium may play

a physiological role as part of a control on levels of the endogenous antioxidant,

glutathione. This may also be important with respect to toxic interactions of chemicals

(WHO 2000)

2. 25.11 Titanium (Ti)

Titanium is one of the most common in the earth's crust (ninth in abundance 0.6% by

mass); it occurs in a number of minerals as well as in living system and natural bodies

of water. Titanium is used widely in the chemical industry. (Kabata and Pendies,

2000).

2. 25.12 cobalt (Co)

Numerous studies have been made of plant uptake of Co from soils, and it has been

shown that enrichment of the soil with Co has led to increased levels of this metal in

plants. Co is also easily taken up by leaves through the cuticle; therefore, foliar

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applications of Co in solution are known. In nature, although plant species range widely

in their content of Co, toxicity symptoms are not often observed. When a high Co level

is readily available, in polluted soil in particular, it can seriously affect plant growth and

metabolic functions to be effective in the correction of Co deficiency. (Kabata and

Pendias 2000)

2. 25.13 Niobium (Nb)

Niobium, also known as columbium, is a chemical element with the symbol Nb

(formerly Cb) and atomic number 41. Niobium is a light grey, crystalline, and

ductile transition metal. Pure niobium has a Mohs hardness rating similar to that of

pure titanium (G.V. Samsonov, 2015).

2.26 Previous studies:

There are no intensive studies that handled the physic characteristics of Guiera

Senegalensis (Gabeysh) plant, but some studies have discussed the uses of its extract in

the medical uses.

2.26.1 ETHNOBOTANICAL SURVEY AND PHYTOCHEMICAL

STUDIES OF GUIERA SENEGALENSIS LAM. IN MUBI LOCAL

GOVERNMENT OF ADAMAWA STATE

The Sudano-Sahelian species Guiera senegalensis is a small shrub found mainly

in West Africa. It is well known in the Sahel, where it grows gregariously, and forming

abundant single-species colonies on fallow clay or sandy soils. Six (6) traditional

medical practitioners were interviewed from different location in the study area (Mubi

North and Mubi South L.G.A). The ethnobotanical survey revealed that various plant

parts can be used to relief various sickness (Malaria, Fever, Dental absesse, e.t.c.) With

the leaves (8) being the most frequently used part. New uses of plant part by traditional

medical practitioners were recorded especially the use of decocted leaves to relief

abdominal pains and migraines. Phytochemical analysis of most used part of the plant

were carried out which revealed the presences of some major classes of secondary

metabolites, namely; anthraquinones, terpenoids, saponins, alkaloids, flavonoids, tanins

and cardiotrnic and cyanogenic glycosides. Further investigation should be carried out

to extract the active component in Guiera senegalensis which will serve as a potential

medicine for the phytotherapeutic arsenal (Zakawa et al, 2018).

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2.26.2 Guiera senegalensis (Gs) is a well-known traditional medicinal

plant in Africa

Whose leaves extract and roots powder are used for treatment of diseases and

wounds in Western Kordufan, Sudan. The aim of this study was to investigate the

phytochemical analysis, toxicity, and the antifungal activity of Gs leaves extract.

Extract of the leaves of Gs was tested for its antimicrobial activity against Stemphylium

solani, Aspergillus flavus, Trichoderma viride, Penicillium Spp., Fusarium

verticillatum, Cladosporium cladosporioides, and Fusarium solani. This present study

showed that Gs leaves extract has no inhibition activity against all of the tested fungal

strains. On the other hand, the toxicity test, which was conducted by using brine shrimp,

suggests that Gs leaves extract is apparently not toxic. The phytochemical screening

revealed that Gs leave extract contains alkaloids, flavonoids, terpenoids, tannin,

carbohydrates, proteins, steroids, and saponins. The results of this preliminary

investigation suggests that the medicinal plant extract may be safe to use as a drink for

treatment of various diseases as has been practiced for years in the villages of Western

Sudan. More research is needed to investigate if there is any side effect when the extract

is taken orally. Further, the medicinal properties of the phytochemical compounds of Gs

need to be further investigated (Nabaa, 2016).

2.26.3 Introduction: Guiera senegalensis J. F. Gmel

Known locally in Sudan as ―Ghobeish‖ is a small herb, African species that is

found mainly in West Africa. It has widespread uses in traditional medicine. In the

current study, the putative anti-pyretic activity of the ethanolic extract of G.

senegalensis leaves is assessed. Methodology: 200 and 400 mg/kg body weight of G.

senegalensis leaves extract were investigated on induced pyretic and non-pyretic rats.

Pyrexia was induced in rats by sub-cutaneous injection of yeast solution. Temperature

of rats was measured before and after treatment at 1, 2, 3, and 4 hours. Results: 400

mg/kg body weight of G. senegalensis ethanolic extract administered to hyperthermic

rats caused a significant (P≤0.05) decrease in temperature after 1 hour of treatment

when compared with the effect of standard group that was administered with

paracetamol. 200 mg/kg of the extract has shown a decreasing effect on the temperature

of the non-pyretic rats. Phytochemical screening of G. senegalensis leaves indicated the

presence of large amounts of flavonoids and tannins, moderate amounts of steroids and

cumarin, and little amounts of triterpenes. Conclusion: From these findings, it is

concluded that G. senegalensis ethanolic extract has evidence of reducing hyperthermia

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in experimental animals and this effect may be correlated to other biological activities

of this medicinal plant (Reem, 2018).

2.26.4 Phytochemical and pharmacological study of roots and leaves of

Guiera senegalensis J.F. Gmel (Combretaceae)

The chemical composition of total alkaloids from leaves and roots of Guiera

senegalensis was investigated. Three beta-carboline alkaloids were purified: in addition

to harman and tetrahydroharman, known in roots and leaves, harmalan (dihydroharman)

was isolated for the first time from roots of Guiera senegalensis. Guieranone A, a

naphthyl butanone, was also purified from leaves and roots. The in vitro antiplasmodial

activity and the cytotoxicity of extracts and pure compounds were evaluated. Each total

alkaloid extract and beta-carboline alkaloids presented an interesting antiplasmodial

activity associated with a low cytotoxicity. Harmalan was less active than harman and

tetrahydroharman. Guieranone A showed a strong antiplasmodial activity associated

with a high cytotoxicity toward human monocytes. Its cytotoxicity was performed

against two cancer cell lines and normal skin fibroblasts in order to study its anticancer

potential: Guieranone A presented a strong cytotoxicity against each cell strains.

Finally, we evaluated the potent synergistic antimalarial interaction between Guiera

senegalensis and two plants commonly associated in traditional remedies: Mitragyna

inermis and Pavetta crassipes. Three associations evaluated were additive. A synergistic

effect was shown between total alkaloids extracted from leaves of Guiera senegalensis

and those of Mitragyna inermis. This result justified the traditional use of the plants in

combination to treat malaria (Julien Fiot et al, 2006).

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CHAPTER THREE

MATERIALS AND METHODS

3.1 Introduction

This chapter will deal with different practical and experimental aspects such as

description of the study area, leaves sampling of the Guiera Senegalensis plant,

preparation of samples and measurement of heavy element concentration by XMET

5000.

3.2 Material

The Guiera Senegalensis plant grows in its natural habitat in the Abu Zabad

area in West Kordofan, Sudan, where the study was conducted. The ghoulish plant is

generally present as a shrub that can grow to a height of 3 to 5 meters and samples were

taken from trees ranging from 1.5 to 2.5 meters in height.

Figure (3-1) shows the grouse shrub in the study area. The stem of the Guiera

Senegalensis plant contains many of the nodes that form outer branches have short oval,

gray-green leaves. This and others Features that distinguish the plant are used to

describe the grouse as a silvery-green plant Prominent in the Land of the Brush. The

Guiera Senegalensis plant grows naturally and intensively in the Al-Ghubaish area, Abu

Zabad locality and its surrounding areas Western Sudan, and locals consider it one of

the most important medicinal plants in the region.

Figure (3-1): Guiera senegalensis in Abu Zabad locality of Western Kordofan State,

Sudan.

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3.3 Study area:

3.3.1 description of the study area:

The city of Abu Zabad is located in the state of West Kordofan, and it is about 166

kilometers southwest of the city of Al Ubayyid, the capital of the state of North

Kordofan. The locality of Abu Zabad includes five administrators, and it is located

between the two circles of width 20-29 and between longitudes 16-19. show as fig(3.2) .

3.3.2 location map of the study area:

Figure (3.2) location map of the study area

3.4 The method of work

3.4.1The first step:

Ten samples were collected from three different sites randomly at three areas in West

Kordofan (Zaklouna, northwest of the Abu Zabad station transmutation power

electricity and Um Drouta) in Abu Zabad City. The sample was taken from the leaves

and then dried at room temperature for a few days to ensure complete dryness and

stored in plastic boxes illustrated in Figure (3.3), identified with symbols (A1, A2, A3, A4,

A5, A6, A7, A8, A9, A10), and then transferred to the technical oil laboratory to be prepared

by the XMET5000 device.

Figure (3.3) the leaves and then dried at room temperature for a few days to

ensure complete dryness and stored in plastic boxes illustrated in Abu Zabad City

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3.4.2 The Second step: X-MET5000

This light-weight, handheld EDXRF analyzer provides rapid, non-destructive,

point and shoot screening of plastics, PCBs, cables, plastic housings, solder material,

fasteners, sheet metal and other electronic components. When used in combination with

the powerful user interface it provides information for quick and reliable Go/No-Go

decisions. When testing non-uniform components, the X-MET5000 averaging feature

will give additional confidence to screening. A fully configurable user interface allows

the user to specify alarm limits and testing criteria. Data measured with the X-

MET5000 can be easily transferred to a PC for further inspection and report generation.

Rapid analysis and reporting avoids delays generally associated with laboratory based

analysis, allowing quick screening of a large number of samples. The X-MET5000 can

be taken to the sample wherever it is located. It can sort PVC and Br or Sb containing

plastics in seconds and helps to support the Waste Electrical and Electronic Equipment

(WEEE) recycling. Industries with high reliability exempt applications, like aerospace,

medical equipment and military systems, may use the X-MET5000 to ensure the

presence of adequate lead in their product components, especially in finishes and solder

joints for reasons of product safety and reliability as Show in fig (3.4) (Oxford

Instruments, 2008).

Figure (3.4) X-MET5000

3.4 Description X-MET5000:

The X-MET allows easy editing of the grade libraries, including the addition of new alloys and

naming of alloys. The integrated grade library contains:

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Nickel Alloys, Stainless Steels, Cobalt Alloys, Low Alloy Steel, Tool Steels, Copper Alloys,

Titanium Alloys, Zirconium Alloys, Aluminum Alloys. The X-MET is capable of storing

thousands of grade identifications and it’s easy to add new elements or to create a custom

library. The top of the range X-MET5100 combines Oxford Instruments’ groundbreaking

Silicon Drift Detector (SDD) with a powerful 45kV X-ray tube. This cutting edge technology

delivers a five times faster measurement speed, much better detection limits and significant

accuracy improvement over conventional systems. Isn’t it time you used X-MET to improve

your productivity?

Engineered for high performance and reliability, this hand-held XRF, analyser combines

Oxford Instruments’ patented Penta PIN® detector technology offering guaranteed fast

analysis and lower limits of detection for all elements of interest.

X-MET5000 portable X-ray detector was used to measurement and investigates the samples

was taken from study area. The X-MET5000 is hand-held EDXRF analyzer provides rapid,

non-destructive, point and shoots screening of plastics, PCBs, cables, plastic housings, solder

material, fasteners, sheet metal and other electronic components. When used in combination

with the powerful user interface it provides information for quick and reliable Go/No-Go

decisions. When testing non-uniform components, the X-MET5000 averaging feature will give

additional confidence to screening. A fully configurable user interface allows the user to

specify alarm limits and testing criteria. Data measured with the X-MET5000 can be easily

transferred to a PC for further inspection and report generation. Rapid analysis and reporting

avoids delays generally associated with laboratory based analysis, allowing quick screening of

a large number of samples. The X-MET5000 can be taken to the sample wherever it is located.

It can also be used as a quick, on-site, quality control tool to analyze other elements such as

Sn, Ag, Cu, Sb, Bi, etc., in solder and Cl, Ca, Sb, Ni, Sr, Zn, As and Ba in plastics and

components. It can sort PVC and Br or Sb containing plastics in seconds and helps to support

the Waste Electrical and Electronic Equipment (WEEE) recycling. Industries with high

reliability exempt applications, like aerospace, medical equipment and military systems, may

use the X-MET5000 to ensure the presence of adequate lead in their product components,

especially in finishes and solder joints for reasons of product safety and reliability. The X-

MET5000 can be taken to the sample wherever it is located. It can sort PVC and Br or Sb

containing plastics in seconds and helps to support the Waste Electrical and Electronic

Equipment (WEEE) recycling. Industries with high reliability exempt applications, like

aerospace, medical equipment and military systems, may use the X-MET5000 to ensure the

presence of adequate lead in their product components, especially in finishes and solder joints

for reasons of product safety and reliability (Oxford Instruments, 2008).

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3.4.1 High speed on-site measurement:

Rapid, simple on-site screening

• Directly from the ground

• In sample bags or cups

• Laboratory quality analytical data by measuring prepared samples in bench-top mode

• Analyze any sample type, including soil, rock, dirt, humus, sand, powder, liquid etc.

3.4.2 Rugged and reliable tool for fast analysis

• Withstands all weather conditions and rough treatment

• IP54 (NEMA 3) approved. Superior dust and moisture protection

• High-strength environmentally sealed housing

• Long battery operating time, charge indicator on battery and user interface.

3.4.3 High performance

• Fast, single-shot heavy element analysis:

Pb, Cr, Cu, Zn, Ni, Co, Mo, W, V, Mn, Fe, Ti, Nb etc.

• Fast measurement time: 30 – 120 seconds (X-MET5000) or 5 – 30 seconds.

• Low detection limits, X-MET5000 can typically detect 5 – 30 ppm concentration with

a 120s.

• High speed automatic averaging: Calculates averages of 2 - 50 measurements and

saves individual results and averaged results (Oxford Instruments Analytical Ltd,

2008).

Figure (3.5) color touch screen display visible

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Figure (3.6) Element ranges of X- Met 5000 and X- Met 5100

(Oxford instrument, 2009)

3.5 Sample preparation

XRF analysis is a physical method which directly analyses almost all chemical

elements of the periodic system in solids, powders or liquids. These materials may be

solids such as lass, ceramics, metal, rocks, coal, plastic or liquids, like petrol, oils,

paints, solutions or blood. With XRF spectrometer both very small concentrations of

very few ppm and very high concentrations of up to 100 % can directly be analyzed

without any dilution process.

In this study, the sample used is of Guiera senegalensis (Ghubaysh) of ten

samples from different areas around Abu Zabad City.

Figure (3.7) X-MET5000

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CHAPTER FOUR

RESULT ANDDISCUSSION

4.1 Introduction

The primary objective of this chapter is to present and discuss the results

obtained from the experimental work of this study on samples of Guiera senegalensis

(Ghubaysh) plant in Abu Zabad City in West Kordofan State.

4.2 Results

The ten samples of leaves Guiera senegalensis were analyzed by XRF the different is in

samples.

Table (4. 1): showing the concentration of elements in the sample (A1)

ELE Concentration% STD

Cr 0.07 0.028

Ni 0.00 0.000

Cu 0.01 0.002

Zn 0.43 0.002

Pb 1.25 0.002

Mn 0.00 0.018

Fe 0.45 0.018

Figure (4. 1) shows the concentration of sample (A1)

Cr Ni Cu Zn Pb Mn Fe

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

Co

ncen

tra

tion

mg

/g

ELE

Sample 1

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Table (4.2): showing the concentration of elements in the sample (A2)

ELE Concentration% STD

Cr 0.05 0.121

Ni 0.21 0.509

Mo 2.76 0.136

Cu 5.17 0.205

W 10.16 1.405

V 0.78 0.299

Mn 1.12 0.382

Fe 36.04 1.025

Figure (4.2) shows the concentration of sample (A2)

Cr Ni Mo Cu W V Mn Fe 0

5

10

15

20

25

30

35

40

Concentration mg/g

ELE

Sample 2

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Table (4.3) showing the concentration of elements in the sample (A3)

ELE Concentration% STD

Cr 0.04 0.021

Ni 1.27 0.001

Cu 2.1 0.001

Zn 0.23 0.002

Mn 0.00 0.013

Fe 1.63 0.042

Figure (4.3) shows the concentration of sample (A3)

Cr Ni Cu Zn Mn Fe 0.0

0.5

1.0

1.5

2.0

2.5

Concentration mg/g

ELE

Sample 3

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Table (4.4): showing the concentration of elements in the sample (A4)

ELE Concentration% STD

Cr 0.00 1.#00

Ni 0.59 1.#00

Mo 1.70 1.#00

Cu 0.09 1.#00

W 8.62 1.#00

V 0.93 1.#00

Mn 0.90 1.#00

Fe 12.37 1.#00

Figure (4.4) shows the concentration of sample (A4)

Cr Ni Mo Cu W V Mn Fe 0

2

4

6

8

10

12

14

Concentration mg/g

ELE

Sample 4

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Table (4.5): showing the concentration of elements in the sample (A5)

ELE Concentration% STD

Cr 0.05 0.120

Ni 0.02 0.385

Mo 4.13 1.122

Cu 0.95 0.285

W 4.03 1.027

V 0.80 0.300

Mn 1.66 0.378

Fe 9.37 0.887

Figure (4.5) shows the concentration of sample (A5)

Cr Ni Mo Cu W V Mn Fe 0

2

4

6

8

10

Concentration mg/g

ELE

Sample 5

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Table (4.6) showing the concentration of elements in the sample (A6)

ELE Concentration% STD

Cr 0.00 1.#00

Ni 0.00 1.#00

Mo 2.02 1.#00

Cu 0.32 1.#00

W 12.83 1.#00

V 1.22 1.#00

Mn 0.52 1.#00

Fe 86.21 1.#00

Figure (4.6) shows the concentration of sample (A6)

Cr Ni Mo Cu W V Mn Fe 0

20

40

60

80

100

Concentration mg/g

ELE

Sample 6

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Table (4.7): showing the concentration of elements in the sample (A7)

ELE Concentration% STD

Cr 0.08 0.001

Ni 0.01 0.003

Cu 0.23 0.002

Zn 0.01 0.001

Pb 0.08 0.003

Mn 0.06 0.026

Fe 2.19 0.051

Figure (4.7) shows the concentration of sample (A7)

Cr Ni Cu Zn Pb Mn Fe 0.0

0.5

1.0

1.5

2.0

2.5

Concentration mg/g

ELE

Sample 7

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Table (4.8): showing the concentration of elements in the sample (A8)

ELE Concentration% STD

Cr 3.11 0.140

Ni 8.61 0.456

Mo 2.11 0.130

Cu 0.32 0.277

W 3.52 0.956

V 4.09 0.240

Mn 0.30 0.303

Fe 2.09 0.877

Figure (4.8) shows the concentration of the sample (A8)

Cr Ni Mo Cu W V Mn Fe 0

2

4

6

8

10

Concentration mg/g

ELE

Sample 8

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Table (4.9): showing the concentration of elements in the sample (A9)

ELE Concentration% STD

Cr 21.91 0.734

Ni 1.71 0.147

Mo 0.12 0.016

Cu 0.17 0.065

W 0.20 0.111

Ti 0.11 0.098

V 0.06 0.096

Mn 0.85 0.364

Fe 23.02 0.707

Co 0.90 0.209

Nb 0.25 0.016

Figure (4.9) shows the concentration of sample (A9)

Cr Ni Mo Cu W Ti V Mn Fe 0

5

10

15

20

25

Concentration mg/g

ELE

Sample 9

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Table (4.10): showing the concentration of elements in the sample (A10)

ELE Concentration% STD

Cr 44.3 1.72

Ni 5.21 1.09

Mo 2.25 0.00

W 9.23 0.00

V 0.04 0.02

Ti 0.00 0.52

Fe 22.2 1.66

Figure (4.10) shows the concentration of sample (A10)

Cr Ni Mo W V Ti Fe

0

10

20

30

40

50

Co

ncen

tra

tion

mg

/g

ELE

Sample 10

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4.3 Discussion:

In this work different samples were giving and all data for these samples are

listed in tables and plotted in figures, while for the samples results will be presents the

measured values of concentration element.

plant leaves samples (A1) collected from Zaklouna village in Abu Zabad city

were analyses by X-MET5000, was reported in table (4.1) and plotted in figure (4.1)

.Hence, the result of concentration of (Pb, Fe, Zn, Cr, Cu, Mn) was to be (Avg STD)

(1.25 0.002, 0.45 0.018, 0.43 0.002, 0.07 0.028, 0.01 , 0.00 0.018%)

respectively . Upper comparing the results, the concentration of (Pb, Fe and Zn) was

higher than other element; the reason could be referenced to geological setting. Sample

(A2) collected from Zaklouna Village in Abu Zabad City, was reported in table (4.2)

and plotted in figure (4.2) results the high concentration of (Fe,W) to be founded

(36.04 1.025, 10.16 1.405%) were the low concentration of (Cu, Mo, Mn, V, Ni,

Cr) were (5.17, 2.76, 1.12, 0.78, 0.21, 0.05 0.205, 0.136, 0.382, 0.2999, 0.509,

0.121%) respectively. For sample (A3) collected from north west of the Abu Zabad

station transmutation power electricityin Abu Zabad City, was reported in table (4.3)

and plotted in figure (4.3) shows the high concentration of (Cu, Fe, Ni) was to be (2.1

0.001, 1.63 0.042, 1.27 0.001 %), on the other hand the low concentrations of the

(Zn, Cr, Mn) were to be (0.23, 0.04, 0.00 0.002, 0.021, 0.013%) respectively. Father

more for sample (A4) collected from north west of the Abu Zabad station transmutation

power electricity in Abu Zabad City, was reported in table (4.4) and plotted in figure

(4.4) .Hence, the result of high concentration of (Fe, W and Mo) to be (12.37 1.#00,

8.62 1.#00, 1.70 1.#00%) respectively, and the low concentrations of the (V, Mn, Ni,

Cu, Cr) ( 0.93, 0.90, 0.59, 0.09, 0.00 1.#00, 1.#00, 1.#00, 1.#00, 1.#00, 1.#00%)

respectively. Sample (A5) collected from north west of the Abu Zabad station

transmutation power electricity in Abu Zabad City, was reported in table (4.5) and

plotted in figure (4.5) results the high concentration of (Fe ,Mo and W) to be founded

(9.37 0.887 ,4.13 1.122 ,4.03 1.027%) were the low concentration of (Mn, Cu, V,

Cr, Ni) were (1.66, 0.95, 0.80, 0.05, 0.02 0.378, 0.285, 0.300, 0.120, 0.385%)

respectively. For sample (A6) collected from Um drouta samples in Abu Zabad City,

was reported in table (4.6) and plotted in figure (4.6) were to be the high

concentration of (Fe, W) was (86.21 1.#00,12.83 1.#00%) and the low

concentration of (Mo, V, Mn, Cu, Cr, Ni) were (2.02, 1.22, 0.52, 0.32, 0.00, 0.00

1.#00, 1.#00, 1.#00, 1.#00, 1.#00, 1.#00%) respectively. On the other had the sample

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(A7) collected from Um drouta samples in Abu Zabad City, was reported in table (4.7)

and plotted in figure (4.7) were results the high concentration of (Fe) to be founded

(2.19 0.051%) were the low concentration of (Cu, Pb, Cr, Mn, Ni, Zn) were (0.23,

0.08, 0.08, 0.06, 0.01, 0.01 0.002, 0.003, 0.001, 0.026, 0.003, 0.001%) respectively.

Sample (A8) collected from Um drouta samples in Abu Zabad City, was reported in

table (4.8) and plotted in figure (4.8) results the high concentration of (Ni) to be

founded (8.61 0.456%) were the low concentration of (V, W, Cr, Mo, Fe, Cu, Mn)

were (4.09, 3.52, 3.11, 2.11, 2.09, 0.32, 0.30 0.240, 0.956, 0.140, 0.130, 0.877,

0.277, 0.303%) respectively, sample (A9) collected from Um drouta samples in Abu

Zabad City, was reported in table (4.9) and plotted in figure (4.9) results the high

concentration of (Fe, Cr) to be founded (23.02 0.707, 21.91 0.734%) were the low

concentration of (Ni, Co, Mn, Nb, W, Cu, Mo, Ti, V) were (1.71, 0.90, 0.85, 0.25, 0.20,

0.17, 0.12, 0.11, 0.06 0.147, 0.209, 0.364, 0.016, 0.111, 0.065, 0.016, 0.098, 0.096%)

respectively. And sample (A10) collected from Um drouta samples in Abu Zabad City,

was reported in table (4.10) and plotted in figure (4.10) results the high concentration

of (Cr, Fe) to be founded (44.3 1.72, 22.2 1.66%) were the low concentration of

(W, Ni, Mo, V, Ti) were (9.23, 5.21, 2.25, 0.04, 0.00 0.00, 1.09, 0.00, 0.02, 0.52%)

respectively.

The results reported there are varieties in concentration of element from sample to

sample, this is attributed to the types of plants cultivated in those orchards, the

geological nature of the region.

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CHAPTER FIVE

CONCLUSIONS AND RECOMMENDATION

5.1 Conclusion

This study can do for elements in (Zaklouna, northwest of the Abu Zabad station

transmutation power electricity and Um drouta ) in Abu Zabad City, West Kordofan.

Devices as X MET 5000 which work on the principle of small and easy to use

and metallic items appear in a single measurement. Three different groups of Ghubaish

were analyzed according to regions (Zaklouna - north west of the Abu Zabad station

transmutation power electricity - Um drouta ) were (A1, A2 – A3, A4, A5 – A6, A7, A8,

A9, A10) respectively, were analyzed using x- ray fluorescence. The comparison was

done between these samples, a greet differences were found between this samples.

This great variation in the concentration of the studied elements (Fe, W, Cr,

Ni, Cu, Zn, Pb, Mn, Mo, V, Ti, Co, Nb) in the study areas. the highest concentration

was that of iron (Fe). It ranges between (0.45 mg/g ± 0.018%) in Zaklouna and (86.21

mg/g ± 1. #00%) in Um drouta, depending on the nature of the geographical location

and the human activities spread throughout the study area. While there was no

concentration recorded for the elements in six samples in three areas studied there

elements was (Pb, Zn, Ti, Co, Nb). In there are other four samples studied areas, the

highest concentration was that of lead (Pb) Which ranges between (1.25 mg/g ±

0.002%) in Zaklouna and (0.08 mg/g ± 0.003%) in Um drouta, And the concentration of

Zinc (Zn) ranged between (0.43 mg/g ± 0.002%) in Zaklouna and (0.01 mg/g ± 0.001%)

in Um drouta, The concentration of Titanium (Ti) was (0.11 mg/g ± 0.098%), and that

of Cobalt (Co) was (0.90 mg/g ± 0.209%), and that of Niobium (Nb) was (0.25 mg/g ±

0.016%), The confirms that the plant has any degree of toxicity and it is Safe to be used

medicinally

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5.2 Recommendation

The study recommended examining the concentration of elements in the

Ghubaysh plant by using different methods of spectrophotometry using other X-ray

devices that read a greater number of elements.

Based on the results obtained in this study, the study recommended that samples be

evaluated and measured at the study site by means of more X-ray line force detection

and spectrophotometers. Use X MET 5000 on other plants in this area to confirm the

concentrations of these elements. With a variety of sample selection methods.

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61

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