!"#  $  #

 

%&"#&
$#   '( 

) & %*&# 
  '

 ( 
  $
   

 

  +
""# ,  '"""#   -
'"""#
 
 

.'

.'
$
  
 
 '  (  
  (
  
 $ $  $
'
/ 
$# '
 

'
 
 #0

 '
//



 (
' 

 ($(
   $

 1
   
  2

 

 '

/  ((  
 '(( (   
  
   
0

 '
// '
 
    !"#
%&"#%*&# ( 
 

  ( + 3 ,3  
-3
 
((   /
   /
     
 .'
 
 0



 

04%.1' 
% -(!5
/
(
6'(!(0 0
10%& % 0!(0 07(
60%6'

 (

 %1
8'
 ('4
 
5
/
(".0
    



 
 





 


 !!"#$ !!!" % !!!"


 




 

 

 
   

 
   
 

 


 
  

 

 
 




 ! 

 

"



 
# 

 

$  !%
 !

   
& 
$

'  

 
'  

($
 

' 

# %
 %
)   %
*  %
'  
  $


'
 

 

+ 
 


" %
 
 
 

&

'  !

#  




  
$,

 

( 

$


  

 
 
-
 
 
   
. 
 
   

 
 

 
 
  

 
  
 

  

 


 ! 

"-
 
 


 


 


(

  %
 

 



  


  


 


. 



 
 %

 %

 %
 
 %




$ 

  
 

 
$



$ -




 
 

 
 -

 






  

 

 


 


-
-
/

/
 
$$$   
0 

 
1"
1"#23.
" 
 







  


4&
)*
5
/
+)

  
 6
78%
99:::
& %
  

) 2 

; 
*
 

&




 
 


<

"
-
   %=-


   %
7>:9
/- 
?
7>:9
4&
)*
5
/
+)
"
3 
 

"
 

& 
7>:9

Extraction and Spectrophotometric determination of Zn(II),La(III) and

Ce(III) Ions using New Organic Reagent in Different analytical Samples
Dr.Sahar Aqeel Hussein Al-aasam

Dr. Rafi K. Al-Kubaisy

Dr.Taghreed H. Al-Noor

List of Contents
Subject
1-1
1-2
1-3
1-4
1-5
1-6
1-7
1-8
1-9
1-9-1
1-9-2
1-9-3
1-10

Subject
2-1
2-1-1
2-1-2
2-1-3
2-1-4
2-1-5
2-2
2-3
2-3-1
2-3-2
2-3-3

Chapter One:- Introduction

Solvent extraction
Distribution coefficients and distribution ratios
Percentage of extraction(E)
Chemical interactions in the aqueous and
organic phases
Extraction systems
Extraction equilibria
Organic solvent choose
Azo compound
Chemistry of the elements
Chemistry of Zinc
Chemistry of Lanthanum
Chemistry of Cerium
Literatures review
Aim of the work

Chapter Two:- Experimental part

Instruments
UV-Visible spectrophotometer
Fourier transform infrared spectrophotometer
Atomic absorption spectrophotometer
CHN/O analyzer
Other supplementary equipments used in this work
Chemicals
Synthesis of organic reagents
Synthesis of 2-[4-bromo-3,5-diethylphenylazo]4,5diphenyl imidazole ( BDPI)
Synthesis of 2- [(4- Benzyloxy phenyl)azo]- 5nitro-4-phenyl imidazol (BANI)
Synthesis of4-[N-(5-methyl isoxazol-3-yl) benzene
4


No.Page
11
12
13
13
14
15
15
16
17
17
19
20
21
28

Page
29
29
29
29
29
29
30
30
30
31
32

sulfonamide azo]-1- Naphthol . (AMBN)

2.4
Extraction of Zinc(II)
2-4-1
Desired solutions
2-4-2
UV-visible spectrophotometry
2-4-3
Dithizone spectrophotometric method
2-4-4
The main method for extraction of Zn(II)
2-4-5
Parameters optimization of solvent extraction
2-4-5-1
Effect of acidic function
2-4-5-2
Effect of Zn(II) concentration
2-4-5-3
Effect of shaking time
2-4-5-4
Stoichiometry
2-4-5-5
Effect of organic solvent
2-4-5-6
Temperature Effect
2-4-5-7
Methanol effect
2-4-5-8
Effect of interference study
2-4-5-9
Effect of electrolytic salts
2-4-5-10
Synergism effect
2-4-6
Preparing of calibration curve for Zn (II) for
spectrophotometric determination
2-5
Extraction of La(III)
2-5-1
Desired solutions
2-5-2
UV-visible spectrophotometry
2-5-3
Arsenazo ( III ) spectrophotometric method
2-5-4
The main method for extraction of La(III)
2-5-5
Parameters optimization of solvent extraction
2-5-5-1
Effect of acidic function:2-5-5-2
Effect of La(III) concentration
2-5-5-3
Effect of shaking time
2-5-5-4
Stoichiometry
2-5-5-5
Effect of organic solvent
2-5-5-6
Temperature effect
2-5-5-7
Methanol effect
2-5-5-8
Effect of interference study
2-5-5-9
Effect of electrolytic salts
5


33
33
34
34
34
35
35
35
35
36
37
37
38
38
38
38
39
39
39
39
40
40
41
41
41
41
41
43
43
43
43
44

2-5-5-10
2-5-6

Synergism effect
Preparing of calibration curve for La(III)for
spectrophotometric determination
2-6
Extraction of Ce(III)
2-6-1
Desired solutions
2-6-2
UV-visible spectrophotometry
2-6-3
8-Hydroxyquinoline spectrophotometric method
2-6-4
The main method for extraction of Ce(III)
2-6-5
Parameters optimization of solvent extraction
2-6-5-1
Effect of acidic function
2-6-5-2
Effect of Ce(III)concentration
2-6-5-3
Effect of shaking time
2-6-5-4
Stoichiometry
2-6-5-5
Effect of organic solvent
2-6-5-6
Temperature effect
2-6-5-7
Methanol effect
2-6-5-8
Effect of interference study
2-6-5-9
Effect of electrolytic salts
2-6-5-10
Synergism effect
2-6-6
Preparing of calibration curve for Ce(III)for
spectrophotometric determination
2-7
Preparation of samples solution for determination
of Zn(II),La(III) and Ce(III)
2-8
Sample collection and preservation Water and soil
2-9
Spectrophotometric Determination of Zn(II)
,La(III) and Ce(III) in different samples

Subject
3-1-1
3-1-2
3-1-3

Chapter Three
Zinc(II)
Spectrophotometric studies
Calibration curve of Zn(II):
Optimum conditions for extraction efficiency of
Zn2+
6


44
44
44
44
45
45
45
46
46
46
46
47
48
48
49
49
49
49
50
50
50
50

Page
51
54
54

3-1-3-1
3-1-3-2
3-1-3-3
3-1-3-4
3-1-4
3-1-5
3-1-6
3-1-7
3-1-8
3-1-9
3-1-10
3-1-11
3-1-12
3-1-12-1
3-1-12-2

Effect of acidic function

Effect of metal ion concentration
Effect of shaking time
Stoichiometry
Effect of organic solvent
Temperature effect
Methanol effect
Effect of interferences
Effect of electrolyte salts
Synergism effect
Effect of organic reagent
Spectrophotometric studies
Optimum conditions for extraction efficiency of
Zn2+
Effect of acidic function
Effect of metal ion concentration

54
56
57
58
63
66
68
69
70
71
72
73
73
73
75

3-1-12-3

Effect of shaking time

78

3-1-12-4
3-1-13
3-1-13-1
3-1-13-2
3-2-1
3-2-2
3-2-3

Stoichiometry
Spectrophotometric determination
Calibration curve of Zn(II)
Determination of Zn(II)in the selected samples
Spectrophotometric studies
Calibration curve of La(III)
Optimum conditions for extraction efficiency of

79
84
84
85
89
92
93

3-2-3-1
3-2-3-2
3-2-3-3
3-2-3-4
3-2-4
3-2-5
3-2-6
3-2-7

La3+
Effect of acidic function
Effect of metal ion concentration
Effect of shaking time
Stoichiometry
Effect of organic solvent
Temperature effect
Methanol effect
Effect of interferences
7


93
94
96
97
101
104
106
107

3-2-8
3-2-9
3-2-10
3-2-11
3-2-12
3-2-12-1
3-2-12-2

Effect of electrolyte salts

Synergism effect
Effect of organic reagent
Spectrophotometric studies
Optimum conditions for extraction efficiency of
La3+
Effect of acidic function
Effect of metal ion concentration

108
109
110
111
111
111
113

3-2-12-3

Effect of shaking time

3-2-12-4
3-2-13
3-2-13-1

Stoichiometry
Spectrophotometric determination
Calibration curve of La(III)

3-2-13-2

Determination of La(III))in the selected samples

123

3-3-1
3-3-2
3-3-3

Spectrophotometric studies
Calibration curve of Ce(III)
Optimum conditions for extraction efficiency of

124
127
128

3-3-3-1
3-3-3-2
3-3-3-3
3-3-3-4
3-3-4
3-3-5
3-3-6
3-3-7
3-3-8
3-3-9
3-3-10
3-3-11
3-3-12
3-3-12-1

Ce3+
Effect of acidic function
Effect of metal ion concentration
Effect of shaking time
Stoichiometry
Effect of organic solvent
Temperature effect
Methanol effect
Effect of interferences
Effect of electrolyte salts
Synergism effect
Effect of organic reagent
Spectrophotometric studies
Optimum conditions for extraction efficiency of
3+
Ce
Effect of acidic function
8


115
117
122
122

129
130
131
132
137
140
142
143
144
145
146
146
147
147