Solvent Extraction of Zn(II),La(III) and Cd(III).

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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