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العنوان
Synthesis and characterization of some New Azo Compounds and their Metal Chelates /
المؤلف
Ali, Eman Ali Mohamed.
هيئة الاعداد
باحث / إيمان على محمد على
مشرف / مصطفي إبراهيم مصطفي
مناقش / سيد أحمد عبدالعزيز شامة
مناقش / محمد أحمد قاسم
الموضوع
chemistry.
تاريخ النشر
2014.
عدد الصفحات
151 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
Analytical Chemistry
تاريخ الإجازة
1/1/2014
مكان الإجازة
جامعة بنها - كلية العلوم - الكيمياء التحليلية
الفهرس
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Abstract

Synthesis and characterization of some new azo
compounds and their metal chelates
This thesis consists of three main chapters
Chapter 1
The introduction; in which a literature survey about the preparation, characterization and spectral behavior of azo compounds and their metal chelates is introduced. This chapter includes also hints about the previous studies carried out on the application of azo compounds in micro determination of metal ions.
Chapter 2
This is the experimental part of the thesis. It includes detailed description of the instruments used, methods of preparation of azo compounds and solutions as well as the experimental techniques used throughout the work.
Chapter 3
In which the results obtained and their discussion are introduced. This chapter is divided into three main parts.
Part (A): deals with the preparation and characterization of four azo compounds prepared from 2,4-dihydroxybenzoic acid as a coupler and four aniline derivatives as diazonium salts (m-nitro, p-hydroxy, p-carboxy and p-methyl). The prepared azo compounds were characterized by elemental analysis, electronic absorption spectra in ethanol and different organic solvents, IR spectra and 1H NMR spectra. The acid dissociation constants (pKH) of the azo compounds were determined from the spectral behavior in buffer solutions using the limiting logarithmic, half – height and Colleter methods.
Part (B):deals with the use of the prepared azo compounds in the spectrophotometric determination of Co2+, Ni2+ and Cu2+ as an analytical application. The optimum conditions favoring the formation of soluble colored complexes such as:
- Effect of pH
- Determination λmax at which complex species absorb
- Effect of time and temperature on the complex formation
- Effect of reagent concentration, sequence of addition, buffer type and buffer volume.
- Determination of the stability constants of the formed complexes
Verification of Beer’s lawwere extensively studied.
The new method allows the determination of the metal ions
Cobalt(II),Nickel(II) and Cooper (II) under investigation up to 80,90 And 90 µg/ml respectively.
Part (C): deals with the synthesis and characterization of the solid complexes formed between Co2+, Ni2+ and Cu2+ and the azo compounds under investigation. The chemical structure of the solid chelates was elucidated from elemental analysis, molar conductivity, thermogravimetric analysis and IR spectroscopy. The formation of complexes was firstly confirmed from conductometric titration.
SUMMARY
Synthesis and characterization of some new azo
compounds and their metal chelates
This thesis consists of three main chapters
Chapter 1
The introduction; in which a literature survey about the preparation, characterization and spectral behavior of azo compounds and their metal chelates is introduced. This chapter includes also hints about the previous studies carried out on the application of azo compounds in micro determination of metal ions.
Chapter 2
This is the experimental part of the thesis. It includes detailed description of the instruments used, methods of preparation of azo compounds and solutions as well as the experimental techniques used throughout the work.
Chapter 3
In which the results obtained and their discussion are introduced. This chapter is divided into three main parts.
Part (A): deals with the preparation and characterization of four azo compounds prepared from 2,4-dihydroxybenzoic acid as a coupler and four aniline derivatives as diazonium salts (m-nitro, p-hydroxy, p-carboxy and p-methyl). The prepared azo compounds were characterized by elemental analysis, electronic absorption spectra in ethanol and different organic solvents, IR spectra and 1H NMR spectra. The acid dissociation constants (pKH) of the azo compounds were determined from the spectral behavior in buffer solutions using the limiting logarithmic, half – height and Colleter methods.
Part (B):deals with the use of the prepared azo compounds in the spectrophotometric determination of Co2+, Ni2+ and Cu2+ as an analytical application. The optimum conditions favoring the formation of soluble colored complexes such as:
- Effect of pH
- Determination λmax at which complex species absorb
- Effect of time and temperature on the complex formation
- Effect of reagent concentration, sequence of addition, buffer type and buffer volume.
- Determination of the stability constants of the formed complexes
Verification of Beer’s lawwere extensively studied.
The new method allows the determination of the metal ions
Cobalt(II),Nickel(II) and Cooper (II) under investigation up to 80,90 And 90 µg/ml respectively.
Part (C): deals with the synthesis and characterization of the solid complexes formed between Co2+, Ni2+ and Cu2+ and the azo compounds under investigation. The chemical structure of the solid chelates was elucidated from elemental analysis, molar conductivity, thermogravimetric analysis and IR spectroscopy. The formation of complexes was firstly confirmed from conductometric titration.