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تحضير مشتق جديد للبايروزولون ازو واستعماله في تقدير الكميات الضئيلة لبعض الايونات الفلزية بالطرائق الطيفية == Preparation of New Pyrozolone Azo Derivative And Use It For Micro Determination of Some Metal Ions By Spectrophotometric Methods
Author name:
شيماء حسن ملاح
Supervisor name:
حسين جاسم محمد
General topic:
Chemistry
Specific topic:
Chemistry
Degree:
Master
University:
University of Al-Qadisiyah - Faculty Of Education - Chemistry Department
Language:
Arabic
University location:
Qadisiyah
First pages:
25T1511 - p.pdf
Abstract:
تضمن البحث تحضير الكاشف الجديد 3 - (?4 - انتي بايرايل ازو) - 1 - نايتروزو - 2 - نفثول واجراء دراسة اولية مع (9) ايون فلزي واستحداث طريقة طيفية لتقدير كل من النحاس (II) والكوبلت (II) بهذا الكاشف في الوسط المائي، اذ كان الطول الموجي الاعظم للكاشف (374) نان | The research includes primary study of the reaction of 3 - (4? - Antipyriyl azo) - 1 - Nitroso - 2 - naphthol (APANN) with (9) metal ions and spectrophotometric method for the determination of copper (II) and Cobalt (II) ions with this reagent. The wavelength of maximum absorption (?max) for the reagent is (374) nm and for complexes formed between these ions with this reagent was found at (430.5) nm and (432) nm for both copper (II) and Cobalt (II( respectively in aqueous medium, also the optimum conditions for the reaction of these ions with the reagent were employed ,such as the volume of reagent solution, time, temperature, type of buffer, order of addition and effect of pH, calibration curves of these complexes were constructed. Beer's law was obeyed in the range (0.1 - 2.5) ppm of copper with a correlation coefficient (R2= 0.9971) and molar absorptivity ? = 1.83 × 104 L.mole - 1.cm - 1 and Sandell sensitivity was (0.00349) ?g.cm2 - , as for Cobalt, the range was (0.1 - 2.5) ppm with a correlation coefficient (R2= 0.9965) and molar absorptivity ? = ) 3.3×104 ( L.mol - 1.cm - 1 ,and Sandell sensitivity was (0.0018)µg.cm - 2. The stoichiometry of the formed soluble complexes between copper (II) and Cobalt(II) with reagent was investigated by both the continuous variations method and mole ratio method, the ratio (M : L) was (1 : 2) for Copper complex and Cobalt complex at pH (8.5) for both complexes. The stability constant (Ksta) for the complexes of copper (II) and Cobalt (II( was equal to (8.237 ×108 L.mol - 1) and (1× 108 L.mol - 1) respectively. Precision and accuracy of the analytical procedure were showed for (0.5) ppm of Cu (II) and Co (II) that R.S.D.% was equal to (0.97), (0.73) , (Erel, Re)% (0.6, 99.4)%, (0.4, 99.6)% for these ions, respectively. The analytical procedure were showed for (1) ppm of Cu (II) and Co (II) R.S.D.% was equal to (0.41,0.60) , (Erel, Re)% (0.3, 99.7)%,(0.2, 99.8)% for these ions respectively. The interference of metal ions in the presence of related ions was determined, as well as, masking of these ions by suitable masking agents was studied. The study of effect of three kinds of surfactants on the absorptions of the complexes and calculation of stability constants and treatment of the results statistically and make comparison with aqueous medium were done. The physical properties of precipitants were studied through the establishment of melting point, solubility and molar conductivity as well as the measurement of infrared spectra , and C.H.N, with the suggestion of structural formula of the formed complexes with the reagent (APANN). The method was applied for the determination of the content of copper (II) in tea leaves samples and Cobalt (II) in raw caw milk samples. Finally ,The biological activity of these complexes was tested with four types of bacteria.
