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تحري الخواص الحرارية لبعض السوائل الايونية الحاوية على اليوريا والاستمايد == Investigation of Thermal Properties for some Ionic Liquids containing Urea and Acetamide

Author name: هدى سلام عبد
Supervisor name: هادي محمد علي عبود
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Characterization of some room temperature ionic liquids (RTILs) as candidates for thermal storage media and heat transfer fluids in thermal applications were investigated. Five ionic liquids prepared from ammonium alum [NH4Al(SO4)2.12H2O] pronounced S, as inorganic salt with urea [NH2CONH2] pronounced U, or acetamide [CH3CONH2] pronounced A, as organic compounds, and aluminum nitrate [Al(NO3)3.9H2O] pronounced N with urea or acetamide compounds in different mole ratios were investigated alone and with addition of some improving materials to study their synergetic effect using thermo - gravimetric analysis (TGA), Differential Scanning Calorimetery (DSC), X - ray diffraction (XRD), Fourier Transform Infrared (FTIR) spectroscopy and conductivity measurements. Thermo - physical properties such as enthalpy ΔH, heat capacity Cp and thermal energy storage capacity were determined. It was found that hydrated aluminum nitrate : acetamide (1 : 22 mole ratio, AN2IL) alone and hydrated ammonium aluminum sulfate : urea (1 : 5 mole ratio, USIL) alone or with addition of some materials characterized with high density, chemical stability, heat capacity, thermal energy storage capacity and wide temperature range. The results indicated that ionic liquids alone or with addition of some materials could be considered as a promising candidate for liquid thermal storage media and heat transfer fluids.Studying the synergetic effect by addition of some alkali metal hydroxide (NaOH) with hydrated aluminum nitrate : urea (1 : 1.2 mole ratio, UNIL) and KOH with hydrated ammonium aluminum sulfate : urea (1 : 5 mole ratio, USIL) ionic liquids increased thermal energy storage capacity of these ionic liquids, while the addition of NaOH to hydrated aluminum nitrate : acetamide (1 : 22mole ratio, AN2IL) gave less thermal stability and storage capacity of ionic liquid.Also addition of alkaline earth metal oxide MgO, CaO to hydrated ammonium aluminum sulfate : urea (1 : 5 mole ratio, USIL) and BaO to hydrated aluminum nitrate : urea (1 : 1.2 mole ratio, UNIL) decreased thermal stability, heat capacity and thermal energy storage capacity than ionic liquid alone.Moreover, addition of transition metal oxide (VOSO4.5H2O, CuO and ZnO) to hydrated ammonium aluminum sulfate : urea (1 : 5 mole ratio, USIL) increased thermal stability and storage capacity of hydrated ammonium aluminum sulfate : urea (1 : 5 mole ratio, USIL), while the addition of NiO to hydrated ammonium aluminum sulfate : urea (1 : 5 mole ratio, USIL) only improve thermal stability of ionic liquid

التثبيت الضوئي لمتعدد كلوريد الفانيل باستخدام معقدات مخلبية == Photostabilization of poly(vinyl chloride) by chelate complexes

Author name: علي نجاح حسن
Supervisor name: عماد عبد الحسين يوسف السراج
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Five metal complexes of Cu(II), Cd(II), Zn(II), Ni(II) and Sn(II) with {4 - (Benzylidene - amino) - 5 - pyridin - 4 - yl - 4H - [1,2,4]triazole - 3 - thiol}, of Schiff base ligand (L), were prepared in alcoholic medium.The ligand (L) and its metal complexes were characterized qualitatively by using : FTIR, UV - visible spectroscopy, magnetic susceptibility, conductivity measurements and 1H NMR only for ligand. The ligand acted as bidentate which coordinated to the metal ions through sulphur and nitrogen of Azomethine group.According to the spectral data of the complexes a tetrahedral geometry was suggested for these complexes, except Cu(II) complex which exhibited octahedral geometry distorted to square planar structure.The metal complexes were used to enhance the photostabilization of PVC contains a concentration of ML2 0.5 % by weight. The photostabilization of PVC films were studied at room temperature under irradiation of light with λ=313 nmand an intensity of 7.75 X 10 - 7 einstein dm - 3 sec - 1.The photostabilization activity of these compounds was determined bymonitoring the carbonyl (ICO), polyene (Ipo) and hydroxyl (IOH) indices and weightloss method with irradiation time. It was found that the (ICO), (Ipo) and (IOH)indices values increased with irradiation time and this increase found to depends on the type of additives.The surface morphology for these films was studied during irradiation time.The changes in viscosity average molecular weight of PVC with irradiation time were also tracked (using THF as a solvent). The quantum yield of the chain scission (Φcs) of these complexes in PVC films was also evaluated.The following trend was obtained for the photostabilization effect on PVC films in presence of additives as shown below : CuL2 , CdL2 , ZnL2 , SnL2 , NiL2 Increasing the photostability According to the obtained experimental results, mechanisms were suggested, depending on the structure of the complexes.

الاكسدة الضوئية التحفيزية للفينول الاحمر على دقائق ثنائي اوكسيد التيتانيوم النانوبلوري == Photocatalytic Oxidation of Phenol Red on Nanocrystalline TiO2 Particles

Author name: احمـــد عبد الله حسين
Supervisor name: هـــلال شهاب وهاب
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: انجزت هذه الدراسة البحثية للتفكك الضوئي للصبغة العضوية الفينول الاحمر كنموذج للملوثات الفينولية وذلك باستخدام ثنائي اوكسيد التيتانيوم النانوي المحضر مختبريا وفي وسط مائي.استخدمت تقنيات تشخيصية عديدة مثل المجهر الالكتروني الماسح وحيود الاشعة السينية ومطياف الانتشار الانعكاسي والمجهر الالكتروني التنافذي وطيف رامان لدراسة شكل السطح والحجم الحبيبي والمساحة السطحية وطاقة الفجوة لثنائي اوكسيد التيتانيوم النانوي المحضر. وجد ان متوسط حجم الحبيبة هو 9, 9.95, 11 نانو باستخدام مجهر الالكتروني الماسح, مطياف الانتشار الانعكاسي وحيود الاشعة السينية على التوالي.وتم كذلك احتساب المساحة السطحية وحجم المسامات باستخدام منظومةBET حيث كانت النتائج للمساحة السطحية 48 م2\غم وحجم المسامات 3.7 نانو مما يؤكد كون ثنائي اوكسيد التيتانيوم النانوي ذات مسامات صغيرة. ((mesoporos.تمت دراسة تاثير العديد من المتغيرات التجريبية على عملية التفكك الضوئي مثل كمية ثنائي اوكسيد التيتانيوم النانوي, حامضية المحلول, التركيز الابتدائي للفينول الاحمر, شدة مصدر التشعيع, الحجم الحبيبي لثنائي اوكسيد التيتانيوم النانوي واضافة المؤكسدات.ثبتت الظروف التجريبية المثلى لعملية التفكك الضوئي لصبغة الفينول الاحمر عند الدالة الحامضية 4.5 والتركيز الابتدائي للفينول الاحمر مساويا الى 10.3 ملغم\لتر وكمية المحفز ثنائي اوكسيد التيتانيوم مساويا الى 500 ملغم\لتر, حيث تم الحصول على ثابت سرعة التفاعل بقيمة 0.01052 لكل دقيقة وعمر نصف العملية 1.098 ساعة عند الظروف المثلى.اوضحت دراسة حركية التفكك الضوئي للفينول الاحمر بان العملية من الدرجة الاولى. اضافة على ذلك تم احتساب الناتج الكمي لعملية التفكك الضوئي حيث تساوي 0.1.اظهرت النتائج بان عملية الاكسدة الضوئية للفينول الاحمر بواسطة ثنائي اوكسيد التيتانيوم النانوي تفضل كيمياء الهيدروكسيل لانه عند اضافة بيروكسيد الهايدروجين حفزت عملية التفكك وتحسنت وتاكيدا على هذا الكلام عند اضافة ايزو بروبانول ثبطت عملية تفكك الفينول الاحمر لانه يعتبر من اهم المثبطات لجذر الهيدروكسيل. وتم كذلك احتساب الدوال الثرموديناميكية الاساسية لعملية التفكك الضوئي للفينول الاحمر مثل طاقة التنشيط وطاقة جبس والانثالبي والانتروبي. | In the current research study, the photocatalytic (photodecolorization) degradation of the phenolic model ecotoxicant, phenol red dye has been investigated using laboratory synthesized anatase TiO2 nanoparticles in aqueous solution. The prepared nano TiO2 powder has been characterized using several advanced instruments including, Scanning Electron Microscopy (SEM), Energy Dispersive X - Ray Spectroscopy (EDXS), X - Ray Diffraction (XRD), Diffused Reflectance UV - VIS spectrometry (DUR - UV - VIS), Transmission Electron Microscopy (TEM), Brunauer - Emmett - Teller (BET) theory and Raman Spectrometry. Average particle size of 9, 9.95 and 11 nm was found using TEM, XRD and SEM, respectively. The surface area and pore size were also measured employing BET nitrogen adsorption apparatus which resulted in surface area of 48 m2/g and a pore size of 3.7 nm, which indicates the mesoporosity of the prepared nano anatase TiO2 particles. The impacts of several operational parameters for the photodegradation process were explored encompassing, TiO2 loading, solution pH, initial phenol red concentration, UV light source intensity, photocatalyst particle size and added oxidants. Under optimum experimental conditions, 4.5 solution pH, 500 mg/l TiO2 loading and 2.9 x 10 - 5 mol /l (10.3 mg/l) phenol red, the value of the apparent rate constant, kapp , obtained has been 0.01052 min - 1 (17.53x 10 - 5 sec - 1) and the half life of the process, accordingly is equal to 1.098 hours.The kinetic of phenol red photobleaching has also been studied and it was found that it follows the pseudo first order pattern regardless of reaction conditions. Furthermore, the apparent quantum yield for the photodecolorization process was also determined and found to be approximately 0.1.Results reveal that the photooxidation process of phenol red follows hydroxyl type chemistry in which the addition of hydrogen peroxide has contributed massively in the promotion of the process rate and yield, and further, suppressed to a great extent by addition of isopropanol as .OH radical scavenger.The main process activation thermodynamic parameters namely, Gibbs energy, enthalpy and entropy were also deduced following the computation of photolysis activation energy employing the well known Arrhenius relation.

تحري قنص غاز ثاني اوكسيد الكربون بواسطة السوائل الايونية عند درجة حرارة الغرفة == INVESTIGATION OF CO2 GAS CAPTURING BY ROOM TEMPERATURE IONIC LIQUIDS

Author name: ايفون اكرم عبد الجبار
Supervisor name: هادي محمد علي عبود
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Some ionic liquids were investigated for abilities to capture CO2 alone or with added some catalysts at room temperature under atmospheric pressure to increase the capacity of ionic liquids to capture carbon dioxide gas some catalysts were found effective such asHydrated aluminum nitrate/urea ionic liquid with added CaO and NaOH , monoethanolamine and ammonium chloride were added to hydrated ammonium aluminum sulphate/urea ionic liquid did not show in FTIR sign of either physical or chemical absorption of CO2 . The addition of NaOHaq to hydrated ammonium aluminum sulphate/urea ionic liquid showed a new vibration absorption at 1666 cm - 1 and changing the frequencies in the amine group vibrational bands above 3000 cm - 1 . While the distilled water when added to the ionic liquid hydrated ammonium aluminum sulphate/urea showed a broaden effect on the high vibrational bands above 2500 cm - 1 and the carbonyl group vibrational band at 1662 cm - 1 was not effected .Calcium oxide was added to hydrated ammonium aluminum sulphate/urea showed a new splitting vibration absorption bands at 1666 cm - 1 ,1618 cm - 1 .Aluminum chloride - urea ionic liquid very effective to capture carbon dioxide gas without add any catalysts showed a chemical absorption of CO2 1655 cm - 1 while aluminum chloride - acetamide showed weaker or no ability to capture CO2 .

تحضير مركبات عضوية اروماتية تحوي على ذرات غير متجانسة لغرض استخدامها كمثبطات للتاكل لمعدن الحديد في محلول حامضي == Preparation of Aromatic Organic Compounds containing Hetero - atoms as Corrosion Inhibitors for Mild Steel in Acidic Solution

Author name: حنان حسين علي
Supervisor name: مهدي صالح شهاب
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:

تحضير معقدات لاعضوية مشتقة من 4 - امين - 5 - بيريدايل 4,2,1 ترايزول - 3 - ثايول ودراسة الثباتية الضوئية - 4H - لها لبوليمر البولي ستايرين == Synthesis of inorganic complexes derived from 4 - amino - 5 - (pyridyl) - 4H 1,2,4 triazole - 3 - thiol and study their photochemical stability with polystyrene

Author name: رغد علي عبد الرسول حداد
Supervisor name: عماد عبد الحسين يوسف السراج
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Five transition metal complexes of Ni(II), Cu(II), Zn(II), Cd(II) and Sn(II) with {4 - amino - 5 - (pyridyl) - 4H - 1,2,4 - triazole - 3 - thiol}, as a ligand (L) has been prepared in alcoholic medium. These complexes are : 1. Bis(4 - amino - 5 - (pyridyl) - 4H - 1,2,4 - triazole - 3 - thiol) Nickel(II), Ni(L)2 .2. Bis(4 - amino - 5 - (pyridyl) - 4H - 1,2,4 - triazole - 3 - thiol) Cupper(II), Cu(L)2 .3. Bis(4 - amino - 5 - (pyridyl) - 4H - 1,2,4 - triazole - 3 - thiol) Zinc(II), Zn(L)2 .4. Bis(4 - amino - 5 - (pyridyl) - 4H - 1,2,4 - triazole - 3 - thiol) Cadmium(II), Cd(L)2 .5. Bis(4 - amino - 5 - (pyridyl) - 4H - 1,2,4 - triazole - 3 - thiol) Tin(II), Sn(L)2 .The ligand (L) and its metal complexes were characterized quantitatively and qualitatively by using : FTIR, UV - visible spectroscopy, 1H and 13C NMR, magnetic susceptibility and conductivity measurements. This ligand act as bidentate that coordinated to the metal ions through sulphur and nitrogen of amine group. According to the spectral data of the complexes a tetrahedral geometry was suggested for these complexes except Cu(II) complexes which exhibit a square structure.In this work the prepared complexes of 4 - amino - 5 - (pyridyl) - 4H 1,2,4 triazole - 3 - thiol were used to enhance the photostabilization of Polystyrene (PS).Polystyrene has been mixed with these complexes in chloroform solvent which containing concentration of complex 0.5 % by weight, which produced by the casting method from chloroform solvent. The photostabilization of polystyrene films were studied at room temperature under irradiation of light λ=365 nm wave length with intensity 20.6*10 - 9 Ein Dm - 3 S - 1 .The photostabilization activity of these compounds was determined by monitoring the carbonyl (ICO) and hydroxyl (IOH) indexes, weight loss method with irradiation time. It was found that the (ICO) and (IOH) indexes values increased with irradiation time and this increase depend on the type of additives. The surface morphology for these films was studied during irradiation time. The changes in viscosity average molecular weight of PS with irradiation time were also tracked (using chloroform as a solvent). The quantum yield of the chain scission (Φcs) of these complexes in PS films was also evaluated.The following trend is obtained for the photostabilization effect on PS films in presence of additives as shown below : Sn(L)2 , Cd(L)2 , Ni(L)2 , Zn(L)2 , Cu(L)2 Increasing the photostability According to the experimental results obtained, mechanisms were suggested, depending on the structure of the complexes

تصنيع ودراسة اقطاب بوليمرية جديدة لتقدير الكلاريثرومايسين == Construction and study of new polymeric membrane electrodes for clarithromycin determination

Author name: حيدر قيس منشد
Supervisor name: خالدة حميد محمد السعيدي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: This piece of research includes constructing and characterizing two kinds of ion - selective electrodes (ISEs) based on PVC matrix membrane.First, four ion - selective electrodes for clarithromycin (CLM) which based on clarithromycin - tetraphenylborate (CLM - TPB) ion - pair complex as the electro - active materials were prepared. Second, four ion - selective electrodes for clarithromycin which based on using clarithromycintetraiodomercurate (CLM - TIM) ion - pair complex as the electro - active materials were also prepared. In both kinds of ISEs, some of the selected plasticizers were employed such as; Di - octyl phthalate (DOP), Di - butyl phosphate (DBP), Acetophenone (AP) and Di - butyl phthalate (DBPH) in PVC matrix. This thesis has mainly been structured in three different chapters, each one containing the following information : Chapter one provides a short historical review with the analytical performance characteristics of ISEs are described. The applications of ISEs in pharmaceutical and clarithromycin analyses are well - arranged in tables and the general and specific objectives of thesis are reported. Chapter two corresponds to the experimental part. Reagents, instruments, procedures and detail protocols for the preparation of two kinds of ISEs used in this study are reported.Chapter three contains the experimental results and discussion that lead to the possibility of successful applications the constructed ISEs in pharmaceuticals preparation and clarithromycin measurements. It is reporting the construction of two kinds of larithromycin ISEs; The first kind ISEs were : CLM - TPB+DOP (E1), CLM - TPB+DBP (E2), CLM - TPB+AP (E3) and CLM - TPB+DBPH (E4), give the linear range from (1×10 - 5 - 1×10 - 3, 1×10 - 5 - 1×10 - 3, 5×10 - 5 - 1×10 - 3 and 1×10 - 5 - 1×10 - 3 M), the slopes of (51.206, 53.930, 58.104 and 58.484 mV/decade) respectively, with detection limits of (8×10 - 6, 6×10 - 6, 2×10 - 5 and 9×10 - 6 M), response time of 10 - 3 M (30, 35, 41 and 46 second) and the lifetime were about (24, 30, 12 and 20 days) respectively. The second, were : CLM - TIM+DOP (E5), CLM - TIM+DBP (E6), CLM - TIM+AP (E7) and CLM - TIM+DBPH (E8), give the linear range from (1×10 - 5 - 1×10 - 3, 5×10 - 5 - 1×10 - 3, 5×10 - 5 - 1×10 - 3 and 1×10 - 5 - 1×10 - 3 M), the slopes of (48.445, 42.970, 52.692 and 49.442 mV/decade) respectively, with detection limits of (5×10 - 6, 5.5×10 - 5, 5×10 - 5 and 1.5×10 - 5 M), response time of 10 - 3 M (26, 32, 30 and 48 second) and the lifetime were about (28, 22, 16 and 25 days) respectively.The best electrode is (E4) used to determine the clarithromycin in pure and pharmaceuticals samples. The working pH for (E4) electrode was ranged from (1.5 - 6.5), the selectivity coefficients (Kpot A,B) of ISEs for the CLM have been studied in the presence of interference ions (Na+, K+, Mn+2, Cu+2, Fe+3, Al+3, sucrose and gelatin) by using separated solution and fixed interfering methods and the results was ranged from (4.28×10 - 2 - 8.82×10 - 5), which revealed that there was no effect of the interferences on the determination of CLM in tablets by using the constructed ISE.Therefore the ISE (E4) gave a good electrochemical characterization among the others and it has been used successfully for the determination of clarithromycin in the Claricide tablets using different potentiometric methods.

دراسة طيفية لبعض املاح العناصر الانتقالية في السائل الايوني == SPECTROSCOPIC INVESTIGATION FOR SOME TRANSITION METAL SALTS IN IONIC LIQUID

Author name: مروة حميد فاضل
Supervisor name: هادي محمد علي عبود
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Aluminum chloride - urea ionic liquid was investigated by Lewis acid - base titration with chloride ions for its active species concentration with the aide of electronic spectroscopy. A coordination bonds between aluminum cationic species of the ionic liquid and the aromatic ring of toluene or benzene was assumed to be responsible for new bands formed in visible and ultraviolet regions.Upon Lewis acid - base titration these bands was found to disappear and the concentration of the acidic species therefore was elucidated to be around 75 mole % of the initial aluminum chloride used to prepare a 1.5 mole aluminum chloride to 1 mole urea ionic liquid. The product of this reaction was assumed to be between mole acidic species to mole chloride ion according to the mole fraction elucidated graph.The behavior of some transition metal compounds (chlorides and sulfates) of (Cu(II), Co(II) and Ni(II)) coordination in the ionic liquid was also investigated in this ionic liquid by electronic spectroscopy. Cobalt chloride showed a different behavior than the distorted octahedral geometry of copper chloride as it reacted with the anionic species to precipitate as form of a tetrahedral complex containing urea, aluminum and chloride ions.The behavior of nickel sulfate in the ionic liquid also showed an acid - base reaction with the acidic species of ionic liquid as the bands at 334 nm and 474 nm decreased with increasing the salt concentration. The coordination of Ni(II) cation was found to be an octahedral geometry with stronger ligand field effect. Similar strong ligand field was also observed with copper sulfate which showed four bands resulted from separating metal d - orbitals more obviously than the tetragonal John - Teller effect found with copper chloride in same ionic liquid.

الخواص الثرموديناميكية والحجمية لبعض الفيتامينات الذائبة - مائيا في حامض الهيدروكلوريك المخفف وكذللك في المحاليل المائيه لملح كلوريد الصوديوم عند درجات) 51.392 و51.392 و1.392 . و1.392 . (كلفن == Thermodynamic and Volumetric Properties of Some Water - Soluble Vitamins in Dilute HCl and in Aqueous NaCl Solutions at (293.15, 298.15, 303.15, and 308.15) K

Author name: خطاب عدنان عبد
Supervisor name: تغريد علي سلمان
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Densities , ρ, and viscosity, η, have been measured for ascorbic acid, thiamin HCl, nicotinic acid and pyridoxine HCl have been measured in water and in aqueous sodium chloride solutions at (293.15, 298.15, 303.15 and 308.15) K. The apparent molar volumes were determined from the measured density data. These volumes were extrapolated to zero using suitable empirical or theoretical equations to determine the corresponding infinite dilution values.Ionization of the vitamins under studied were suppressed using sufficiently acidic solutions. Apparent molar volume at infinite dilution for all vitamins, were found to be increase with increasing temperature in acidic solution and the presence of co - solute NaCl. On the other hand, increasing the concentration of co - solute NaCl leads to decrease the apparent molar volumes. These results were interpreted in terms of complex vitaminswater - co - solute NaCl interactions.Apparent molar volumes of transfer at infinite dilution for vitamins from water solutions to NaCl solution at various temperatures in the range (293.15 - 308.15) K were calculated. The resulting data have been utilized to the effect of overlapping of the hydration co - spheres on net volume of vitamins. The viscosity data have been analyzed using Jones - Dole equation, and the derived parameters, Jones - Dole coefficient, B, and Falkenhagen coefficient, A, were interpreted in terms of solute - solvent and solute - solute interactions respectively, for ascorbic acid, thiamin HCl, nicotinic acid and pyridoxine HCl. The variation of B coefficient with temperature, (dB/dT), have been also calculated for vitamin solutions, and the obtained data was interpreted on the basis of the structure - making and structure - breaking behavior.Free energy of activation of viscous flow per mole of solvent, Δμ1°, and solute, Δμ2°, were obtained by application of the transition - state theory to the B coefficient data and the corresponding activation enthalpy, ΔH0, and entropy of activation, ΔS0, of viscous flow were also determined for vitamins.

مثبتات ضوئية جديدة لبولي كلوريد الفانيل باسخدام بعض ايونات العناصر لمعقدات2 - 6 - ميثوكسي نفثالين - 2 - وايل بروبانويت

Author name: حسام اكريم سلمان
Supervisor name: عماد عبد الحسين يوسف السراج | جواد كاظم شنين
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: The preparation of Bis[2 - (6 - methoxynaphthalen - 2 - yl)propanoate] chelate complexes with nickel(II), copper(II), zinc(II), cadmium(II) and tin(II) were described in this thesis.Infrared, ultraviolet - visible, spectrophotometric techniques, magnetic susceptibility, atomic absorption, conductivity measurements and melting point were used to characterize the free ligand and the above chelate complexes. All these complexes were found to act as stabilizer in PVC films.The light of wavelength (313 nm) with intensity of (1.052×10 - 8 ein.dm - 3.S - 1) was used for irradiation of polymer films at room temperature. The rate of photodegradation and photostabilization of PVC film (thickness 30 m) were monitored by measuring the carbonyl, polyene, hydroxyl and chlorine indices (Ico, Ipo, IoH and Icl) values as a function of irradiation time and ultraviolet - visible spectrophotometry using 0.5% wt/wt concentration of stabilizer.It was found that the carbonyl index (Ico), polyene index (Ipo) and hydroxyl index (IoH) values increased with irradiation time, while the chlorine index (ICl) values decreased with irradiation time, and this increase depend on the type of additives (free ligand and complexes).The following trend was obtained for the photostabilization effect of PVC film in presence of these additives : Cd(L)2 > Zn(L)2 > Sn(L)2 > Ni(L)2 > Cu(L)2.According to the experimental results obtained several mechanisms were suggested depending on the structure of the additives. Among these mechanisms, HCl scavenging, UV absorption, peroxide decomposer and radical scavenger for photostabilizer additives.The mode of chain scission was also investigated by measuring the variation of average viscosity molecular weight with irradiation time for PVC films with and without additives. It was found that the values of the variation of average viscosity molecular weight decreased with increasing irradiation time

تحليل الطيف الالكتروني لمركبات ايونات بعض العناصر الانتقالية في سائل ايوني جديد

Author name: زينة نذير رجب
Supervisor name: هادي محمد علي عبود
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: The behavior of some transition metal cations [Cr (III), Fe (III), Fe (II), Co (II), Ni (II) and Cu (II)] were investigated in ammonium alum - urea ionic liquid. The study was followed by UV - Visible electronic spectroscopy to establish their coordination geometry in the liquid and estimate the ionic species attached to the transition metal cations.The reactivity of the metal cations were found to vary from one to another. Chromium (III) cation was found, (as expected) to be in octahedral geometry with ionic liquid species and was inert toward the addition of ligands. Similarly iron (III) did not show a tendency to react with added ligands, yet charge transfer was prevailed. However, interesting iron (II) showed high spin octahedral coordination with thiocyanate ion but a low spin octahedral complex with nitrite ion.Cobalt (II) showed an interesting behavior in alum - urea ionic liquid, as it coordinated in an octahedral geometry with its ionic species. A gradual geometrical changes were appeared as a major change in their spectra most probably forming a mixture of two species tetrahedral with some original octahedral complex when its solution was studied with increasing thiocyanate ion concentration up to 35 thiocyanate : 1 cobalt mole ratio.The solubility limit of nitrite in ionic liquid ceased the concentration ratio of nitrite : cobalt to be 5 : 1.Nickel (II) also showed an octahedral geometry behavior in ionic liquid species. It reacts with added ligands particularly when theconcentration of thiocyanate ion : Ni (II) increased up to 30 to 1 mole ratio, the color changed from pale green to olive - green solution.Cupper (II) cation showed a clear blue solution and its spectra are assigned to be octahedral geometry, while the added nitrite did not show color change but less absorbance was recorded. However, thiocyanate ion seems to react with cupper (II) ionic liquid solution producing suspended green solution with much less absorbance than with ionic liquid.Interestingly, the water molecules present in the original ammonium alum was not found to coordinate with metal cations as their spectra was found to differ when compared with those obtained in aqueous solution.

تصنيع اقطاب انتقائية جديدة لتقدير كل من الكلور امفينيكول صوديوم ساكسينيت والحديد الثلاثي وتطبيقاتها في المستحضرات الصيدلانية == Construction of new Ion Selective electrodes for Determination Chloramphenicol sodium succinate and Iron(III) and their applications in pharmaceutical samples

Author name: وئام رعد عزيز
Supervisor name: خالدة حميد محمد السعيدي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Two kinds of electrodes were prepared in this study based on PVCmatrix. Four ion selective electrodes for Chloramphenicol sodiumsuccinate which based on chloramphenicol palmitate (CPP) and sodiumtetraphenylborate (TPB) as additive, Another Four ion selectiveelectrodes for Iron(III) based on Chloramphenicol sodium succinate - Iron(III) [CPSS - Fe(III)] ion - pair complex as the electro - active material,.Many plasticizers used :  Di - butyl phthalate (DBPH) Di - butyl phosphate (DBP) Di - octyl phthalate (DOP) Tri - butyl phosphate (TBP)The electrodes parameters were include, linear concentration range,Nernestian slope, limit of detection, response time, life time, working pHrang and selectivity were evaluated. Also the statistical treatments wereapplied for the results that include : relative standard deviation (RSD),relative error (RE), error and confidence limit for concentration. The resultsshowed : 1 - ISES for Chloramphenicol sodium succinate : CPP+TPB+DBPH (membrane A1), CPP+TPB+DBP(membrane A2),CPP+TPB+DOP (membrane A3), CPP+TPB+TBP (membrane A4), givesthe slopes (53.98, 51.45, 49.66 and 48.98 mV/decade), linear range from(1x10 - 4 - 1x10 - 1, 5x10 - 4 - 1x10 - 1, 1x10 - 4 - 1x10 - 1, 5x10 - 4 - 1x10 - 1), withdetection limit (5x10 - 5M, 2x10 - 5 M, 3x10 - 5 M and 1x10 - 5 M), responsetime of 10 - 3M (15, 18, 20 and 35 second) and the lifetime were about (50,15, 23 and 21 day ). The working pH ranges were ranged from (2 - 7.5).The electrode A1 (CPP+TPB+DBPH) has been used to determineVIChloramphenicol sodium succinate in the pharmaceutical samples of(Chloramphenicol sodium succinate injection).2 - ISES for Iron(III) : CPSS - Fe(III)+DBP (membrane B1), CPSS - Fe(III)+DBPH (membraneB2), CPSS - Fe(III)+DOP (membrane B3) and CPSS - Fe(III)+TBP(membrane B4), gives the slopes (19.79, 26.60, 16.01 and 13.82), linearrange from (1x10 - 5 - 1x10 - 2 M, 1x10 - 5 - 1x10 - 2 M, 1x10 - 6 - 1x10 - 2 M and1x10 - 5 - 1x10 - 2 M), with detection limit (9×10 - 6 M, 7×10 - 5 M, 2×10 - 6 Mand 9×10 - 5 M), response time of 10 - 3 M (10, 35, 15, 35 and 30 second),lifetime were about (37, 41, 23 and 16 days). The working pH rangeswere ranged from (2 - 6) by using electrode (CPSS - Fe(III)+DBP), andthis electrode has been used to determine Iron(III) in the pharmaceuticalsamples of (Feroglobin Capsules).The selectivity coefficients (KpotA,B) of ISES have been studied for thefollowing interference ions (Na+, K+, Mn+2, Cu+2, Zn+2, Fe+3, Al+3,Chloramphenicol palmitate, folic acid , Sucrose and Gelatin) by usingseparate solution method and fixed interfering mixed method.The UV - spectrophotometric method which includes : - The derivative spectra, the first - derivative (1D) spectra for Chloramphenicol sodium succinate solutions (2 - 64 mg/L) in wavelength equal 258 nm with (r2=0.99925). The analytical methods results showed to be simple, rapid and with a good accuracy by comparing between FirstDerivative (1D) and direct method of Ion selective electrode by using Ftest.The results shown, that the Chloramphenicol sodium succinate can be determined by using Ion selective electrode method because the value of the (F) experimental less than the value of the (F) theoretical at 95% confidence limit. Since Fcalculated‹ Ftable, we oncluded that there is nosignificant difference in precision between two methods

دراسة الذوبان والكيمياء التناسقية لاكاسيد بعض العناصر الانتقاليه للمنصهر الايوني المحضر لمزيج كلوريد الكولين / حامض التارتاريك == Solubility and coordination study of some transition metal oxides in new choline chloride/ tartaric acid ionic liquid

Author name: فرح انور حسن
Supervisor name: هادي محمد علي عبود
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: في هذا البحث تم تحضير نوع جديد من الاملاح المنصهرة في درجة حرارة الغرفة , عن طريق مزج احد املاح جذر الامونيوم الرباعي وهو كلوريد الكولين مع احد المواد لها القابلية على تكوين اواصر هيدروجينية وهو الحامض الكاربوكسيلي الثنائي الكاربوكسيل وهو حامض التارتارك, تم تحضير عده محاليل بنسب مولية مختلفة. ومن المخطط الطوري للمحلول تم الحصول على محلول بدرجه انصهار 5 درجه مئوية.ومن مواصفات هذا الملح المنصهر المحضر هي : له صفات توصيلية , له كثافة عالية , وقيمه الاس الهيدروجيني له واطئه. وايضا في هذا البحث استخدمه الملح المنصهر المحضر كمذيب لا مائي لدراسة قابليه ذوبان بعض اكاسيد العناصر الانتقاليه من السلسلة الاولى وتشمل : [Co3O4, CrO3, NiO, CuO, ZnO]حيث وجد ان لها القابليه على الذوبان في هذا الملح المنصهر المحضر, وتم قياس التركيز ( الاذابة ) عن طريق استخدام جهاز الامتصاص الذري وذالك بدرجه حرارة الغرفه صعودا الى المائة درجة مئوية.اضافة الى ذلك تم حساب الحرارة الكامنة للانصهار لكل واحد من اكاسيد العناصر وتم توضيح تاثير اوربيتال d على قيمة الحرارة الكامنة للانصهار. تم تشخيص المحاليل السابق ذكرها عن طريق جهاز الاشعة الفوق البنفسجية - المرئية (UV. Vis.) لغرض معرفه المعقدات المتكونة ومعرفة التغير في الصيغة التركيبية للاوكسيد . وتم اخذ بنظر الاعتبار تاثير زيادة الحرارة الى درجه حرارة مائه درجه مئوية , حيث ان زيادة درجه الحرارة ليس له تاثير على الصيغه التركيبية الا انه له تاثير على زيادة الاهتزاز الالكتروني. تم حساب معامل راكاح (Racah) ,مقاييس المجال الليكندي , مقدار طاقه الانفصال (Δo) وحساب الامتصاصية المولاريه لكل طيف في جميع درجات الحرارة. | Choline chloride / tartaric acid room temperature ionic liquid was prepared and the obtained phase diagrams of the mixture showed eutectic point at 5 oC. The ionic liquid showed a conductive properties, high density and low PH values. Secondly, the dissolution of Co3O4, CrO3, NiO, CuO, and ZnO. Were studied and found soluble in choline chloride / tartaric acid ionic liquid as their solubilities were determined by measuring the dissolved metal by atomic absorption from room temperature up to 100 oC. The lattice energies of the metal oxides were deduced and the effects of the d - orbital electrons on the lattice energy were compared. In addition to their solubilities the above solution of metal oxides were investigates by ultraviolet visible spectroscopy. The spectra were measured and assigned to the expected coordination in the choline chloride/ tartaric acid ionic liquids, the effect of increasing temperature of the solution up to 100 oC were also studied and showed similar coordination but higher vibration with increasing temperature. Racah factor for there complexes (B) were determined together with field factor, crystal field splitting energy (Δo), nephelauxetic factors and molar absoptivities for each spectra at the variable temperatures.

تحضير وتشخيص الاملاح المنصهرة (السوائل الايونية) المستندة على مركبات السلفونيت == Preparation and Characterization of Molten salts (Ionic Liquids) Based on Sulfonate Compounds

Author name: عهد ديوان ساجت الفتلاوي
Supervisor name: هادي محمد علي عبود
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: تضمنت الرسالة دراسة تحضير وتشخيص املاح منصهرة (سوائل ايونية) تكون منصهرة في درجة حرارة الغرفة حيث تم تحضير كولين دودوسيل بنزين سلفونيت وفينل تراي ميثل امونيوم دودوسيل بنزين سلفونيت وكانت درجة الانصهار لكل منهما هي,118) oC ( 91.9 على التوالي .تم تحضير املاح منصهرة (سوائل ايونية) اخرى بواسطة خلط , صوديوم دودوسيل بنزين سلفونيت , بوتاسيوم دودوسيل بنزين سلفونيت, امونيوم دودوسيل بنزين سلفونيت , بنزويك اسد, ساليسالك اسد مع الكولين كلورايد وقد اظهرت عملية الخلط انخفاض كبير درجة الانصهار عن للمركبات الاصلية.الخليط المكون من( امونيوم دودوسيل بنزين سلفونيت\ الكولين كلورايد) ينصهرعند 15 oC , ايضا خليطي (بنزويك اسد\ الكولين كلورايد ( و) ساليسالك اسد\ الكولين كلورايد ( مع لهما درجة انصهار متشابهة مقدارها 60 oC , وهذة الدرجة تنطبق مع تعريف الاملاح المنصهرة (السوائل الايونية) التي تنصهر في درجة حرارة افل من oC 100, لذلك تعتبر املاح منصهرة في درجة حرارة الغرفة. اظهرت الخلطات المكونة من (صوديوم دودوسيل بنزين سلفونيت\ الكولين كلورايد) و(بوتاسيوم دودوسيل بنزين سلفونيت \ الكولين كلورايد) درجات انصهار اعلى من oC 100 . مجموعة اخرى من الاملاح المنصهرة (السوائل الايونية) التي تم تحضيرها بواسطة خلط نفس المركبات السابقة لكن مع اليوريا بدلامن الكولين كلورايد هذة الاملاح المنصهرة (السوائل الايونية) المكونة من مركبات السلفونيت لهما درجات انصهار اقل مما للاملاح المنصهرة المعتمدة على الكولين كلورايد التي تنصهر عند105 oC , oC 100 , 10 oC على التوالي. بينما في حالة )بنزويك اسد\ اليوريا ( و) ساليسالك اسد\ اليوريا ( تنصهر بدرجات اعلى وكانت, oC 75 , oC 77 على التوالي. الاملاح المنصهرة (السوائل الايونية) تتكون نتيجة التداخل الذي يحصل بين مكونات الخليط وتكون تاصرهيدروحيني او تكون معقد بين مكونات الخليط | The work presented in this thesis includes the preparation and characterization of choline dodecyl benzene sulfonate and phenyl trimethyl ammonium dodecyl benzene sulfonate, which were prepared and showed almost room temperature molten salts (ionic liquids) of 118 oC and 91.9 oC respectively, as shown in scheme (1) : Scheme (1) Other molten salts (ionic liquids) based on mixing sodium, potassium, ammonium dodecyl benzene sulfonate, benzoic acid and salicylic acid with choline chloride showed a larger melting point depression than from of initial components, as shown in scheme (2) and (3) : Scheme (2) (Ammonium dodecyl benzene sulfonate /choline chloride) mixture has a deep eutectic point of 15 oC, while the two mixtures (benzoic acid / choline chloride) and (salicylic acid / choline chloride) gave a similar eutectic point of 60 oC, which were correspond with the room temperature molten salt (ionic liquids) definition, which is melt below the 100 oC. However, (sodium dodecyl benzene sulfonate /choline chloride) mixture and (potassium dodecyl benzene sulfonate /choline chloride) mixture afforded higher eutectic temperature than the room temperature molten salts.Another set of mixtures that based on mixing the same previous compounds, but with urea instead of choline chloride. These mixtures showed with (NaDBS,KDBS and NH4DBS) compounds lower eutectic points than with choline chloride of 105 oC, 100 oC, and 10 oC respectively. While with benzoic acid and salicylic acid afforded a little higher temperature of 75 oC and 77 oC respectively. Compositions of these mixtures attributed to the formation and interaction of hydrogen bonding or the formation of complex compounds of eutectic nature.

الفصل الكروموتوغرافي لبعض الايونات الموجبة وتقديرها بواسطة كاشف التوصيلية والتحليل الضوئي غير المباشر

Author name: لبنى عبد الحسين عبد الامير الشيخ
Supervisor name: شهباز احمد مكي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Cation exchange chromatography with both unsuppressed conductivity detection and indirect photometric detection (IPD) modes were used for the separation and detection of inorganic cations. Salt of weak base diphenylamine has been used as an eluent for several cations both with unsuppressed conductivity detection and IPD. 4 - aminodiphenylammonium chloride possess ion exchange capability, chromatographic selectivity and large molar absorptivity. 4 - aminodiphenylammonium chloride showed a good chromatographic performance toward the analysis of the cations (Lithium, Barium, Iron II and Iron III ) using conventional HPLC equipment with either conductivity or indirect UV detectors. The analysis of these cations using (1×10 - 7 M) 4 - aminodiphenylammonium chloride at pH 5.80 in 5% DMSO, with Dionex Ion Pac CS3 Column, and 1ml/min flow rate was achieved with unsuppressed column conductivity and IPD at 342.5 nm detection. Chromatogram of a separation mixtures containing four cations (Li+, Ba+2,Fe+2 and Fe+3) and other mixture have given well separated peaks using IPD technique. The capacity factor K for the analyzed cations were ranged from (1.70 - 2.44), peak symmetries was ranged from (1.11 - 1.41) and resolution with an average value of (1.310) was optained. The average RSD for tR was 0.435%. The average recovery was 93.1075 % and the average relative error percentage was 6.77 % with unsuppressed conductivity detection . However, using IPD, the peak symmetry was ranged from(1.30 - 1.54), and an average value of resolutin of 1.41 which indicate a good chromatographic performance. The RSD in tR averaged 0.351 %. The average value of recovery was 95.975 %. Calibration curve for all analyzed cations were linear from their detection limit to at least 10 ppm. The correlation coefficients for the linear calibration curve were ranged from (0.9991, 0.9998) with both detection techniques. The detection limit was ranged from (0.025, 0.1) ppm for unsuppressed conductivity detection compared to (0.02, 0.05) ppm for IPD

التثبيت الضوئي لمتعدد (كلوريد الفانيل) باستعمال معقدات ثئاني (2 - امينو خلات بنزوثايزول) == PHOTOSTABILIZATION OF POLY(VINYL CHLORIDE) BY BIS(2 - AMINO ACETATE BENZOTHIAZOLE ) COMPLEXES

Author name: هدیل عادل عباس
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: In this work , Bis(2 - amino acetate benzothiazole) chelate complexes were prepared . These compounds are : 1 - Bis(2 - amino acetate benzothiazol) nickel(II).2 - Bis(2 - amino acetate benzothiazol) copper(II).3 - Bis(2 - amino acetate benzothiazol) zinc(II).4 - Bis(2 - amino acetate benzothiazol) cadmium(II). 5 - Bis(2 - amino acetate benzothiazol) tin(II).Infrared, ultraviolet - visible, spectrophotometric techniques, magneticsusceptibility, atomic absorption conductivity measurement and other physical properties were used to characterize the free ligand and the above chelate complexes.All these compounds were act as stabilizer in PVC films.The rate of photodegradation and photostabilization of PVC film (thickness 30mm) were monitored by measuring the carbonyl, polyene and hydroxyl indices (Ico, Ipo and IoH) values as afunction with irradiation time and ultraviolet - visible spectrophotometry using the concentrations of additive 0.5% wt/wt. The light of wavelength 313 nm with intensity (1.052*10 - 8 ein.dm - 3.S - 1) was used for irradiation of polymer films at room temperature.It was found that the carbonyl index (Ico) polyene index (Ipo) and hydroxyl index(IoH) values increased with irradiation time, and this increase depend on the type of additives (free ligand and complexes). The following trend was obtained for the photostabilization effect of PVCfilm in presence of these additives : Sn(H)2 > Cd(H)2 > Ni(H)2 > Zn(H)2 > Cu(H)2. According to the experimental results obtained several mechanisms were suggested depending on the structure of the additives. Therefore HCl scavenging, UV absorption, peroxide decomposer and radical scavenger for photostabilizer additiveswere suggested.

تحضيـروتشخيص مركبات مقلدة للانسولين == SYNTHESIS AND CHARACTERIZATION OF INSULIN - MIMETIC COMPOUNDS

Author name: عمار جهاد صادق العبدلي
Supervisor name: اياد حمزة جاسم
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
Language: English
University location: Baghdad
First pages:
Abstract: تهيئ الكيمياء اللاعضوية مجالا خصبا لتصميم وتحضير مركبات صيدلانية لمعالجة الامراض العسيرة المعالجة في الوقت الحالي.منذ فترة طويلة استخدمت الادوية الفلزية لعلاج واعادة وظيفة فسلجة الجسم الى حالتها الاولية.ان عنصري الفناديوم والكروم يقدمان حالة مدهشة من بين العناصر الانتقالية حيث لها سلطة وصفة كيموفيزيائية نكشف من خلالها صفة مهمة كمقلدات لعمل الانسولين. ولهذا تم دراستها جيدا في علاج مرض السكري للنوع الاول والثاني.ان تصميم الادوية الفلزية في بحثنا يقيم بالدرجة الاولى بالتشابه الفراغي للاعمال السابقة والتركيب المبسط وصفة التواجد البايولوجي والذوبانية والامتصاصية.تم تحضير اربعة مركبات مختلفة لتتاصر مع فلزات VO (II) وCr (III) الايونية لتكون ثمانية معقدات مختلفة تم اختيار ستة احماض امينية مختلفة لتتاصر مع فلزات VO (II) وCr (III) الايونية لتكون اثنا عشر معقد مختلف تم اختيار الماركبتو حامض الخليك وحامض المانديلك للتاصر مع فلزات VO (II) وCr (III) الايونية لتكوين اربع معقدات مختلفة.تم اختيار خمسة سكريات مختلفة لتتاصر مع فلزات VO (II) وCr (III) الايونية لتكون عشرة معقدات مختلفة.تم عزل وتشخيص عدد من المركبات المختلفة عن طريق دراسة صفاتها الكيموفيزيائية بواسطة تحليل المعادن وتحليل عناصر C.H.N.S، واطياف التردد والانتقالات الالكترونية، والصفات التوصيلية والمغناطيسية، بالاضافة الى دراسة اطياف الرنين المغناطيسي النووي للهيدروجين.تمت دراسة تكوين بعض المعقدات في المحلول باتباع طريقة النسبة المولارية mole ratio.ان نتائج الدراسات في الحالة الصلبة والسائلة اعطتنا نتائج متطابقة. | Biomedical inorganic chemistry offers the potential for the design novel therapeutic agents for the treatment of diseases, which are currently intractable. Therapeutic metalodrugs have since long been employed to restore human physiology. Vanadium and chromium presents an outstanding case of a transition elements, the omnipotent physicochemical properties of which have unearthed it’s potential use as a serious insulin mimtic agents, well suited in the treatment of the heterogeneous disease of diabetes mellitus types I and II.The design of such metallodrugs has been at the fore front of the research depending on analogy of the previous work, simple structure, bioavailability, solubility and absorption property.Four different analog ligands have been synthesized to coordinate with VO (II) and Cr (III) metal ions to produce eight different complexes.Six different amino acids have chosen to coordinate with VO (II) and Cr (III) metal ions to produce twelve different complexes.Marcapto acetic acid and mandelic acid are also chosen to coordinate with VO (II) and Cr (III) metal ions to produce four different complexes.Five different sugars have been chosen to coordinate with VO (II) and Cr (III) metal ions to produce ten different complexes.Several of the synthesized compounds were isolated and characterized by studying their physicochemical properties such as C.H.N.S and metal analysis, vibrational and electric spsectra, conductivity, magnetic properties, in addition to 1H.N.M.R spectral study for some complexes.The formation of some of the complexes were studied in solution following the mole ratio method. The results of both solid state and solution studies gave identical results.

تحضير اصباغ ازو بوليمرية بالكلة بولي (كلوريد الفاينيل) بحلقات البنزين باستخدام تفاعل فريدل - كرافتس == Preparation of polymeric Azo dyes via alkylation of Poly(vinylchloride) on benzene rings using Friedel - Craft، s Reaction

Author name: ايمان اسماعيل جبار الساعدي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Baghdad
First pages:
Abstract: في هذه الدراسة تم تحضير عدد من اصباغ الازو وذلك بتفاعل املاح الديازونيوم مع الفينولات . وفيما يلي التراكيب الكيميائية للاصباغ المحضرة (1 - 20)2. جري تفاعل فريدل - كرافتس بين اصباغ الازو المحضرة وبولي (كلوريد الفانيل ) مكونة اصباغا بوليميرية مختلفة فيما ياتي اسماءها وتراكيبها الكيميائية.3. في هذه الدراسة شخصت جميع المركبات الوسطية والاصباغ البوليميرية المحضرة بطيف الاشعة تحت الحمراء IR ، وطيف الاشعة فوق البنفسجية U.V، بالاضافة الى تحليل العناصر، وتم قياس لزوجة الاصباغ البوليميرية المحضرة ، وتبين ان لها اوزان جزيئيه ضمن المدى المتوسط ، هذا بالاضافة الى القياسات الفيزياوية المختلفة الاخرى من درجات التلين، ودرجات الانصهار لنماذج من الاصباغ البوليميرية المحضرة.4.الاصباغ البوليميرية المحضرة في هذه الدراسة اثبتت كفاءتها وصلاحيتها لصباغة القطن والخشب والبلاستيك ، وقد تم طلاء نماذج من تلك المواد وثبتت انها غير قابلة للذوبان في الماء وذات الوان زاهية ومميزة . | 1. Several azo dyes were prepared according to literature procedures .Diazonium salts were allowed to react with phenols to obtain the following azo dyes : . 2. The prepared azo dyes were allowed to react with Poly(vinylchloride) using Friedel Craft، s reaction and the following polymeric dyes were obtained : 3. All products , intermediates and polymeric dyes were characterized by IR, UV, elemental analysis , and chemical reaction. The viscosity’s of the prepared dyes showed them to be low to medium molecular weights. 4. Application of the prepared polymeric azo dyes in Coatins Wood and plastic showed them efficient and water insoluble. Their colors were bright and durable.

التقدير الطيفي لايون النحاس بوساطة الطريقة المباشرة وغير المباشرة بنقطة الغيمة باستخدام الحامض الامينيي الميثيونين == Spectrophotometric Determination of Copper Ion by Direct Method and Indirect Cloud Point Using the Amino Acid Methionine

Author name: اسماء نهاد زكي
Supervisor name: رافع قدوري عطيوي | سمية محمد عباس
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Baghdad
Language: English
University location: Baghdad
First pages:
Abstract: تشمل هذه الدراسة طريقتين مهمتين في التطبيق التحليلي لتعيين وفصل واغناء ايون النحاس الثنائي بطريقة نقطة الغيمة والطريقة الطيفية وذلك باستخدام مطياف الاشعة الفوق البنفسجية - المرئية. في الجزء الاول : تم استخدام الحامض الاميني الميثونين ككاشف تحليلي الذي يشكل مركب مخلبي مع ايون النحاس في الطور المائي وبدرجة حموضة محددة, والذي تكون له اعظم امتصاصية عند طول موجي (244 نانوميتر) لمعقد النحاس - الميثونين ضد الميثونين كبلانك.وتم دراسة الظروف الفضلى للتفاعل بالاضافة الى العوامل التحليلية الاخرى وافضل نتائج تم الحصول عليها لمنحني المعايرة والبيانات الاحصائية تحت الظروف الفضلى التي تم الحصول عليها بالطريقة الطيفية المباشرة لكميات صغيرة من النحاس, يطاوع قانون لامبرت بير في مدى تراكيز (0,1 - 10) ميكروغرام/مل مع امتصاصية مولارية (5842 لتر.مول - 1.سم - 1) وحد الكشف (0,0238 ميكروغرام/مل) في هذه الدراسة لوحظ حدوث تداخلات بعض المعادن مثل النيكل (II)والكروم(III) في ايون النحاس وقد تجاوزت الحد المسموح للتداخل , لذلك تم تطبيق الطريقة المقترحة بنجاح لتحديد ايون النحاس في عينات مختلفة من المياه.اما الجزء الثاني من الدراسة تستند على تكوين معقد كاره للماء بين ايون النحاس والميثونين الغنية بالترايتون 100 - X من خلال منهجية الاستخلاص بنقطة الغيمة الى جانب القياس الطيفي للاشعة فوق البنفسجية - المرئية, في هذه الطريقة يتشارك ايون الفلز مع الحامض الاميني الميثونين في تفاعل لتشكيل معقد مخلبي كاره للماء ويتم استخلاص هذا المعقد في درجة حموضة معينة عن طريق الاستخلاص بنقطة الغيمة باستخدام المركب السطحي غير الايوني ترايتون 100 - X كوسيط للاستخلاص.الطور العضوي الغني بالمادة السطحية يتم اذابتها باضافة الميثانول ويتم قياس المعقد طيفيا عند طول موجي (294 نانوميتر) لتحسين العوامل التي تؤثر على كفاءة استخلاص ايون النحاس باستخدام احد عوامل التحليلية وتشمل هذه العوامل درجة حموضة المحلول تركيز الليكند والمادة السطحية, درجة الحرارة والوقت التي تم تحديدها بالاضافة الى الكتيونات التي تعتبر متداخلات في ظل الظروف المثلى للتفاعل وقد تحقق عامل اغناء النحاس وكان منحني المعايرة الخطي (0,1 - 4) ميكروغرام/مل, حد الكشف والحد الكمي (0,0071) (0,0215) على التوالي. وتم مقارنة الطريقة المقترحة مع الطريقة الطيفية المباشرة لتعيين ايون النحاس ومن خلال النتائج المعروضة نلاحظ اختلافات كبيرة في الدقة والتوافق في الطريقتين وان الاستخلاص بنقطة الغيمة هي الاكثر دقة وتوافقية. تم تطبيق هذه الطريقة في عينات المياه. في هذه الدراسة تم تعيين تكافؤية المعقد عن طريق النسب المولية, التغيرات المستمرة (طريقة جوب) في درجة حموضة معينة واظهرت النتائج ان نسبة التكافؤ بين ايون النحاس الميثيونين هي 1 : 2. | This study in whole comprises two significant approaches in analytical application for direct determination and separation with preconcentration of copper ion by cloud point extraction methodology coupled with UV - Visible spectrophotometry.In the first part : The amino acid methionine was used as a chelating agent to form a complex with copper ion in aqueous phase at specific pH, which exhibits maximum absorption at (max= 244nm) against reagent blank. The optimum reaction conditions and other analytical parameters were evaluated. The results showed better optical characteristics for calibration curve and statistical data were obtained under optimum conditions using direct Spectrophotometric determination of micro amounts of copper ion. “Beer's law” is obeyed in the concentration range (0.1 - 10)g.mL - 1 , having molar absorptivity of 5842L. mol - 1. cm - 1. The value of detection limit was 0.0238g.mL - 1 . Interference study indicated that some metal ions like Ni+2, Cr+3 have exceeded the allowable limits of interference for copper ion absorbance signal. The proposed method was applied successfully for the determination of copper ion in various water samples.Part Two : Deals with the formation of a hydrophobic complex between copper ion and methionine in rich - surfactant phase, by “cloud point extraction” (CPE) methodology, coupled with UV - Visible spectrophotometry. This method involved reaction of copper ion with methionine as a chelating agent to form a hydrophobic complex. Which was extracted at specific pH by CPE technique using nonionic surfactant Triton X - 100.as an extraction medium. The complex was surrounded by surfactant micelles. The surfactant - rich phase was diluted with methanol and the complex was measured spectrophotometrically at it's (max= 294nm). Different factors that can influence the extraction efficiency of copper ion has been optimized by using one - factor - at - a - time (OFAT). These factors include solution pH, reagent and surfactant concentrations, temperature and incubation time. Besides the interference effect of cations was also considered under the optimized conditions, “preconcentration factor” of 90 was achieved. The linear range was (0.1 - 4)g.mL - 1 with “limit of detection” and limit of quantification (0.0071), (0.0215)g.mL - 1 respectively and molar absorptivity of (19621.5) L. mol - 1. cm - 1.The Stoichiometric study was determined by “mole ratio method and continuous variation method” (Job's) at specific pH. The results showed that the Stoichiometric ratio between copper ion and methionine was 1 : 2.The proposed method is compared with the direct spectrophotometry determination of copper ion and the results have shown that there is a significant differences in accuracy and precision between the two methods and the cloud point extraction which indicates that the latter is more accurate and more precise. The suggested method was applied successfully for the determination of copper ion in water samples

تحضير مشتقات جديدة للفينوكسثين == Synthesis of New Phenoxathiin Derivatives

Author name: اياد احمد محمد
Supervisor name: سعاد مصطفى الاعرجي
General topic: Chemistry
Specific topic: Organic Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: تضمن البحث تحضير اربعين مشتقا" جديدا" من مشتقات الفينوكسثين التي تحتوي على حلقات غير متجانسة . وقد تم تشخيصها جميعا" بالطرائق الطيفية : طيف الاشعه تحت الحمراء ( ( FT - IR وطيف الاشعه فوق البنفسجية ( ( UV وطيف الرنين النووي المغناطيسي( 1H - NMR ) لعشرة مركبات وهي [ 1] , [ 2 ] , [ 3e] ,[ [ 3h , [ 4a] , [ 4g ] , [ 5a] , [ 5d] , [ 6e] , [ 6j] , بالاضافة الى تعيين بعض الخصائص الفيزياوية مثل درجة الانصهار واللون . وقد صنفت جميع هذه المركبات المحضرة الى اربعة مجاميع تحتوي كلا" منها على عشرة مركبات .المجموعة الاولى : وهي مشتقات لــ 2 - ( اوكسي الكين - 1 - يل ) الفينوكسثين [ 3a - 3j] والمحضرة من تفاعل 2 - اسيتيل فينوكسثين مع مختلف المركبات العطرية الالدهايدية وبوجود هيدروكسيد الصوديوم . اما المجاميع الثلاثة الاخرى فقد تم تحضيرها من تفاعل مركبات المجموعة الاولى مع كلا" من : 1 - الهيدرازين بوجود حامض الخليك للحصول على مشتقات 2 - ( 1 - اسيتيل بايرازولين - 3 - يل ) للفينوكسثين [ 4a - 4j] .2 - الفنيل هيدرازين بوجود البايبيردين لتعطي مشتقات 2 - ( 1 - فنيل بايرازولين - 3 - يل ) فينوكسثين [ 5a - 5j] .3 - هيدروكـــلوريد الهيدروكسيل امـــين فــــي محـــلول هـــيدروكسيد الصوديـــوم الايــــثانولي لتـــــعطي 2 - ( ايزواوكسازولين - 3 - يل ) فينوكسثين [ 6a - 6j] .جميع مركبات المجامــــيع الثلاثة اعـــــلاه معوضة في الموقــــع ( 5 ) في كلا" مـــن حــــلقات البايرازوليــــن والايزواوكسازولين بمجاميع اريل وحسب المركبات العطرية الالدهايدية المستخدمة في تحضير مركبات المجموعة الاولى . | This work comprises the synthesis of forty new phenoxathiin derivatives containing heterocyclic moieties. All the synthesized compounds were characterized by such spectroscopy means namely FT - IR , ultra violet , and 1H - NMR analysis ( for ten compounds [ 1 ] , [ 2 ] , [ 3e ] , [ 3h ] , [ 4a ] , [ 4g ] , [ 5a ] , [ 5d ] , [ 6e ] , [ 6j ] )with thin layer, melting point and color. These heterocyclic compounds were synthesized in four groups , each one containing ten compounds .The first group is made up of 2 - (oxoalken - 1 - yl ) phenoxathiin derivatives [ 3a - 3j ] obtained from the reaction between 2 - acetylphenoxathiin with different aromatic aldehyde in the presence of sodium hydroxide .The other three groups involve compounds produced from reaction between each compound from the first group with each of : 1 ) Hydrazine hydrate in acetic acid to get 2 - ( 1 - acetylpyrazolin - 3 - yl ) phenoxathiin derivatives [ 4a - 4j ] .2 ) Phenyl hydrazine in presence of piperidine to yield 2 - (1 - phenylpyrazolin - 3 - yl) phenoxathiin derivatives [ 5a - 5j ] . 3 ) Hydroxylamine hydrochloride in ethanolic sodium hydroxide solution to give 2 - (isoxazolin - 3 - yl) phenoxathiin derivatives [ 6a - 6j ] . All these compounds of three groups above are substituted in the position ( 5 ) in both the pyrazoline and isoxazoline rings with different aryl groups according to the aromatic aldehyde used in the preparation of the first group series compounds .

تحضيروتشخيص وقياس قيمة الفعالية البايلوجية لعدد من الايمايدات الحلقية الجديدة المعوضة على ذرة النيتروجين والحاوية على حلقات غير متجانسة == Synthesis, Characterization and Evaluation of Biological Activity of Several New N - Substituted Cyclic Imides Containing Heterocycles

Author name: احمــد سعــدي حسـن
Supervisor name: احلام معروف العزاوي
General topic: Chemistry
Specific topic: Organic Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: يهدف بحثنا الى تحضير ايمايدات حلقية معوضة على ذرة النتروجين وحاوية على حلقات غير متجانسة ولغرض تحقيق هذا الهدف تم انجاز الخطوات التالية : 1 - تضمن الجزء الاول تحضير ستراكون ايمايدات معوضة بحلقات غير متجانسة هي مركبات N - (معوض بنزوثايزول - 2 - يل) ستراكون ايمايد [24 - 36] .2 - تضمن الجزءالثاني تحضير N - فنيل ستراكون ايمايدات مرتبطة بحلقة البنزوثايازول عن طريق مجموعة السلفون امايد هي N - (4 - N - معوض بنزوثايازول - 2 - يل) سلفون اميدوفنيل ستراكون ايمايدات [40 - 49].كما تضمن هذا الجزء تحضير N - فنيل ستراكون ايمايدات مرتبطة بحلقات غير متجانسة مختلفة عبر مجموعة السلفون امايد هي N - (4 - (N - مركبات حلقية غير متجانسة) سلفون اميدو فنيل) ستراكون ايمايدات [50 - 53].3 - تضمن الجزءالثالث تحضير N - بنزيل ستراكون ايمايدات مرتبطة بحلقة البنزوثايزول عن طريق مجموعة السلفون امايد هي مركبات N - (4 - (N - معوض بنزوثايزول - 2 - يل) سلفون اميدو بنزيل) ستراكون ايمايدات [57 - 66]. كما تضمن هذا الجزء تحضير N - بنزيل ستراكون ايمايدات معوضة بحلقات غير متجانسة مختلفة عن طريق مجموعة السلفون امايد هي مركبات N - (4 - (N - مركبات حلقية غير متجانسة) سلفون اميدو بنزويل) ستراكون ايمايدات [67 - 70]. 4 - تضمن الجزء الرابع من هذا البحث تحضير ايمايدات حلقية مثل (فثايل ايمايد وسكسن ايمايد) عن طريق جسر استامايدي.وهي المركبات N - (2 - استاميدو (معوض بنزوثايزول - 2 - يل) فثايل ايمايدات [81 - 90]. ومركبات N - (2 - استاميدو معوض بنزوثايزول - 2 - يل) سكسن ايمايدات [91 - 100]. لتحضير الايمايدات المطلوبة تم اتباع الخطوات التالية : ا - تم مفاعلة الامين الاولي الحاوي على حلقات غير متجانسة N - (معوض بنزثايزول - 2 - يل) مع كلوروكلوريد الاستيل لتحويلها الى مركبات 2 - (2 - كلورو استايل امينو) معوض بنزوثايزولات [71 - 80].ب‌ - تم تحويل الفثايل ايمايد والسكسن ايمايد الى املاح البوتاسيوم المقابلة.جـ - تفاعل مشتقات استيل امينو المحضرة في فقرة (ا) مع املاح الفثايل ايمايد والسكسن ايمايد المحضرة في فقرة (ب) لانتاج الفثايل ايمايدات N - (2 - استاميدو - (معوض بنزوثايزول - 2 - يل) فثايل ايمايدات [81 - 90]. والسكسن ايمايدات N - (2 - استاميدو (معوض بنزوثايزول - 2 - يل) سكسن ايمايدات [91 - 100].تم تعيين درجات الانصهار للمركبات المحضرة اجمع في هذا البحث وكما تم تشخيصها طيفيا عن طريق مطيافية الاشعة تحت الحمراء FT - IR وفق البنفسجية U.V. كما استخدمت مطيافية الرنين النووي المغناطيسي 1H - NMR و13C - NMR في تشخيص بعض المركبات المحضرة، فضلا عن اجراء بعض الكشوفات النوعية ذات الفائدة التشخيصية.5 - يتضمن الجزء الخامس الدراسة البايلوجية وذلك للتحري وتقيم الفعالية البايلوجية للمركبات المحضرة ضد انواع من البكتريا والفطريات عزلت كليا من حالات مرضية (بشرية) في مختبرات مستشفى الكاظمية وقد شملت الدراسة على مايلي : ا - دراسة تاثير المركبات المحضرة على نوعين من البكتريا الموجبة لصبغة كرام وهي (ستافلو اوريس وستربتو كوكس بايوجينس). ب - وكذلك على نوعين من البكتريا السالبة لصبغة كرام وهي (سيدومونس واي كولاي). جـ - وقد تم استخدام نوع واحد من الفطريات وهو (كانديدا البكان).وقد اوضحت نتائج الدراسة بان اغلب المركبات المحضرة ذات فعالية بايلوجية | The present work involved synthesis of several N - substituted cyclic imides containing hetero rings.Performing this target includes the following parts : 1 - The first part of this work involved synthesis of several N - substituted Citraconimides containing benzothiazole ring N - (substituted benzothiazole - 2 - yl) Citraconimides [24 - 36]. 2 - The second part involved preparation of N - (phenyl Citraconimides) attached to benzothiazole rings through sulfonamide group (N - (4 - N - substituted benzothiazole - 2 - yl) Sulfonamido phenyl) Citraconimides [40 - 49] and N - phenyl citraconimides attached to hetero cyclic rings through sulfonamide group [50 - 53]. 3 - The third part involved synthesis of N - benzyl citraconimides attached to benzothiazole rings through Sulfonamide group N - (4 - (N - substituted benzothiazole - 2 - yl) Sulfonamido benzyl) citraconimides [57 - 66] and N - Benzylcitraconimide attached to different heterocyclic rings through sulfonamide group [67 - 70]. 4 - This part involved preparation of phthalimides and succinimides attached to benzothiazoles through acetamido group.Producing the desirable phthalimides [81 - 90] and succinimide[91 - 100].All the prepared compounds in this work were characterized by recording their melting points, infrared (FTIR) and ultraviolet (U.V) spectra. H - NMR and C13 - NMR spectra for some of them were recorded also.5 - This part involved evaluation of the biological activity of the prepared compounds against two types of (Gram positive) bacteria including [Staphylococcus aurous and Streptococcusgain] and two types of (Gram negative) bacteria including [E.coli and Pseudomonas aeruginosa].Moreover biological activity of the prepared compounds ast fungi [Candida albicans].were studied also.The results showed that most of the prepared compounds have good biological activity against the mentioned organisms

تحضير وتشخيص مركبات خماسية وسداسية وسباعية الحلقة غير متجانسة == Synthesis and Identification of Five, Six and Seven membered ring of Heterocyclic derivativese

Author name: شذى سلمان حسن عباس
Supervisor name: ابتسام خليفة جاسم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Baghdad
First pages:
Abstract: يتضمن موضوع البحث في هذه الرسالة تحضير مركبات حلقية غير متجانسة خماسية وسداسية وسباعية متنوعة ابتداء من ماليك اسد داي هايدرزايد والذي حضر باستعمال ثنائي اثيل ماليت المقابل بتفاعلها مع الهيدرازين المائي وقد تم تقسيم هذا العمل الى اربعة اقسام : القسم الاول : يتضمن هذا القسم تحضير مركبات الفثالازين - 3و8 - دايون, والبريدازين - 6,3 دايون اوكسادايازول, اوكسازولين, ترايازول, ثايادايازول والتي اشتقت من تفاعل مالونك اسد داي هايدرزايد (1) مع مواد عضوية مختلفة وخطوات التفاعل موضحة في المخطط رقم (1).القسم الثاني : يتضمن هذا القسم تحضير ثايو سيميكاربزايد, سيميكاربزايد, اوكسازولين وثايازوالدين والتي اشتقت من تفاعل مالونك اسد داي هايدرزايد (1) مع مواد عضوية مختلفة وخطوات التفاعل موضحة في المخطط رقم (3).القسم الثالث : يتضمن هذا القسم تحضير مركبين جديدين من قواعد شف مشتقة من تفاعل مالونك اسد داي هايدرزايد (1) مع الالديهايد الاروماتية, حيث تمت عملية الغلق الحلقي باستعمال الفثاليك انهدريد لتحضيراوكسازيبين وخطوات التفاعل موضحة في المخطط رقم (2). | This work involves synthesis of different five, six and seven membered heterocyclic rings starting from Malonic acid dihydrazide which was synthesized from the corresponding diethyl malonate on its reaction with hydrazine hydrate. This work is divided into four different parts : First part : This part involved the synthesis of oxadiazole[9], triazole[3,19,22], thiadiazole[11,18] , thiadiazine[4], , pyridazin - 3,6 - dione [5] ,phthalazin - 3,8 - dione[6] and pyrazole[7,8] from compounds [a], [1] with different organic materials as shown in Schemes (I).Second part : This part involved the synthesis of thiosemicarbazide[16], semicarbazide[20],Thiazolidine[17] and Oxazoline[21]derivatives from malonic acid dihydrazide [1], as shown in Scheme (III).Third part : This part involved the synthesis of two new Schiff bases[12,14]derived from malonic acid dihydrazide [1] with two aromatic aldehydes and cyclization by the treatment with phthalic anhydride resulted oxazepines [13, 15] as shown in Scheme (II).

تحضير وتشخيص ليكاند قاعدة شف جديدة مشتقة من 4 - امينو انتي بايرين ومعقداتها مع بعض الايونات الفلزية ودراسة فعاليتها المضادة للبكتيريا == Synthesis And Characterization of New Schiff Base Ligand Derived From 4 - Aminoantipyrine And It'S Complexes With Some Metal Ions And Their Antibacterial Effective Study

Author name: هيام هادي علكم
Supervisor name: ساجد محمود لطيف
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Baghdad
Language: Arabic
University location: Baghdad
First pages:
Abstract: تضمن البحث تحضير ليكاند قاعدة شف جديدة (L) ثنائية السن نوع (NO)1,5 - dimethyl - 4 - ( 2 - oxo - 1,2 - diphenyl ethylidene amino) - 2 - phenyl - 1,2dihydropyrazol - 3 - one.وذلك من مفاعلة 4 - aminoantipyriene مع Benzil باستعمال الايثانول وسطا للتفاعل. | This work covers the synthesis and characterization of the new Schiff base bidentate ligand(L) type (NO) 1,5 - dimethyl - 4 - (2 - oxo - 1,2 - diphenylethylidene amino) - 2 - phenyl - 1,2 dihydropyrazol - 3 - oneThe ligand (L) was prepared from reaction of 4 - aminoantipyrine with Benzil under reflux in ethanol solvent. The Ligand Complexes for the metal ions : VO(II) ,Mn(II) , Co(II) , Ni(II) , Cu(II) , Zn(II) , Cd(II) and Hg(II) were prepared. The Ligand and its complexes were characterized by spectral methods [FT - IR , UV - Vis , Atomicabsorption , 1HNMR ] in addition to molar conductivity , Microanalysis (C.H.N) , Magnetic moment effect and melting point and mole ratio Ligand : Metal. From the above data for the ligand and its complexes , we suggested that the ligand (L) behaves as bidentate on complexation with metal ions Via Natom of ( C = N) group and O atom for ( C = O) of pyrazol ring. The suggested molecular formula and geometrical structure are : 1 - Squarepyrimide for [VO(L) (SO4) (H2O) ] 2 - Tetrahedral for [M(L)Cl2]. n H2O M = Zn (II) , n = 1 M = Cd(II) and Hg(II) ; n =0 3 - Octahedral for [M(L)2Cl X ]. Y M = Mn(II) , X = Cl , Y = H2O M = Co(II) , Ni(II) and Cu(II) X = H2O , Y = Cl

تحضير وتشخيص بعض المعقدات الفلزية احادية ومختلطة الليكاند المشتقة من سلفاميثاكزول و4,4' - ثنائي مثيل - 2,2' - باي بريدال == Synthesis And Characterization of Some Metal Complexes With Mono And Mixed Ligand Derived From Sulfamethoxazole And 4,4' - Dimethyl - 2,2' - Bipyridyl

Author name: ميسون مزهر عـبد الحسـن
Supervisor name: محاسن فيصل الياس
General topic: Chemistry
Specific topic: Inorganic Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: تم في هذا البحث تحضير معقدات جديدة للعناصر الثقيلة Rh(III)} وPd(II) Pt(IV)و {Au(III) من تفاعل الليكاند (sulfamethoxazole L1) مع ايونات املاح هذه الفلزات بالطريقة التقليدية وتم تحضير معقدات جديدة اخرى في الحالة الصلبة بواسطة تفاعل مزيج من (sulfamethoxazol | In the present study, new heavy metal complexes of sulfamethoxazole (SMX) as L1 have been prepared with Pd(II), Au(III), Rh(III) and Pt(IV) ions , in a solid state by conventional method. Two mixed ligands were chosen : sulfamethoxazole and 4,4/ - dimethyl - 2,2/ - bipyridyl (L2). This is done to prepare another series of complexes with some metal ions ( Co(II), Ni(II), Cu(II), Cd(II), Cr(III) , V(IV), Pd(II) and Au(III)) in order to investigate the coordination behavior of these ligands(L1) and (L2) toward these metal ions.These complexes, already prepared by the solid state, were characterized by the elemental analysis (C.H.N.S) and FT - IR , UV - Vis spectroscopy, in addition to the flame atomic absorption, magnetic susceptibility , melting point and conductivity measurements. According to the results obtained, it is noticed that ligand L1, with the light and heavy metal ions, clearly behaves as a bidentate through the O atom of sulfonyl group and N atom of sulfonylamid group for all the prepared complexes except Cu(II) and Ni(II). In this case, the ligand confirms that the bonding of the metal ion in a tridentate chelate through the O atom of sulfonyl group and N atom of sulfonylamid group and N atom of amine group.While L2 behaves as a bidentate ligand through two N atom. Conductivity measurements have shown that all the prepared complexes are ionic except PdL1L2 complex. Based on the results of the measurements, the following formula have been suggested for the new prepared complexes : - [VOL1L2]SO4.2H2O and [CuL1L2]2( NO3)4.0.5H2O have square pyramidal geometry while the following complexes are having octahedral geometry : - [CrL1L2 Cl2] Cl.H2O,[NiL1L2NO3]2 ( NO3)2.0.5 H2O,[PdL1L2 Cl2].0.5H2O,[PtL1Cl3H2O]Cl.H2O, [Au L1L2Cl2] Cl.2H2Oand the complexes below have tetrahedral geometry : - [CoL1L2] (NO3)2.3H2O,[CdL1L2](NO3)2.3H20 while [PdL1Cl]2 Cl2.H2O,[AuL1Cl2]Cl.3.5H2O,[RhL1ClH2O]Cl2.0.5H2O have square planar geometry.Different bonding and structural behaviors were revealed throughout the study of coordination chemistry of the newly prepared metal complexes.The nature of bonding between the metal ion and the donor atoms of the ligands were demonstrated by calculating Racah parameter and the other ligand field parameters which were calculated using suitable Tanaba - Sugano diagrams.The nature of the complexes in ethanol solution was studied for some of the prepared complexes such as (RhL1,PdL1,PtL1 and AuL1) in the solution state to determine the ratio between ligand to metal state by using the molar ratio method which gave results which approximately identical results when compared to those obtained from the isolated solid state. Besides the stability constant of the prepared complexes were studied and it was found that they were stable in molar ratio 1 : 1.

تحضير وتشخيص مشتقات جديدة للكومارين - 3 - كاربوكسلك اسيد == Synthesis And Characterization of New Derived From Coumarin - 3 - Carboxylicacid

Author name: كوثر عبد الواحد عبد الحميد
Supervisor name: شذى فاضل نارين الزبيدي
General topic: Chemistry
Specific topic: Organic Chemistry
Degree: Master
Language: Arabic
University location: Baghdad
First pages:
Abstract: تعد مشتقات الكومارين مهمه من الناحية البايلوجية والصناعيه والدوائيه وعلى هذا الاساس استمرت الدراسات في تحضيرمشتقات جديده للكومارين وعليه فقد تم في هذا البحث تحضير عدد من مشتقات للكومارين وعددها 23)) بالاضاقة الى المركب 2 - oxo - 2H - coumarin - 3 - carbox | The coumarin and his derivatives class of heterocyclic compoundsThey are presente in a large family of products with broad biological and industrial activities.This fact leads as to synthesis twenty eight compounds of heterocyclic by several methods show in diagrams (1, 2).Than we characterized this compounds by some spectral analysis Such as : (FT - IR), (GCMS), (H - NMR) and determination of their physical properties such as melting points and color.This work involved : 1. Synthesis of base compound ( coumarin 3 - carboxylic ) by reaction Malonic acid with Salicylaldehyde in Petroleum ether as a solvent.2. Synthesis of k1 by reaction ( coumarin 3 - carboxylic ) with Thionyl chloride in Dichloro methane as a solvent.3. Synthesis of k2 by reaction k1 with hydrazine hydrate 99%. 4. Reaction k2 with six kinds of aromatic aldehyde to Synthesis of Schiff Bases : K8 - k7 - k6 - k5 - k4 - k35. Synthesis of five from Tetrazoles compounds by reaction Schiff Bases With sodium azide in dioxane as a solvent. 6. Synthesis of five from thiazolidinone compounds by reaction Schiff Bases with Mercapto acetic acid in THF) as a solvent. 7. Synthesis of five from azetidinone compounds by reaction Schiff Bases with ChloroacetylChloride in Dioxane as a solvent. 8. Synthesis of five of thiourea compounds by reaction Schiff Bases with thiourea in methanol as a solvent.
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