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تحضير و تشخيص انابيب الكاربون النانوية من بعض الكحولات و التطبيقات الضوئية == Synthesis and Characterization of Carbon Nanotubes from some Alcohols and Photo Applications

Author name: غسان جاسم محمد علي
Supervisor name: فلاح حسن حسين
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: هذه الرسالة ركزت على تحضير انابيب الكاربون النانوية (CNTs) من انواع مختلفة من الكحولات (الايثانول, 1- بروبانول و 2- بروبانول) باستخدام طريقة الترسيب الكيميائي للبخار(CVD) بوجود وعدم وجود العامل المساعد. العامل المساعد المستخدم في هذا التحضير هو الحديد المحمل على اوكسيد المغنيسيوم (Fe/MgO). | ظروف تجربة تحضير انابيب الكاربون النانوية تضمنت نوع المصدر الكاربوني و نوع الغاز الناقل و سرعة المرور و نوع الساند ونوع المحفز و حرارة النمو و زمن التحضير للنمو. تم الحصول على انابيب الكاربون النانوية من هذه الطريقة وباتباع هذه الضروف التي تضمنت : استخدام الكحولات كمصدر للكاربون في ثلاثة اشكال ( ايثانول, 1- بروبانول و 2- بروبانول). ان نوع المحفز والساند كانت مزيج من معدنين Fe/MgO عند نسبة ثابتة 1-10. ان وقت التحضير كان 1 : 30 ساعة, حرارة النمو كانت 750 درجة مئوية وان نوع الغاز الناقل كان النايتروجين مع سرعة مرور 100 مل\الدقيقة. | تقنيات مختلفة استخدمت لتشخيص انابيب الكاربون النانوية المحضرة. التقنيات المستخدمة هي انعكاس الاشعة السينية (XRD) و اطياف رامان و المجهر الالكتروني النافذ(STEM) و المجهر الالكتروني(SEM) ومجهر ايون الهليوم (HIM) و طاقة الاشعة السينية المتشتتة (EDX)و التحليل الوزني الحراري .(TGA) | التحليل بتقنية XRD و EDX استخدم للحصول على معلومات حول هيكل لانابيب الكاربون النانوية ومكونات العناصر الموجودة في العينة. استخدم مطياف رامان للتحقق من تكون انابيب الكاربون النانوية وكذلك جودة هذه الانابيب. تشير نتائج اطياف رامان الى انه تم الحصول على الحزم الرئيسية لانابيب الكاربون النانوية والتي تؤكد على تكون هذه الانابيب. تشير صور HIM وSEM و STEM الى ان انابيب الكاربون النانوية المحضرة لديها متوسط اعلى طول 10 مايكروميتر واقل قطر يتراوح بين 5-8 نانوميتر ومع عدد طبقات يتراوح بين 3-6 طبقة. | درست الفعالية الضوئية للعامل المساعد P25/CNTs باستخدام مركب الكوبال امين. العديد من العوامل العملية المؤثرة هي مثل وزن العامل المساعد المستخدم CNTs/TiO2 (175\5, 175\15, 175\25) ملغم و نوع الغاز المستخدم و مع تركيز 40 ppm من صبغة الكوبال امين. | هذا التفاعل يبين ان المزيج 15 و 175 ملغم من CNTs و P25 على التوالي اعطى افضل كفائة ازالة مقارنة مع المزيجين الاخرين وهو يتساوى مع كفائة ازالة P25 175 ملغم لوحده. | == This thesis focuses on the synthesis of carbon nanotubes (CNTs) from different types of alcohols (ethanol, 1-propanol and 2-propanol) via chemical vapor deposition (CVD) method in the presence and absence of catalyst. The catalyst used in the synthesis is iron loaded over magnesium oxide (Fe/MgO). | The conditions of experiment of synthesis CNTs include : type of carbon source, type of carrier gas, flow rate, type of support, type of catalyst, growth temperature and synthesis time of growth. CNTs were obtained from this method and by following these conditions which include : using alcohols as carbon source in three forms (ethanol, 1-propanol and 2-propanol). Type of catalyst and support were mixture of two materials Fe/MgO at fixed ratio 1 : 10. The synthesis time was 1.5 hr, growth temperature was 750 oC and the type of carrier gas was nitrogen gas with flow rate 100 ml/min. | Various experimental techniques were used for characterization of the synthesized CNTs. The techniques used are x-ray diffraction (XRD), Raman spectroscopy, scanning transmission electron microscopy (STEM), scanning electron microscopy (SEM), helium ion microscopy (HIM), energy dispersive x-ray (EDX) and thermo gravimetric analysis (TGA). XRD and EDX analysis were used to obtain information about structure of CNTs and the composition of elements in the sample. Raman spectroscopy was used to investigate the confirm of CNTs and the quality of the tube. The result of Raman spectra indicate that the main band of CNTs was obtained and which it investigates the confirm of CNTs. The STEM, SEM and HIM images indicate that the synthesized CNTs that has average highest length around 10 μ and lower diameters for synthesized CNTs ranged from 5-8 nm and with number of layers ranged from 3-6 layers for CNTs. | The photo-efficiency of P25/CNTs catalyst is studied using cobalamine as a model compound. The effect of several operation parameters, such as the effect the weight of the catalyst used P25/CNTs (175/5, 175/15, 175/25) mg, the type of gas used (air and nitrogen gas) and with 40 ppm of cobalamine dye. | This reaction shows that the mixture of 15 and 175 mg of CNTs and P25 respectively gave best removal efficiency as compared with the two mixture and equal to the removal efficiency of P25 (175 mg) alone |

تاثير بعض مكونات القهوة على فعالية انزيم ? - Galactosidases المستخلص من بكتريا الفم المرتبطة بالبخر الفموي == Effect of Some Coffee Components on The Activity of ? - Galactosidase Isolated From Oral Bacteria Associated with Halitosis

Author name: اميرة مريبي زرزور عبد الفضلي
Supervisor name: عودة مزعل الزاملي | قاسم نجم ثويني
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: This study includes extraction and purification of α-galactosidase enzyme from Erysipelothrix rhusiopathiae associated with halitosis infections & estimating the inhibition behaviors of some coffee components (caffeine and chlorogenic acid) on the activity of this enzyme. These isolates were collected from outpatients attending Dental Clinical in Al-Zahra Hospital , Al-Kut/ Wasit province, Iraq during (March to October 2014) with age of (21-60 years old ), clinically diagnosed as having halitosis; from 100 patients (30 : 30%) had positive bacterial culture. Thirteen (43.3%) of these 30 patients were females; (6 : 46.1%) of them with gram negative bacteria whereas (7 : 53.8 %) were having gram positive bacteria, while (17 : 56.6%) were collected from males, (8 : 47.0%) having gram negative bacteria, and ( 9 : 52.9%) with gram positive bacteria. Among the gram negative bacteria isolated, four(20.0%) isolates belonged to Veillonella spp., 3 to Porphyromonas endontalis (15.0%), and 2 to Prevotella intermedia (10.0%). Whereas gram-positive isolates were 4 belonged to Erysipelothrix rhusiopathiae (20.0%), 4 to Streptococcus salivariu ( 20.0%), and 3 to Streptococcus oralis (15.0%). Further identification of these isolates was performed depending on commercial systems (Api20E ), in addition to Vitek2 system which also has the ability to identify the ability of bacteria to produce galactosidase and determine its type (either α-galactosidase or β-galactosidase). So that Vitek2 system helped us to select an isolate with ability to produce α-galactosidase. | Identification of Erysipelothrix rhusiopathiais was based on gram staining, colonial morphology, hemolytic and biochemical properties. Identification of the isolates was confirmed by Api20E system and automatic Vitek2 system. These 4 isolates were designated by the | II | researcher as E. rhusiopathiae IrqA1, E. rhusiopathiae IrqA2, E. rhusiopathiae IrqA3, and E. rhusiopathiae IrqA4. | Erysipelothrix rhusiopathiae IrqA2 was used for extraction and purification of α -galactosidase. This isolate was selected because it had a higher enzyme activity (730 U/ml). α-galactosidase enzyme has been extracted from a selected Erysipelothrix rhusiopathiae IrqA2 isolates and its concentration of protein was estimated to be 19.56 mg/ml as a crude protein. The activity of the enzyme was measured using ( p-nitrophenyl- α -D-galactopyranoside) as substrate , then purification steps included precipitation by 40% ammonium sulfate ( yielded 4.74mg/ml protein) with activity 515.2U/ml ,dialysis , DEAE- cellulose chromatography of partially purified α-galactosidase after ammonium sulfate precipitation showed one peak with maximum activity 331.15U/ml ( 0.537mg/ml of protein) .After ion-exchange chromatography, SDS-PAGE showed protein band at 55KDa) represented subunit of the partially purified enzyme . Kinetics parameter were calculated , Km (5.5 mM )& Vmax (8.3 μmol /min). The enzyme showed maximum activity at 45°C at pH 6.5 . | The effect of caffeine on partially purified α -galactosidase activity revealed non-competitive inhibition (decrease Vmax 6.2μmol/min, unchanged Km value 5.5 mM ). However, the effect of chlorogenic acid showed an uncompetitive inhibition on enzyme activity .Which reflected that the enzyme has a single catalytic site since the change in Km (3.1 mM ) & Vmax (4.1 μmol/min) was observed . Worldwide and based on literature review, this is the first study for extraction of α-galactosidase enzyme from this bacterium.

دراسة مقارنة تاثير عقاري كلابنكلامايد والميتفورمين على فعالية اراجدونيت 15 لايبوكسيجينيز واكسدة الدهون الفوقية في امصال بعض المرضى العراقين المصابين بالسكري النوع الثاني

Author name: حيدر خابط عبود القيسي
Supervisor name: محمود حسين هدوان
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: Diabetes mellitus is a group of metabolic disorders described with chronic hyperglycemia arising from disorders in insulin secretion, insulin action or both. The presence of these consequences in chronic hyperglycemia led to damage, dysfunction, and failure of some organs, principally eyes, kidneys, heart, nerves, and blood vessels. | Enzymatic lipid oxidation comprises an enzyme as a catalyst, and provides very specific stereo and regiospecific compounds. Non-enzymatic does not produce specific compounds, many stereo-and positional isomers produced. There are three families of enzymes implicated in the oxidative metabolism of arachidonic acid. These involve the lipoxygenases, which form leukotrienes (LT), hydroperoxyeicosatetraenoic acids (HPETEs), hydroxyeicosatetraenoic acids (HETEs), and hydroxyoctadecadienoic acids (HODEs). | The aims of the study are : | - Determining the effects of glibenclamide and metformin on the following parameters : lipid profile, lipid peroxidation, total antioxidant capacity, α-tocopherol, total oxidant status and arachidonate 15-lipoxygenase activity | - Developing a new precise method for assessment catalase activity and compared it with ordinary methods. | The study included a hundred and twenty patients with diabetes type II aged between (44.5±9.2) years old models were obtained from patients in a clinical study in Al-Najaf Center for Diabetes and Endocrinology (Al-Najaf City, Iraq) additionally to sixty individuals representing a healthy control group aged between (42.4±7.2) years old within the period of March 2015 to the end of December 2015. | ABSTRACT | ii | The study includes the following groups : | 1- Patients with diabetes type II (30males & 30 females) were treated with metformin (Glucophage). | 2- Patients with diabetes type II (30males & 30 females) were treated with (Daonil) Glibeneclamide. | 3- Healthy subjects (30males & 30 females) were selected as a control. | Subjects have been diagnosed with diabetes, according to World Health Organization (WHO) standards, which include that all patients within the study does not suffer any of the cases high blood pressure, not smoking, not abusing alcohol or any treatment. All cases outside of these criteria were excluded from the study, the use of serums and blood as models for the study were obtained on serums from the blood of patients and healthy controls to be measured levels of both glucose blood in the case of fasting cholesterol , triglyceride and lipoproteins (HDL-c, LDL-c, VLDL-c,) as well as the measurement of hemoglobin level glycated HbA1c in the blood and so were measured concentration malondialdehyde MDA as an indicator of lipid peroxidation way spectrofluorometer , total reactive oxygene species as an indicator total oxidant status, also have been measured total antioxidants and measuring the concentration of vitamin E, the development of a new way to measure the effectiveness of an catalase enzyme through add correction factors to the equation first Order Reactions to increase accuracy and precision , measure the levels of enzyme Arachidonate 15-lipoxygenase , it was shown that there were significant differences and other variables were not significant for all the different types of diabetes-related treatment. It was found by studying the effectiveness of the enzyme 15- lipoxygenase not changed with the male patients treated with mtformin and glibenclamide compared with healthy | ABSTRACT | iii | controls, but there were significant decrease in the efficiency with female therapists with glipenclamide and mtformin there is a significant increase in the concentration of MDA in each of the male and females treated with metformin and glibenclamide in contrast, a decrease in the ability of antioxidants in both males and females treated with glibenclamide but this ability does not change with both male and female therapists patients with metformin . | Conclusion | oxidation of lipids enzymatic and non enzymatic leads to the formation of lipid peroxides that have a direct impact on the diabetes and that the lipoxygenase enzyme the source of enzymatic sources that reduce antioxidants and increase the concentration of free radicals. glibenclamide reduces concentration of the enzyme as well as increase antioxidants capacity and reduces lipid peroxides and reduce HbA1C In addition Show that the patients were treated with metformin or glibenclamide had non-significantly changed in serum α-tocopherol levels than the control group. | The results show decrease HDL levels; when compared with healthy subjects, but incresed LDL, VLDL, TC, and TG ; that is may be related to increased oxidative stress.

التكسير الضوئية المحفزة لصبغة Orange G بواسطة العامل المساعد المزدوج Nb2O5/Sb2O3 ودراسة الحركيات == Photocatalytic degradation of Orange G dye by using coupled Nb2O5/Sb2O3 and study the kinetic

Author name: مروة محمد علي عبيد حسان
Supervisor name: ندى يحيى فيروز
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: This study includes the preparation of new coupled Nb2O5/Sb2O3 by using dry mixing methods for Niobium pentoxide and Antimony trioxide at different ratios of (0.25 : 0.75 ,0.5 : 0.5 and 0.75 : 0.25) W/W % and calcination at different temperature 400 °C , 500 °C and 600 °C . The prepared catalyst was characterized by X-ray diffraction , Fourier Transform Infrared Spectroscopy Technique (FT-IR) , Atomic Force Microscopy (AFM), UV-Vis spectroscopy and measure band gap energy for the prepared coupled catalyst. The photocatalytic degradation of Orange G dye was evaluated under using high pressure mercury lamp after determining the wavelength of Orange G dye at λ max (475 nm). | The result showed that percentage of new coupled Nb2O5/Sb2O3 (0.5 : 0.5) at calcination temperature equal to 600 °C higher activity than other ratio at different calcination temperature. The limited optimum conditions of photocatalytic degradation of Orange G dye by the prepared coupled catalyst have been done using different parameters includes the best of weight of catalyst, initial of dye concentration , effect of pH solution .Also the effect of temperature has been studied to find the active energy (Ea) of photocatalytic reaction by new coupled Nb2O5/Sb2O3 equal to 26.109 KJ/mol . | The dye degradation followed pseudo first order kinetic. Also study effect addition of hydrogen peroxide and recycle of the catalyst.

دراسة محاكاة لميكانيكية تفاعل الادرنالين ونمذجة جزيئات دوائية شبيهه == Simulation Study of Reaction Mechanism for Adrenaline and Modulation Analog Moieties Drugs

Author name: هالة ثامر محمد
Supervisor name: عباس عبد علي دريع الصالحي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: استعملت طرق الحسابات النظرية لميكانيك الكم مثل الحسابات شبه التجريبية (PM3) وحسابات نظرية دالة الكثافة minimal STO-3G)) باستخدام برنامج Hyperchem 8.09 العالمي والذي يحتوي على معظم حسابات ميكانيك الكم. | تضمن العمل جزئين : | في الجزء الاول من البحث تم دراسة سلسلة تفاعلات لتخليق الادرنالين من الحامض الاميني (الفينايل انلاينين) نظريا. حيث تم اقتراح نواتج محتملة مختلفة لكل تفاعل في سلسلة تفاعلات تخليق الادرنالين. تم اختيار النواتج الاكثر احتمالا بالاعتماد على خصائصها الالكترونية لاثبات مسار التفاعلات الخمسه لتخليق الادرنالين في جسم الانسان. | تم حساب الطاقة الكلية وطاقة نقطة الصفر وطاقة الاوربتالات الجزيئية لتقدير طاقة فجوة الحزمة لجميع المركبات. و قيمة طاقة فجوة الحزمة مساوية الى (0.870 و 0.787 و 0.101 و 0.119 و 1.915و eV 0.593) للفينايل انيلين و تايروسين و دوبا ودوبامين و نورادرنالين والادرنالين على التوالي. تم حساب هذه الطاقات باستخدام نظرية دالة الكثافة minimal STO-3G. | تم حساب طاقة التنشيط وثابت سرعة التفاعل و الدوال الثرموديناميكية للتفاعلات الخمسة ولجميع النواتج المحتملة باستعمال الحسابات الشبه التجريبية. حسب ثابت سرعة التفاعل لل فينايل انيلين و تايروسين و دوبا ودوبامين و نورادرنالين والادرنالين وكان مساوي الى 5.554*1012 و 5.572*1012 و 7.857*1012 و 1.331*1013و s-11.116*1013على التوالي. تم الحصول على هذه النتائج باستخدام الحسابات شبة التجريبية. | اما الجزء الثاني تضمن اقتراح عدة ادوية مساعدة لمعالجة مرض الشلل الرعاشي (البريكنسون). | تم حساب الخصائص الهندسية والاطياف الاهتزازية لجميع الادوية المساعدة المقترحة لاختيار الافضل في معالجة مرض الشلل الرعاشي | بواسطة حساب الطاقة الكامنه للسطح و شحنة الاصرة وطول الاصرة وزاوية الاصرة وعزم ثنائي القطبين والمجال الكهربائي و طاقة الاوربتالات الجزئية وطاقة فجوة الحزمة. | توصلت الدراسة الى : | ان افضل دواء مساعد مقترح هو M-6-Sphe لامتلاكه اقل طاقة والتي تساوي--132291.816 kCal/mol و حرارة تكوين مساوية الى -400.534 kCal/mol. وذلك لامتلاكة اقل قيمة لعزم ثنائي القطبين مساوية الى 3.028 Debye, ولهذا السبب يكون محب للدهون اكثر من بقية الادوية المساعدة , وكذلك يمتلك اعلى قيمة لطاقة فجوة الحزمة مساوية الى 8.786 eV, الامر الذي يؤهله ليكون العلاج الامثل من بقية الادوية. | تم دراسة المجال الكهربائي والتوزيع الذري وطول الاصرة والاوربتالالت الجزيئية M-6-SPhe تم اختبار الحالة الانتقالية لتكوين 3, 4-HYM-6-Sphe من خلال حسابات طاقة نقطة الصفرو التردد الخيالي لتشخيص افضل حالة انتقالية ومن ثم اقتراح ميكانيكية التفاعل. تم حساب طاقة التنشيط وثابت السرعة ومسار التفاعل والدوال الثرموديناميكية لتفاعل التكوين. | == Abstract | Quantum methods like Semi-empirical (PM3), and Density functional theory (minimal STO-3G) have been performed by using reliable, well-known programs Hyperchem 8.09, which includes most of quantum mechanics treatments. | The work include two parts : | In the first part, a sequence reactions for Adrenaline synthesis from Phenylaniline have been studied theoretically. Different probable products have been suggested for each reaction in a sequence reaction for Adrenaline synthesis. The most probable products have been selected depending on the electronic properties to prove the pathway of five reactions to synthesizes Adrenaline in the human body. | Total energy, zero point energy (ZPE) and molecular orbital (HOMO&LUMO) have been calculated to estimate the energy gap for all reactions components. The energy gap is equal to (0.870, 0.787, 0.101, 0.119, 1.915, and 0.593 eV) for Phe, Tyr, DOPA, Daopamine, Noradrenalin and Adrenaline respectively. These energy gaps have been calculated by using DFT minimal STO-3G. | Activation energy, rate constant and thermodynamic functions (heat of formation change of reactions, entropy change of reactions, and Gibbs free energy change of reactions) of five reactions were calculated for the different probable products by using Semi empirical methods. The calculations show that the most probable products have rate constant that’s equal to (5.554*1012, 5.572*1012, 7.857*1012, 1.331*1013, 1.116*1013 s-1) for Phe, Tyr, DOPA, Daopamine, Noradrenalin and Adrenaline respectively. These results were obtained by using Semi empirical methods. | In the second part, different prodrugs have been suggested to treat Parkinson's disease. | Geometrical properties and vibration spectra have been calculated for all the suggested prodrugs to estimate the best prodrugs for Parkinson's disease treatment by calculating the potential energy surface, atomic charge, bond length, bond angle, dipole moment, electrostatic potential and molecular orbital energy with energy gap. | From this study it found that : | The M-6-SPhe prodrug has -132291.816 kCal/mol less energy than other prodrugs, so it is consider the favorite, and it has -400.534 kCal/mol heat of formation. It also, has the lowest value of dipole moment equal to 3.028 Debye, so become more lipophilic than other prodrugs. It has the highest value of the energy gap that equals 8.786 eV, which is the best conditions to be the perfect prodrug to treat Parkinson's disease. The electrostatic potential, atomic charge, bond length, and molecular orbital have been studied for M-6-SPhe. | Examination of real transition state of 3, 4-HYM-6-SPhe formation reaction has been tested through the calculations of ZPE and imaginary frequency to investigate the transition state and then suggest the reaction mechanism. Activation energy, rate constant, reaction path and

تحضير ودراسة بعض مركبات الفثالوسيانين المعوضة الجديدة == Synthesis and Study of Some New Substituted Phthalocyanines

Author name: حسين علي محمد
Supervisor name: مهند موسى كريم الحجامي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: المركبات المعوضة الجديدة للفثالوسيانين تم تخليقها من المادتين الاساسيتين 4- نايتروفثالونيترل و 4- امينو فثالونيترل لينتج المركبات رباعي (( 5-(3-دوديسنايل )-2,5-داي اوكسي بيرولدين-1-يل)-2-هيدروكسي بنزويك اسيد) زنك فثالوسيانين (C1) و رباعي (( 5-(3-دوديسنايل )-2,5-داي اوكسي بيرولدين-1-يل)-2-هيدروكسي بنزويك اسيد) نحاس فثالوسيانين(C2) و رباعي (دو ديسينايل سكسينك انهايدريد ) زنك فثالوسيانين (H1) و رباعي (دو ديسينايل سكسينك انهايدريد ) نحاس فثالوسيانين (H2)و ازا- دايمرك سداسي (دو ديسينايل سكسينك انهايدريد ) نيكل-زنك فثالوسيانين(F) بواسطة عدة خطوات وقد شخصت المركبات المحضرة الجديدة بواسطة تقنيات تحليل العناصر, الاشعة تحت الحمراء ، الرنين النووي المغناطيسي , والتحليل الطيفي للاشعة فوق البنفسجية المرئية. | هنالك خمسة مسارات لتخليق المركبات | المسار الاول | 4- نايترو فثالونيترل يتفاعل مع كلوريد الزنك بوجود ثنائي مثل امينو ايثانول كمذيب لينتج المركب 4ʹʹʹʹ,4ʹʹʹ,4ʹʹ,4ʹ-رباعي نايترو زنك فثالوسيانين(A1). الاخير يتفاعل مع 5-امينو سلسلك اسد لينتج رباعي (5-امينو حامض السالسليك) زنك فثالوسيانين (B1). بعد ذالك دو ديسنايل سكسنك انهايدرايد اضيفت الى مجموعة الامين الموجودة في المركب (B1) لينتج المركب رباعي (( 5-(3-دوديسنايل )-2,5-داي اوكسي بيرولدين-1-يل)-2-هيدروكسي حامض البنزويك) زنك فثالوسيانين (C1). | | المسار الثاني | 4- نايترو فثالونيترل يتفاعل مع كلوريد النحاس بوجود ثنائي مثل امينو ايثانول كمذيب لينتج المركب 4ʹʹ,4 4ʹʹʹʹ,4ʹʹʹ-رباعي نايترو نحاس فثالوسيانين(2A). الاخير يتفاعل مع 5-امينو سلسلك اسد لينتج رباعي (5-امينو حامض السالسليك) النحاس فثالوسيانين (B2). بعد ذالك دو ديسنايل سكسنك انهايدرايد اضيفت الى مجموعة الامين الموجودة في المركب (B2) لينتج المركب رباعي (( 5-(3-دوديسنايل )-2,5-داي اوكسي بيرولدين-1-يل)-2-هيدروكسي حامض البنزويك)النحاس فثالوسيانين (C2). | | | | | | المسار الثالث | 4-امينو فثالونيترل تفاعل مع كلوريد الزنك بوجود ثنائي مثل امينو ايثانول كمذيب لينتج المركب 4ʹʹʹʹ,4ʹʹʹ,4ʹʹ,4ʹ-رباعي امينو زنك فثالوسيانين(G1). الاخير تفاعل مع دو ديسنايل سكسنك انهايدرايد لينتج المركب رباعي (دو ديسنايل) زنك فثالوسيانين (H1). | | المسار الرابع | 4-امينو فثالونيترل تفاعل مع كلوريد النحاس بوجود ثنائي مثل امينو ايثانول كمذيب لينتج المركب 4ʹʹʹʹ,4ʹʹʹ,4ʹʹ,4ʹ-رباعي امينو النحاس فثالوسيانين(G2). الاخير تفاعل مع دو ديسنايل سكسنك انهايدرايد لينتج المركب رباعي (دو ديسنايل) النحاس فثالوسيانين (H2). | | المسار الخامس | 4-امينو فثالونيترل و 4-نيترو فثالونيترل تفاعل مع كلوريد الزنك او كلوريد النيكل بوجود ثنائي مثل امينو ايثانول كمذيب لينتج المركب 4ʹʹ,4ʹ,4 ثلاثي امينو-4ʹʹʹ -نايترو زنك فثالوسيانين ((D1 و المركب 4ʹʹ,4ʹ,4 ثلاثي امينو-4ʹʹʹ -نايترو النحاس فثالوسيانين ((D2. المركب ((D1 تفاعل مع المركب ((D2 لينتج المركب ازو- دايمرك نيكل-زنك فثالوسيانين(E) وبعد ذلك دو ديسنايل سكسنك انهايدرايد تضاف لينتج المركب ازو- دايمرك سداسي (دو ديسينايل سكسينك انهايدريد ) نيكل-زنك فثالوسيانين(.(F | المخطط التالي يوضح جميع المركبات المحظرة | == A new substituted phthalocyanines were synthesized from starting materials 4-nitro phthalonitrile and 4-amino phthalonitrile afforded tetra-( (E)-5-(3-(dodec-1-enyl)-2,5-dioxopyrrolidin-1-yl)-2- hydroxybenzoic acid )zinc phthalocyanine (C1), tetra-( (E)-5-(3-(dodec-1-enyl)-2,5-dioxopyrrolidin-1-yl)-2- hydroxybenzoic acid) copper phthalo -cyanine (C2), tetra-( dodecenyl succinic anhydride) zinc phthalocyanine(H1), tetra-( dodecenyl succinic anhydride) copper phthalocyanine (H2) and Azo-dimeric hexa substituted dodecenyl succinic anhydride nickel-zinc phthalocyanine (F) by Many steps. The newly synthesized compounds have been characterized by elemental analysis, FT-IR, 1H NMR, UV-Visible and fluorescence spectroscopies techniques. | There are five lines to synthesis the main goals molecules : | First line : | The reaction of 4- nitro Phthalonitrile with ZnCl2 in the presence of dimethyl amino ethanol (DMAE) afforded 4,4ʹ,4ʹʹ,4ʹʹʹ- tetranitro zinc phthalocyanine(A1). Compound A1 was reacted with 5-amino salicylic acid to yield tetra-(5-amino salicylic acid)zinc phthalocyanine(B1). After that, dodecenyl succinic anhydride was added on amine group of benzoic rings afforded tetra-( (E)-5-(3-(dodec-1-enyl)-2,5-dioxopyrrolidin-1-yl)-2-hydroxybenzoic acid )zinc phthalocyanine(C1). | Second line : | Reacted of 4- nitro Phthalonitrile with CuCl2 in the presence of DMAE afforded 4,4ʹ,4ʹʹ,4ʹʹʹ- tetranitro copper phthalocyanine (A2), which was reacted with 5-amino salicylic acid to yield tetra-(5-amino salicylic acid)copper phthalocyanine (B2). After that, dodecenyl succinic anhydride was added on amine group of benzoic rings afforded tetra-((E)-5-(3-(dodec-1-enyl)-2,5-dioxopyrrolidin-1-yl)-2-hydroxybenzoic acid) copper phthalocyanine (C2). | | Third line : | The reaction of 4- amino Phthalonitrile with ZnCl2 in the presence of DMAE afforded 4,4ʹ,4ʹʹ,4ʹʹʹ- tetra-amino zinc phthalocyanine(G1). Compound G1 was reacted with dodecenyl succinic anhydride afforded tetra-(dodecenyl succinic anhydride) zinc phthalocyanine (H1). | Forth line : | Reacted of 4- amino Phthalonitrile with CuCl2 in the presence of DMAE afforded 4,4ʹ,4ʹʹ,4ʹʹʹ- tetraamino copper phthalocyanine (G2), which was reacted with dodecenyl succinic anhydride afforded tetra-(dodecenyl succinic anhydride) copper phthalocyanine (H2). | Fifth line : | The reaction of 4- amino Phthalonitrile with 4- nitro Phthalonitrile and ZnCl2 or NiCl2.6H2O in the presence of DMAE afforded 4,4ʹ,4ʹʹ-triamino-4ʹʹʹ-nitro Zinc phthalocyanine (D1) and 4,4ʹ,4ʹʹ-triamino-4ʹʹʹ-nitro nickel phthalocyanine (D2). Compound D1 was reacted with D2 afforded Azo-dimeric hexaamino substituted nickel-zinc phthalocyanine (E). After that, dodecenyl succinic anhydride was added on amine group afforded Azo-dimeric hexa substituted dodecenyl succinic anhydride nickel-zinc phthalocyanine (F). | The following scheme explains steps of reaction for the prepared compounds |

دراسة امتزاز الفينول من المحلول المائي على الكاربون المنشط : توازنا حركيا و ثرموديناميكيا == Adsorption of Phenol from Aqueous Solution on Activated Carbon : Equilibrium, Kinetics and Thermodynamic Study

Author name: فرح سلام دعبول
Supervisor name: فلاح حسن حسين
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: ركزت الدراسة على تحضيرمركب من الكاربون المنشط من نوى النخيل العراقي بواسطة التنشيط الفيزيائي و الكيميائي تحليل الاشعة السينية و تحليل المجهر الالكتروني الماسح اثبتت ان المادة المتكونة هي الكاربون المنشط و تم تحضير مركب من الكاربون المنشط و ثنائي اوكسيد التيتانيوم ودراسة خصائص هذا المركب باستخدام تقنيات مختلفة. تم قياس قابلية الامتزاز وفعالية التحفيز الضوئي الكاربون المنشط والمركب المحضر من الكاربون المنشط وثنائي اوكسيد التيتانيوم من حيث سعة الامتزاز والتكسير الضوئي المحفز للمحلول المائي الفينول. | تتكون الرسالة من خمسة اجزاء رئيسة : في الجزء الاول تم تحضير الكاربون المنشط بواسطة التنشيط الفيزيائي و الكيميائي . في الجزء الثاني تم تحضير مركب من ثنائي اوكسيد التيتانيوم باستخدام طريقة الصول جل من مركبين كلوريد التيتانيوم والتيتانيوم ايزوبريبوكسايد. في الجزء الثالث تم تحضير مركب من الكاربون المنشط وثنائي اوكسيد التيتانيوم باستخدام طريقة التجفيف والتبخير البسيط. | في الجزء الرابع تمت دراسة الخصائص الكيميائية والسطحية للمركب المحضر باستخدام تقنيات تحليل رامان و تحليل الاشعة السينية وتحليل الاشعة تحت الحمراء و تحليل المجهر الالكتروني الماسح. تم استخدام تحليل رامان لفحص التداخل الحاصل بين الكاربون المنشط وثنائي اوكسيد التيتانيوم. تشير النتائج الى ازاحة القمم الرئيسية للكاربون المنشط وثنائي اوكسيد التيتانيوم عن مواقعها الاصليه وهذا يشير بوضوح الى التداخل القوي الحاصل بين الكاربون المنشط وثنائي اوكسيد التيتانيوم والذي يمكن ان يؤدي الى انتقال الشحنة من ثنائي اوكسيد التيتانيوم الى الكاربون المنشط وبذلك يمنع عمليه اعادة الاتحاد للشحنات المهمه في عمليه التكسير الضوئي للفينول. | تم حساب معدل الحجوم البلورية لثنائي اوكسيد التيتانيوم وللمركب المحضر من الكاربون المنشط وثنائي اوكسيد التيتانيوم من خلال معادلة شرر والتي كانت مساوية الى 22.797 nmو 24.026 nm لثنائي اوكسيد التيتانيوم وللمركب المحضر على التوالي. | تم دراسة طبيعة تشكل المركب المحضر باستخدام تحليل المجهر الالكتروني الماسح. تشير الصور الناتجة من المجهر الالكتروني الماسح بان الكاربون المنشط توزعت بشكل متجانس خلال حشوة ثنائي اوكسيد التيتانيوم مع ملاحظة تجمعات من دقائق ثنائي اوكسيد التيتانيوم. تم حساب معدل حجوم الدقائق وكانت مساوية الى 100 nm والتي تتطابق مع نتائج حيود الاشعة السينية. | في الجزء الخامس تم اجراء تطبيقين على العوامل المساعدة : | اختير المحلول المائي للفينول كنموذج للمياه الملوثة. تم دراسة سعة امتزاز الفينول في المحلول المائي على سطح الكاربون المنشط, وتم التركيزعلى تاثير عدة عوامل على حركيات الامتزاز عند ظروف ثابتة, مثل كتلة العامل المساعد و الدالة الحامضية وزمن الامتزاز و درجة الحرارة. استخدمت ايزوثيرمات لانكماير وفرندلش و تمكن كموديلات للامتزاز. استخدمت موديلات حركيات الامتزاز الثلاثة وهي حركيات الدرجة الاولى الكاذبة وحركيات الدرجة الثانية الكاذبة و موديل انتشار الدقائق لتفسير حركيات الامتزاز. ووجد بان نتائج الامتزاز العملية كانت مطابقة اكثر الى موديل حركيات الدرجة الثانية الكاذبة. وقد تم دراسة تاثير درجة الحرارة لحساب الدوال الثرموديناميكية مثل قيم طاقة كبس والانثالبية والانتروبية . وقد دلت الدوال الثرموديناميكية الناتجة بان طبيعة امتزاز الفينول تلقائي باعث للحرارة. | تم دراسة الفعالية الحفازية الضوئية من خلال الاكسدة الضوئية المحفزة للفينول لجميع النماذج المحضرة بنسب مختلفة بوجود الاشعة فوق البنفسجية نوع A كمصدر للتشعيع وتمت مقارنة النتائج العملية مع النتائج العملية لثنائي اوكسيد التيتانيوم التجاري (P25). تمت متابعة الانحلال الضوئي الصبغة بواسطة اي عامل مساعد محضر من خلال دراستها طيفيا. تبين النتائج المستحصلة ان الاكسدة الضوئية المحفزة جميعها تطيع معادلة المرتبة الاولى الكاذبة. بينت النتائج تحسن الفعالية الحفازية الضوئية لجميع النسب المحضرة من المركب مقارنة مع ثنائي اوكسيد التيتانيوم لوحده. كذلك بينت النتائج بان اعلى نسبة انحلال ضوئي كانت في المركب AC (10%)/P25 بواقع 6%5. وكانت نسبة الانحلال الضوئي للفينول لنماذج P25 و AC (10%)/P25 مساوية الى 35 و 56% على التوالي. يبدو واضحا بان فعالية المركب AC (10%)/P25اعلى بحدود 1.14 مره من ثنائي اوكسيد التيتانيوم لوحده . | == In this thesis, the preparation of activated carbon (AC) by physical and chemical activation from Iraqi date palm seeds has been explored. In particular, optimized growth conditions that allow the production of long, well aligned, high-quality AC are established. The AC was prepared using a temperature of 700 °C for 120 min, using carbonaceous gas to nitrogen flow rate in a 1 : 1 ratio. SEM and XRD analysis of the prepared composite indicate this product is activated carbon and intermediates in the production of AC/TiO2 composites, and analyzing the prepared composite using different techniques. The adsorption capability of the AC and the photocatalytic activity of the prepared AC/TiO2 samples were quantified in terms of their adsorption capacity and the photocatalytic degradation of phenol. | This research consists of five main parts : | 1. The AC was prepared using physical and chemical activation process. | 2. The TiO2 was prepared from titanium isopropoxide (TIP) and | titanium chloride (TiCl4) using simple sol-gel process. | 3. The AC/TiO2 composites were prepared using simple evaporation | and a drying process. | 4. The structural, morphological and chemical properties of the | prepared AC, TiO2 and AC/TiO2 composites were investigated by | different analytical techniques such as Raman spectroscopy, X-ray | XRD, FTIR and scanning electron microscope (SEM). Raman spectroscopy was used to investigate the interaction of the titanium dioxide (TiO2) with the AC. | | | The results indicate that the main bands of the TiO2 and AC shifted, clearly indicating that the strong interaction between the TiO2 and the AC could enhance the charge transfer from the TiO2 to the AC to separate and stabilize the charge and thereby hinder charge recombination. The Scherrer equation was used to calculate the average crystallite sizes of the TiO2 and AC/TiO2 composites via XRD data. According to calculations, the average crystallite sizes of the TiO2 and AC (10%)/ TiO2 composites were 22.797 and 24.026 nm, respectively. | The morphology of the AC/ TiO2 composites was studied using SEM. The SEM images explain that the AC is homogenously distributed throughout the TiO2 matrix with an apparent agglomeration of the TiO2 particles. The average sizes of the catalyst particles are 100 nm, which is in good agreement with the XRD measurements. | | In the fifth part, two models of applications were performed : | The adsorption capacity of an aqueous solution of phenol was used as a wastewater model to study the treatment activity of AC and AC/TiO2. The adsorption capacity of an aqueous solution of phenol on the AC surface was investigated, particularly focusing on the influence of the experimental parameters on the kinetics adsorption at constant conditions, such as AC dosage, contact time, pH and temperature. Langmuir, Freundlich and Temkin isotherms were utilized as the model adsorption equilibrium data. The Freundlich isotherm model was the most adequate. The pseudo-first order, pseudo-second order and intraparticle diffusion models were used to explain the adsorption kinetics. The experimental adsorption data fitted with the pseudo-second order kinetic. The effect of temperature was quantified by calculating different thermodynamic factors such as G, H and S changes. Thermodynamic parameters indicate that the adsorption is exothermic and spontaneous in nature. | | The photocatalytic activity of the AC/TiO2 composites with 10% of AC was studied and compared with the TiO2. The UV light photocatalytic activity was evaluated by the photocatalytic degradation of phenol in an aqueous solution. The obtained results are discussed in terms of its photodegredation efficiency The comparisons of photocatalytic activity showed that all prepared AC/TiO2 composites was more active than the TiO2 alone. After 60 minutes of UV irradiation, the AC (10%)/TiO2 demonstrated the highest photocatalytic photodegredation of phenol, of which almost 56% was removed. Phenolic degradation of TiO2, AC (10%)/TiO2, also achieved 35 and 56%, respectively. It was observed that the AC (10%)/TiO2 composite had higher activity of about 1.14 times more than TiO2 (P25). |

اغناء وفصل وتقدير كميات فوق النزرة لبعض العناصر الثقيلة والادوية باستخدام التقنيات الطيفية التفلورية == Preconcentration, Separation and Determination of Ultra Trace Quantities of Some Heavy Metals and Drugs by Spectroflourometric Techniques

Author name: احمد سعدون عباس وتوت
Supervisor name: قاسم حسن كاظم | عباس نور محمد
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: Chapter One : explaining illustration of the importance of surfactants uses and types, and also known on cloud point extraction method in analytical chemistry , selection methods of its surfactant , phase mechanisms of its method and factor affecting on its . It also involves briefly review on the modern research of the cloud point extraction and applications for the determination of zinc, chromium, lead, cadmium, arsenic and organic compound (drugs) such as Doxycycline Hyclate and Furosemide . | Chapter Two : involved known on different instrumental techniques used , general apparatus and chemicals used in the cloud point extraction in the present work under study. The full analytical procedures for CPE which have been designed for the determination of analytes (elements and drugs) under study were made in the present work. | Chapter Three : contains the results and discussion including for the separation and preconcentration. First part , included separation and determination on nano gram amount for the metal ions which selected under study of an extraction method used surfactants environmental friendly and ability for its determination by preconcentration in a small volume of the surfactant rich phase and also its methods doesn't used the organic solvent that high expensive and toxicity , the second part include for the ability of determination of its drugs under study by its ion selected in part one and obtained a very low limit of detection, very high sensitivity and a high value of enrichment factors by using cloud point extraction joined with spectroflurimetric technique . | First part of chapter three, included the use of Doxycycline Hyclate (DOX-HYC) as an complexing agent for the establishment of ions-drug complex of Cr(III), Zn(II) and Cr(VI) in alkaline medium. This reaction was form by presence of a non-ionic surfactant in solution, in place of complexes organic reagents which have used in CPE in large field . Furosemide as an complexing reagent, on the other hand, was used for the formation of ion-drug complex Cd(II), As(III) and Pb(II) in acidic medium as a hydrophobic molecule suitable for its separation and preconcentration by CPE. Therefore , a spectrofluorimetric study for the determination of its ions to be exact (Cr(III),Zn(II) and Cr(VI)) of these forms in CPE system at λex. and λem. were 415nm and 511 nm respectively. Different boundaries have been optimized such as pH effective , surfactant amount, organic drug concentration, equilibration temperature and incubation(heating) time. | Under its optimum conditions , results showed that the enrichment factor of 70.42, 43.00 and 84.22 were achieved for each Cr(III),Zn(II) and Cr(VI) species respectively. The linear calibration curve at a linear range for Cr(III) was 0.025-1.0 ng mL-1 with detection limit of 0.0034 ng mL-1, for Zn(II) was 10.0-100.0 ng mL-1 with detection limit of 0.182 ng mL-1, and for Cr(VI) was 0.1-1.0 with detection limit of 0.0019 ng mL-1. The precision for (n=7) at 0.1, 50 and 0.5 ng mL-1 Cr(III),Zn(II) and Cr(VI) were of 2.40% , 0.63 % and 1.41% . Because of the lowest detection limit obtained , the developed method was applied for the determination micro amounts of Cr(III),Cr (VI) and Zn(II) in tap water , R.O and honey samples respectively. The proposed method is compared statistically with GFAAS technique in our laboratory using paired t-test , F test and the results have shown that no significant differences at p=0.05 in accuracy and precision. | On the other hand , this proposed method was used for determination of nano gram amounts of Pb(II), As(III) and Cd(II) using cloud point extraction technique . This method involved the formation of an ion - complex between its ions and Furosemide drug (FUR) in acidic solution and the complex is extracted into the non-ionic surfactant (Triton X-114) at optimum conditions. The surfactant-rich phase which contains ions-complex is dissolved with solvent and the solution was measured spectrofluorimeterically at λex and λem = 363 and 409 nm respectively. The effects of the several variables which affect the CPE efficiency are optimized and the thermodynamic study was also examined for all complexes in a non-ionic surfactant under study. The enrichment factor of 62.44, 149.00 and 42.34 for each Pb(II), As(III) and Cd(II) respectively obtained leading to detection limits of 0.0953, 0.0000892 and 0.321 ng mL-1 in aqueous solution for each Pb(II), As(III) and Cd(II) respectively . | The concentrations range obey Beers law of 1.25-15.0 , 0.01-0.1 and 6.75-50.0 ng mL-1 for each Pb(II), As(III) and Cd(II) respectively. The precision for (n=7) at 5, 0.08 and 10 ng mL-1 Pb(II), As(III) and Cd(II) were of 1.96% , 1.52 % and 1.73% . The developed method was used for the determination of its ions in honey, and for Pb(II) and Cd(II) in powder and liquid milk samples, and the results were compared statistically with HGAAS, and GFAAS technique using paired t-test and F -test at p=0.05 concluding there are no significant differences in accuracy and precision. | The second part of this chapter includes, a new spectroflurimetric method has been developed for the determination of its drugs, ( Doxycycline Hyclate and Furosemide) by cloud point extraction system. These determinations were obtained under the optimum conditions and the concentration for the selected drugs were measured using spectroflurimetic at each λem. It was found that the enrichment factors of 74.87, 93.47 and 172.69 for Doxy-Zn(II), Cr(III) and Cr(VI) were achieved leading to the very low limit of detection of 2.2×10-8, 1.3×10-9 and 1.1×10-9 ng mL-1 respectively. While for the complexes of Furo-Pb(II), As(III) and Cd(II) were 111.32, 184.33 and 166.80 respectively, were achieved leading to the low limit of detection of 1.1×10-9, 1.4×10-11 and 2.5×10-11 ng mL-1 respectively . | The established method showed linear calibrations in the range for Doxy-Zn(II), Cr(III) and Cr(VI) were 2.0×10-6 -2.0×10-3 , 1.0×10-7 -1.0×10-3 and 2.0×10-7 -2.0×10-3 ng mL−1 respectively. Also for Furo-Pb(II), As(III) and Cd(II) were 1.0×10-7 -1.0×10-3 , 2.0×10-9 -2.0×10-4 and 2.0×10-9 -2.0×10-4 ng mL−1 respectively .The quantum yield for all complexes that extracted in surfactant rich phase were calculated .The developed method was applied for the determination of the Doxycycline Hyclate in blood serum samples |

دراسة مقارنة لتحضير وتشخيص العامل المساعد Ni3O4 - Co3O4 - Al2O3 واستخدامه في الاكسدة الضوئية والامتزاز لصبغتي Reactive Yellow145 و Bismarck brown G

Author name: ايمان جاسم محمد
Supervisor name: عباس جاسم عطية | صالح هادي كاظم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: تضمنت الدراسة تحضير العامل المساعد Ni3O4-Co3O4-Al2O3 بنسب وزنية مختلفة و بطريقة الترسيب المشترك في درجات حرارة 500 و 600 و 700 م⁰ وبفترة زمنية 4 ساعات وتم تشخيص هذه النسب المحضرة بعدة تقنيات وهي حيود الاشعة السينية (PXRD) وطيف الاشعة تحت الحمراء (FTIR) و التحليل الحراري الوزني والمسح المسعري التفاضلي (TGA/DSC) و قياس المساحة السطحية (BET) ومجهر القوة الذرية (AFM) وتحديد الصفات الفيزيائية والتاكد من المسامية والحجم المسامي والكثافة لهذه النسب بطريقة التشبع بالسائل. بعد ذلك تم استخدام جميع هذه النسب المحضرة والمكلسنة بجميع الدرجات الحرارية في الاكسدة الضوئية المحفزة لصبغتي Bismarck brown G و Reactive yellow145 ووجد ان افضل نسبة تعطي افضل تكسير للصبغتين هي النسبة Cat4 المحضرة من (40 : 40 : 20)% والمكلسنة بدرجة حرارة 600 م⁰ . | درست الظروف المثلى للتكسيرالضوئي المحفز لصبغة Bismarck brown G من اختيار الوزن الامثل للعامل المساعد والدالة الحامضية المثلى و والدرجة الحرارية الفضلى. ووجد ان افضل وزن للعامل المساعد المحضر هو 0.2 غم وافضل دالة حامضية هي 3 وافضل درجة حرارية هي 300 كلفن, كما تم حساب طاقة التنشيطE ∆ لتفاعل الاكسدة الضوئية المحفزة وكانت ) 27.89 ) كيلوجول/ مول. تم دراسة ايزوثيرمي الامتزاز لانكماير وفرندلش وقد وجد ان الامتزاز كيميائي اي يتبع امتزاز لانكماير, كما درست حركيات الامتزاز ووجد ان التفاعل يتبع الرتبة الثانية الكاذبة. كما تم دراسة اعادة التدوير للعامل المساعد المحضر مع هذه الصبغة ووجد ان الفعالية تقل بعد الاستخدام الاول للعامل المساعد وتنخفض الفعالية من 92.4% الى 23.2%. | كذلك درست الظروف المثلى للتكسير الضوئي المحفز لصبغة Reactive yellow 145 ووجد ان افضل وزن للعامل المساعد هو0.1 غم وافضل دالة حامضية هي 3 وافضل درجة حرارية للتكسير هي 296 كلفن, كذلك تم حساب طاقة التنشيط E∆ وكانت (18.11) كيلوجول/مول. ايضا تم دراسة ايزوثيرمي الامتزاز لصبغة Reactive yellow 145 ووجد ان الامتزاز فيزيائي اي يتبع فرندلش ايزوثيرم , ودرست حركيات الامتزاز وكان التفاعل يتبع الرتبة الثانية الكاذبة. كما درست اعادة التدوير للعامل المساعد مع الصبغة وقد وجد ان الفعالية تبقى ثابتة لاستخدامين متتاليين في تكسير الصبغة اما عند استخدامه للمرة الثالثة وجد ان الفعالية تنخفض الى 80.1%. | == This study involves synthesis of the co-catalyst Ni3O4-Co3O4-Al2O3 at different ratios by co- Precipitation method with different calcination temperature 500, 600, 700 ⁰C at a heating rate of 10 C/min under normal atmospheric conditions for four. The obtained materials were characterized using powder X-rays diffraction (PXRD), fourier transform infrared (FTIR), thermogravimatric analysis (TGA/DSC), surface area determination (BET), and atomic force microscopy (AFM), In addition to that some of physical for properties these ratio were undertaken including measurement of porosity, pore volume, and volume density by impregnation method. Then used all of these ratio that calcinated at different temperature in oxidtion process of both reactive yellow 145 (RY145) and Bismark brown G (BBG) from their aqueous solutions. It was found that the catalyst with a ratio of (40 : 40 : 20) %, which was calcinated at 600 ⁰C (denoted as cat4) it’s the bast ratio. | | Removal of BBG was investigated after optimization of removal conditions such as pH of mixture, amount of the used catalyst , duration time of reaction and reaction temperature. The optimum conditions for this case were pH=3, 0.2 g of cat 4 and temperature equal to 27 ºC. Activation energy was calculated using Arrhenius plot and it was around 27.89 kJ/mol. Kinetics of this process was investigated and it was fitted with the pseudo second order kinetics. In addition to that, adsorption isotherms for this process were applied for both Langmuir and Freundlich adsorption isotherms. The obtained results showed that it was agreed with Langmuir adsorption model. recyclization processes were applied for removal of BBG over cat 4, and it was found that the activity of cat 4 was reduced from 92.4% for the first trial to 23.2%. | Removal of RY145 over cat 4 was investigated and the optimum conditions in this case were, pH=3, 0.1 g of the cat 4 and temperature was 23 ºC. Additionally the activation energy was calculated as mentioned above and it was around 18.11 KJ /mol. Kinetics of this processes was investigated and it was similar to that reported for removal of BBG over cat4. Also adsorption isotherms were performed using Langmuir and Freundlich adsorption model and it was found that, it was fitted with Feundlich isotherm model. Cyclization process for RY145 over cat 4 was evaluated and it was found that the activity of cat 4 doesn't change after two successive usages. But the activity of cat 4 was educed third usage and it was declined to reach 80.1%

تحضير وتشخيص معقدات قواعد شف ثنائبة النواة مع ليكندات حلقة كبيرة رباعية السن == Synthesis and Characterization of Schiff Base Binuclear Complexes with Tetra Dentate Macrocyclic Ligands

Author name: طارق حســـــين مغـــــير
Supervisor name: عاشور حمود داود | حسين عبد محمد
General topic: Chemistry
Specific topic: Inorganic Chemistry
Degree: Doctorate
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: تضمن العمل تحضير و تشخيص معقدات ثنائية النوات مختلفة ومتشابهة وبطريقة القالب حيث اعتمد في بداية العمل على تحضير مشتقات هي P1 - P5 مشتقة من ثلاثة مركبات ثنائية الكيتون هي ( البنزويل اسيتون و الازاثين و5و2 هكسات ثنائي الكيتون) حضر ت المشتقات من خلال تفاعل ثنائي الكيتون مع اورثو امينو فينول مرة و مع اورثو امينو ثايوفينول مرة اخرى بعدها تم تحضير نوعين من المعقدات ثنائية النواة النوع الاول هو معقدات ثنائية النواة المتشابهة من خلال استخدام مشتقات مختلفة مع املاح فلزات متشابهة حيث تم تحضير المعقدات بطريقة القالب باستخدام المادة الجسرية مع مكافئين من المشتق و مكافئين من ملح الفلز ليتكون المعقد المطلوب لمعقد ثنائي النواة .. | النوع الثاني من المعقدات ثنائية النواة هي معقدات ثنائية مختلفة النواة اي تستخدم املاح فلزين مختلفين في المعقد الواحد حيث يتم تحضير المعقد المطلوب بطريقة القالب ايضا با ضافة المادة الجسريةهي خماسي اريثرويتول رباعي البروميد مع مكافئين من المشتقات المحضرة و مكافئ واحد من كل ملح من املاح الفلزات المستخدمة و هي النيكل الثنائي و النحاس الثنائي ليتكون المعقد ثنائي مختلف النواة المطلوب . المخططات (1و2و3و4) توضح تلك التفاعلات . | تم استخدام التقنيات الحديثة في تشخيص المركبات المحضرة حيث استخدمت مطيافية الاشعة تحت الحمراء و الفوق البنفسجية - المرئية ومطيافية الرنين النووي المغناطيسي للبروتون و الكاريون - 13 و التشخيص الكمي الدقيق للعناصر ( كاربون نايتروجين هايدروجين كبريت ) و طيف الكتلة كما درست قياسات الحسابية المغناطيسية للمعقدات و توصيل الكهربائية المولارية اضافة الى دراسة الخصائص الفيزيائية للمركبات المحضرة من قياس درجة الانصهار و الذوبانية في مذيبات مختلفة و طيفية الالوان المتكونة. | ومن المعلومات الطيفية و الخصائص الفيزيائية للمركبات المقترحة تم اقتراح الاشكال الفراغية للمعقدات المحضرة كالتالي : | 1. معقدات الكوبلت جميعهراباعي السطوح مع كافة المشتقات المحضرة . | 2. معقدات النيكل هي مربعة مستوية مع كافة المشتقات المحضرة | 3. معقدات النحاس مع P1 هي رباعي السطوح و مربعة مستوية مع بقية المشتقات | == The work covered the synthesis and characterization of homo and hetero nuclear complexes through the template reaction. | The preparation of precursors P1- P5 was carried out via reaction of benzoyl acetone, Isatin and 2,5 hexane dione, the three diones treated with O-aminophenol or O-amino thiophenol. The N2O2 and N2S2 type donor atoms compound was used as | Starting material with metal ions and the bridge penta arythretol tetrabromide | in template reaction to prepare the binuclear complexes. | The first type of complexes was prepared using homo metal ions, the precursors type N2O2 and N2S2 was mixed with pentaerythretol tetrabromide and two equivalents of metal ion salts at the same time stirred and refluxed to produce the complexes in title as homo binuclear macro cyclic compounds . | The second protocol was included the preparation of heterobinuclear complexes, the procedure was carried out via reaction of precursors with bridge compound pentaerythretol tetrabromide with different metal ions salts Cu2+ and Ni2+ to obtains the heterobinuclear complexes as N4S4 and N4O4 Macrocyclic coordination compounds. Schemes (1, 2, 3 and 4) shows all these reactions. | | The prepared compounds and complexes were characterized by different methods. | And the physical properties were studied using FT-IR,UV,1H NMR,13C NMR, mass spectra and C.H.N.S Spectroscopies to identify the prepared compounds. | The solubility of prepared compounds was investigated in different solvents, Molar conductivity was carried out for complexes using DMSO as a solvent The study showed that all complexes were electrolytes with 1 : 4 ratio. | The magnetic susceptibility was measured to determine the magnetic moments of complexes the results showed that the cobalt(II)and copper(II) complexes were Paramagnetic in different values of μeff, while the study shows the Ni2+ | complexes were diamagnetic. | From the spectroscopic and physical studies the suggested geometry of the complexes were as follow : - | 1-The cobalt(II) complexes are tetrahedral with the different precursors. | 2-The nickel(II) complexes are square planar with the different precursors. | 3-The copper(II) complexes are tetrahedral with Precursors P1 ,while the others is square planar |

دراسة التاثيرات الكيموحيوية لمستخلصات نبات الريحان على الارانب المصابه بسمية الكبد من خلال نظام الاكسده - مضادات الاكسده == A Study of Biochemical Effects of Ocimum sanctum L. Extracts on Hepatotoxicity in Rabbits Via Oxidant - Antioxidant System

Author name: سارة صالح مهدي التميمي
Supervisor name: لمياء عبد المجيد المشهدي
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
University: University of Babylon - College Of Science
Language: English
University location: Babylon
Abstract: تضمن البحث دراسة المكونات الفعالة في المستخلصات المائية(الباردة والحارة) والكحولية (70%) لنبات الريحان الذي جمع من الاسواق المحلية في مدينة الحلة. من خلال التقدير النوعي والكمي لمستخلصات نبات الريحان حيث بينت نتائج التقدير النوعي ان المستخلص المائي الحار والكحولي يحتويان مكونات فعالة اكثر مثل الفلافونيدات ,القلويات, الصابونيات ,التانينات ,التربينات , الكلايكوسيدات والاحماض الامينية او الامينات الاولية والثانوية مقارنة بالمستخلص المائي البارد. | اتضح من التقدير الكمي للمستخلصات ان المستخلص المائي الحار والكحولي يحتويان مكونات فعالة مثل الفلافونيدات ,القلويات, الصابونيات والتانينات بنسب مختلفه مقارنة بالمستخلص البارد. و تضمنت الدراسه تقدير الفعالية البايولوجيه للمستخلصات المائيه والكحولية لنبات الريحان باستخدام اربعة انواع مختلفة من السلالات البكتيرية موجبة لصبغة كرام(Staphylococcus aures, Streptococcus pyogenes) وسالبة لصبغة كرام (Salmonella typhi and Klebsiella) باستخدام طريقة الانتشار في الاكار وبتراكيز مختلفة من المستخلصات ( 200,100 , 50)ملغم/مل وبينت النتائج ان المستخلص الكحولي يمتلك اكبر قطر للتثبيط ضد ثلاثة انواع بكتريا هي (Staphylococcus aures, Streptococcus Pyogenes and Klebsiella) عند التركيز 200ملغم/مل مقارنة مع المستخلصات المائية التي تعطي نتائج تثبيط اقل .من هذه النتائج يتضح ان الاستخلاص بالايثانول ( (70%اثبت فعاليته في عزل المكونات الفعالة (نوعيا وكميا) وان التركيز 200ملغم للمستخلص الكحولي هو افضل تركيز مقارنة بالتركيز(100 , 50) ملغم من نفس المستخلص كونه يعطي افضل قطر للتثبيط ضد مختلف انواع البكتريا لذلك اعتبرنا ان الجرعة الفعالة هي 200ملغم/كغم من وزن الجسم حيث استندنا على نتائج التقدير النوعي والكمي والفعالية البايولوجيه في الحصول على الجرعة المؤثرة والتي تم استخدامها بعد ذلك كجرعة مؤثره لعلاج الحيوانات المختبريه المصابة بسمية الكبد. | ولتحديد الزمن الفعال تم تقسيم (30)ارنب والتي تتراوح اوزانهم بين (900-1500)غم الى خمسة مجاميع حيث تحتوي كل مجموعه على ستة ارانب وهذه المجاميع هي : ( (G1 مجموعه السيطرة, ( (G2المجموعه المستحث فيها سمية الكبد بواسطة CCl4)), ( (G3 المجموعة المعالجه ,(G4)المجموعه الوقائية و (G5)هي المجموعة التي تعامل بالمستخلص الكحولي فقط (وتعتبر مجموعة سيطره ثانيه) . وبعدها تم اعطاء المستخلص | | الكحولي لحيوانات المجموعه الثالثة ,الرابعة والخامسة وتم قياس انزيمات الكبد مثل (AST, ALT, ALP , TP and Alb) في اوقات مختلفة لمعرفة الزمن الفعال الذي يؤدي الى اكبر تاثير في وظائف الكبد ,حيث اتضح ان الزمن اربع ساعات هو الزمن المؤثر والفعال والذي تم الاستناد عليه في التجارب اللاحقة. | ولدراسة تاثير المستخلص الكحولي العلاجي والوقائي لنبات الريحان ضد سمية الكبد المستحثة بواسطة رابع كلوريد الكاربون (CCl4) تم قياس انزيمات الكبد مثل AST, ALT, ALP, TP and Alb لهذه المجاميع وبينت النتائج ان مستويات انزيماتAST, ALT and ALP سوف تزداد بينما مستويات انزيمات ((TP and Alb سوف تنخفض بالنسبة للارانب المصابة بسمية الكبد بواسطة رابع كلوريد الكاربون لمدة اسبوع وان معالجة الارانب بالمستخلص الكحولي لنبات الريحان قللت من مستويات انزيمات الكبد لتصبح قريبة من القيم الطبيعية للمجموعة الاولى(مجموعة السيطره) وهذه النتائج توضح الطبيعة الوقائية لنبات الريحان ضد ماده رابع كلوريد الكاربون والتي تسبب تلف الكبد. | اضافه الى ذلك فان دراسة المقاطع النسيجية لكبد الارانب المختبريه تدعم النتائج التي تم الحصول عليها من خلال قياس انزيمات الكبد والتي تبين التاثير الفعال للمستخلص الكحولي لنبات الريحان وذلك يعود الى كون نبات الريحان هو احد النباتات الطبية التي تمتلك خواص مضادات الاكسده. | == The research included the phytochemical study of aqueous(cold and hot)and ethanolic extracts (70%) of Ocimum sanctum L. that were collected from local markets in Hilla. The investigation of phytochemical constituents involved the qualitative and quantitative analysis. The results for qualitative analysis explained that the aqueous hot and ethanolic extracts contained more amounts of active components such as flavonoids, saponins, tannins, alkaloids, terpenoids, glycosides and amino acids or primary and secondary amines rather than cold extract ,while the quantitative analysis illustrated that the aqueous hot and ethanolic extracts containing different percentages of flavonoids, saponins, tannins and alkaloids more than cold extract. | Antibacterial activity was also analyzed for the aqueous and ethanolic extracts of Ocimum sanctum L. with different concentrations (50,100,200) mg/ml using four different bacterial strains which are gram positive : Staphylococcus aures, Streptococcus pyogenes and gram negative : Salmonella typhi and Klebsiella using agar diffusion method and the results showed that ethanolic extract had the biggest zones of inhibition at the concentration 200mg against Staphylococcus aures, Streptococcus pyogenes and Klebsiella compared with aqueous extracts that gave less results of zones of inhibition. | From these results which illustrated that extraction with ethanol (70%) proved its effectiveness in the isolation of active components and the concentration 200mg was the best concentration for ethanolic extract which given the best results of inhibition zones against different types of bacteria. Therefore, the active dose was 200mg/kg body weight based on the results of qualitative, quantitative and antibacterial activity to get the active dose that was used in the treatment of experimental animals induced hepatotoxicity. | To determine the active time , thirty rabbits were divided into five groups for six rabbits in each group with body weight of (900-1500)gm and these groups were : (G1) is the control group that received normal saline, (G2) is the toxic control that received CCl4 for one week, (G3)is the treated group, (G4) is the preventive group and (G5)that treated with ethanolic extract only(it's considered as a second control group).Then ethanolic extract was given to the rabbits of (G3, G4 and G5) and the liver function enzymes like(AST, ALT, ALP, TP and Alb)were measured for these groups in different times to detect the active time which leads to the greater impact in liver function and it became clear that four hours is the active time that was used in the next experiments. | Then to study the hepatoprotective effect of ethanolic extract of Ocimum Sanctum L. on hepatotoxic rabbits that induced by CCl4 , the liver function enzymes such as AST ,ALT ,ALP ,TP and Albumin were measured for these groups and the results indicated that the levels of AST ,ALT and ALP were significantly increased while the levels of TP and Albumin were decreased in rabbits that received CCl4 for one week. Post treatment with Ocimum sanctum L. extract for two weeks made the levels of liver enzymes become nearer to the normal values of G1.These findings demonstrated the protective nature of Ocimum sanctum L. against CCl4 that induced liver damage. In addition, the histopathological studies of liver sections support the results that were obtained from serum liver enzymes which appeared the hepatoprotective effect of ethanolic extract and this was due to the antioxidant properties that have been found in Ocimum sanctum L. plant. |

تخليق مشتقات جديدة لمركبات اللاكتام و البريميدين و دراسة فعاليتها كمضادات للاكسدة و مضادات للاورام == Synthesis, Anti - Oxidant And Anti - Tumor Activity Of New Lactam And Pyrimidine Derivatives

Author name: عبد الرحمن يسر خليفة الغزي
Supervisor name: محمود شاكر مكطوف التميمي | حسام محمد كريديا
General topic: Chemistry
Specific topic: Organic Chemistry
Degree: Doctorate
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: In the end of last century the increasing of cancer disease has been speared in worldwide, has been pushing to investigate more in synthesis a new drug treatment herein, the idea in this thesis three types of heterocyclic compounds | were synthesized : | 1- Synthesis of a series of β-lactams 3(a-h) compounds by using Kinugasa reaction and Staudinger reaction, which β-lactam 3(a-b) compounds (as depicted in scheme below) were synthesized using Kinugasa reaction by reacting alkyne (phenylacetylene and 1-octyne) with the appropriate nitrones 2(a-b) in the presence triethylamine and CuI as catalyst and acetronitrel as solvent at 0˚C. R1 : 4-NHCOCH3 , 3-NO2 R2 : CH3(CH2) , 5 While β-lactam 3(c-h) compounds (as depicted in scheme below) were synthesized using Staudinger reaction by reacting methoxyacetyl chloride with the appropriate imines 2(c-h), in the presence of triethylamine in dry dichloromethane under nitrogen atmosphere at 0˚C.3c : R1= −C6H4Cl , R2= −C6H4− , 3f : R1= −C6H4Me , R2= −C6H4− | 3d : R1= −C6H4Br , R2= −C6H4− , 3g : R1= −C6H4Br , R2= −C6H4− 3e : R1= −C6H4Cl , R2= −C6H4− , 3h : R1= −C4H4N2 , R2= −C6H4− 2- Synthesis of a series of γ-lactams 4(a-h) (as depicted in scheme below) by reaction phenylsuccinic anhydride or 3-(4-chlorophenyl)dihydrofuran-2,5- dione with schiff bases (imines) 2(d,e,g,i,j,k,l,m), by using chloroform as solvent and heated at temperature (55-60˚C) Synthesis of a series of 3,4-Dihydropyrimidin-2(1H)-ones/ thiones 5(a-g) (as | depicted in scheme below) by reaction aldehyde, ethyl acetoacetate and | urea/thiourea under FeCl3.6H2O as catalyst, by using ethanol as solvent and heated at reflux temperature. | H2N NH2 | FeCl3.6H2O | ethanol , reflux | ethyl acetoacetate urea or thiourea aldehyde 5(a-g)The final products were characterized by using the basis of the spectral data : | IR, 1H-NMR, 13C-NMR and Mass. | The antioxidant activity for the synthesized compounds (3g, 4a, 5a) were examined and show highly biological activity response. Moreover, the activity against breast cancer MCF-7 cell line also studied and exhibited highly anti tumor.

تقدير بعض العناصر الثقيلة في نماذج حقيقية باستعمال مركبات ازو - ازوميثين جديدة بواسطة استخلاص نقطة الغيمة == Determination Of Some Heavy Metals In Real Samples Using New Azo - Azomethine Compounds By CPE

Author name: ساجدة صبار عفات
Supervisor name: ساهر عبد الرضا علي الشمخاوي
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Doctorate
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: Since its inception in 1985, Cloud-point extraction (CPE) methodology has constituted an important theme in the analytical chemistry as promising procedure for the separation and preconcentration for the metal ions and organic compounds from the complex matrices samples. Nowadays, it has been begins to take a large noteworthy position among the other modern separation methods in scientific research and application on a high level due to its simplicity, rapidity, more precise and cheapness beside an environmentally-friendly method, therefore, this research includes three main chapters . | Chapter One includes introduction of azo-azomethine compounds and their complexes and a view of the different extraction techniques, fundamental principles and potential applications of CPE methodology in analytical chemistry. It also involves a concise review on the latest developments of the method and its applications for the determination of cadmium, copper and cobalt by CPE . | Chapter Two consists of an outline of different instrumental techniques , general apparatus and chemicals used in the present work. | The synthesis paths of azo-azomethine compounds (L1 to L4) and primary testing of complex formation between metal ions and reagents, determination of λmax . As well as optimization of the experimental conditions (volume reagent, reaction time, temperature and pH) and determination of dissociation degree and stability constant, stoichiometry of the complex (Continuous variation method -Job method). In addition CoCl2.6H2O and L4 with salts CrCl3.6HO and CdCl2.H2O. The analytical | procedures for CPE which were designed for the determination of analytes including optimization of the Parameters for CPE including (reagent concentration, HCl concentration, incubation time, equilibration temperature, thermodynamic study and Triton X-100 volume) were selected in this study. The present CPE method was applied for determination concentration of metal ions (Cd2+, Cu2+ and Co2+) in real samples by FAAS. | Chapter Three included the new azo-azomethine compounds prepared and their complexes which were characterized by various analytical techniques as a UV-Visible spectroscopy(UV-Vis), Infrared Spectroscopy(FT-IR), Nuclear Magnetic Resonance Spectroscopy(1HNMR), Mass Spectra and Molar Electrical Conductivity for complexes and the results were identical to what is expected scientifically. The spatial shape of the complexes which was prepared is (octahedral) and stoichiometry of the complex. It’s ratio 1 : 1. | In chapter three, there are too highlights on the results and discussion in analytical applications for the separation and preconcentration for the metal with separation and extraction method, such as cloud-point extraction (CPE) as an separation technique that uses a surfactant, instead of organic solvents for phase separation. | In the first part of CPE, Analytical reagent namely 6-((1E)-((2-(((E)-2-hydroxy-3-methoxy-4-((6-methoxybenzo[d]thiazol-2- yl)diaz enyl)benzylidene)amino)benzyl)imino)methyl)-2-methoxy-3- ((6- methoxybenzo[d]thiazol-2-yl)diazenyl)phenol (L1) after synthesis and characterization by using various analytical techniques as a preliminary using various analytical techniques as a preliminary step toward its using | as an organic reagent for the formation of an ion-association complex | with copper ion in acidic medium, apt to interact with surfactant in | solution. The L2 as a reagent for the formation of an ion association | complex with copper in acidic solution and the complex is extracted into | the surfactant Triton X-100 at optimum conditions. The surfactant-rich | phase which contains copper complex is mediated with solvent and the | Cu content measured by FAAS (λmax = 324.75 nm) . The effects of the several variables which affect the CPE efficiency are optimized by OFAT procedure beside other parameters with which one is mentioned with Cu(II) . The thermodynamic study was also investigated to expand the understanding of the mechanism of solvation of Cu(II) in the micelles . | Under the optimized condition established, the enrichment factor of 52.574 was achieved for Cu2+ with the L2 . The concentration range of (0.01-3) μg ml-1 leads to detection limit of 0.017238 μg ml-1. The precision for ((%RSD, n=8) at 0.05μg.ml-1 Cu2+ was of %1.063. The developed method was used for the determination concentration of Cu2+ in real samples. The accuracy was determined by recovery percentage for real samples, it’s found good recoveries (100.380-103.377%) for Cu2+ with L2. | In the third part CPE, Analytical reagent namely6-(((2-(((E)-2- hydroxy-3-methoxy-4-(o-tolyldiazenyl)benzylidene)amino) benzyl)imino)methyl)-2-methoxy-3-(o-tolyldiazenyl)phenol(L3)was synthesised and fully characterized by using various analytical techniques | as a preliminary step toward its using as an organic reagent for the formation of an ion-association complex with cobalt ion in acidic medium and the complex is extracted into the surfactant Triton X-100 at optimum conditions for determination of Co(II) as CoCl4 | 2- ion by using the combined cloud point extraction (CPE) methodology. After phas separation, the surfactant-rich phase was diluted with 1M HNO3 in methanol and cobalt (II) ion determined by FAAS technique at λmax of 240.72 nm. The optimization of complexation and extraction conditions was investigated. Thermodynamic parameters of CPE for solubilization process of the ion-pair complex in Triton X-100 were also considered. | Under the optimized conditions, the preconcentration of a 15ml sample which gave preconcentration and enrichment factors were of 15 and 54.078 respectively. The calibration graph was linear in the range of (0.025-3) μg ml-1 with a limit of detection and quantitation limit 0.011534 and 0.038446 μg ml−1. The relative standard deviation for replicate determinations at 0.05μg ml−1 level was of (0.823%, n=8). The proposed | method was applied for the determination of cobalt in river, tap waters, milk, black tea , tobacco and soil by FAAS. The accuracy was determined by recovery percentage for real samples, it’s found good recoveries (101.108-104.918%) for Co2+ with L3 . The study of the stoichiometry for ion association complexes using the slope analysis technique showed that the ion association complex ratio was 1 : 1 for all extracted complexes

دراسات سريرية وجينية في امصال الدم والسائل المنوي للمدخنين وغير المدخنين المصابين بالعقم غير المفسر في محافظة ذي قار - العراق == Biochemical and Genetic Studies of Sera and Semen for Smokers and Non Smokers with Unexplained Male Infertility in Thi - Qar Province/ Iraq

Author name: وسام ريسان نايف المحسن
Supervisor name: رائد معلك حنون | ساجد حسن كزار
General topic: Chemistry
Specific topic: Clinical Biochemistry
Degree: Doctorate
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: This study was conducted on infertile subjects attending to the infertility Unit in Al-Hussein Teaching Hospital in Thi-Qar province south of Iraq, during the period from Aug 2016 to May 2017. The aim of study was to determine the roles of the presence of some biochemical parameters (oxidative stress, antioxidants), antisperm antibodies and polymorphism for glutathione peroxidase (GPx1) and glutathione transferase (GTSp1) in men with unexplained infertility. | Ninety men with unexplained male infertility (UMI) aged (91-91) year and fifty healthy fertile men aged (20-25) year were included in this study as a control group, had no systemic diseases and none were taking an oral antioxidant supplement for three months prior to the study. | The patients and control were divided into two groups (smoker and non smoker). Serum and seminal fluids were collected from each of them, seminogram test (semen analysis) was performed for each participant, and all semen samples were collected following (3-5) days of abstinence. After liquefaction, semen volume, sperm concentration, total sperm count, morphology, motility grades were determined using World Health Organization (WHO) standard procedures. | In this study, there is no significant (P>0.05) between age and body mass index (BMI) of unexplained infertile men compared with age of fertile men (control). The groups of the unexplained infertile males with history of infertility of 3-5 years duration were largest groups who attended medical services. The majority of the unexplained infertile men (90%) complained of primary infertility while the minority of them (10%) complained of secondary infertility. The current study revealed that effect smoking on unexplained infertile group was percentage (44.4%) comparison with control fertile group (36 %). | )II( | The results of semen analysis for the fertile (control) and the unexplained infertile men, revealed no significant differences (P>0.05) in semen volume, liquefaction time, and semen pH between the two groups in (smoker and non smoker). A significant decrease (P<0.05) was seen in the sperm concentration, sperm motility, total progressive sperm (progressive sperm motility and non-progressive sperm motility) and normal sperm morphology in the unexplained infertile group compared with the fertile group (control). While a significant increase (P<0.05) was seen in immotile sperm, sperm agglutination, round cells count and leukocytes in the unexplained infertile group compared with the fertile group (control). | The results showed a significant increase (P<0.05) in serum and seminal plasma Malondialdehyde (MDA) in unexplained infertile (smoker and nonsmoker) groups when compared to fertile (smoker and nonsmoker) groups. The antioxidant such as vitamins (C and E) and glutathione were significantly decreased in serum and seminal plasma for unexplained infertile (smoker and nonsmoker) groups when compared to fertile (smoker and nonsmoker) groups. | A significant increase in serum Ceruloplasmin(Cp) levels in unexplained infertile group comparison with fertile (control) group (P<0.05). Significant differences (P<0.05) in seminal plasma fertile (smoker and non smoker) groups but there was no statistical difference in the Ceruloplasmin level of seminal plasma unexplained infertile between two groups (smoker and non smoker) groups and no significant difference between smoker fertile group with unexplained Infertile (smoker and non smoker) groups. | High prevalence of antisperm antibody (ASA) in seminal plasma for unexplained male infertility a percentage (25.5%) compared with infertility (control) a percentage (14%), and significant differences in ASA seminal plasma | )III( | (Smoker and non smoker) in all groups, which indicator that high in Smoker men compared with non smoker . | In this research found association between the glutathione peroxidase (GPx1) polymorphism and unexplained male infertility, and effect oxidation and antioxidant on these. Therefore, might be a major risk factor of unexplained male infertility in the studied groups, suggested a stronger association between smoking consumption and risk of unexplained male infertility. | The frequency of the glutathione transferase (GSTp1) genotype showed almost no difference between the unexplained infertile men and the fertile controls, therefore, in this case-control study, the GSTp1 variant genotype (Ile/ Ile ,Ile/ Val , Val/ Val) was no significant different in every group of unexplained infertile men compare than in the fertile (control group).This indicating no significant association between GSTp1 and sperm parameters.

دراسة وظائف الكبد وصورة الدهون والاجهاد التاكسدي في مصول النساء قبل وبعد استئصال المرارة في محافظة ذي قار / العراق == Study of Liver Function, Lipid Profile and Oxidative Stress in Sera of Women Pre and Post Cholecystectomy in Province of Thi - Qar/ Iraq

Author name: سمى يعقوب يوسف
Supervisor name: رائد معلك الصالح | مهند عبد الرضا الشريفي
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: The present study has been designed to evaluate and compare changes in patients pre, post and long periods for cholecystectomy on BMI, liver function (Aspartate Amino Transferase (AST), Alanine Amino Transferase (ALT), Alkaline Phosphatase (ALP), Total Bilirubin (TSB), Total Protein (TP), lipid profile (Total Cholesterol (TC), Triglyceride (TG), High Density Lipoprotein (HDL), Low Density Lipoprotein (LDL), Very Low Density Lipoprotein (VLDL)), oxidative stress (Malondialdehyde (MDA), Nitric Oxide (NO)) and antioxidant state (Albumin (Alb), Ceruloplasmin (CP)). | The study includes (192) subjects : (64) normal subjects (control) and (128) patient’s cholecystectomy, their age range (20-69) years, the patients were divided in to three groups : (64) patients pre and 24 hr post operation cholecystectomy, (64) patients after long periods for cholecystectomy, as well as the patients were divided by age into two groups : a premenopausal group and a postmenopausal group. | The results show that there were a significant decreased in the concentration of serum (AST, ALT, TSB, DB, InB, HDL and Alb) in group pre in comparison with each of post (short and long terms) and control groups (p≤0.05). It was found no significant differences in the concentration of serum (AST, ALT, TSB, DB, InB, HDL and Alb) between each of post (short and long terms) groups (p≤0.05). Also it was found significant differences in the concentration of serum (AST, ALT, TSB, DB, InB, HDL and Alb) between each of post (short and long terms) and control groups (p≤0.05). | -----------------------------INDEX--------------------------------- | XII | While the results showed a significant increase in the concentration of serum (ALP, TP, TC, LDL, NO, MDA and Cp) in all patient groups in comparison with control groups (p≤0.05). It was found no significant differences in the concentration of serum (ALP, TP, TC, LDL, NO, MDA and Cp) between each of post (short and long terms) groups (p≤0.05). Also it was found significant differences in the concentration of serum (ALP, TP, TC, LDL, NO, MDA and Cp) between each of post (short and long terms) and control groups (p≤0.05). | Also the results showed a significant increase in the concentration of serum TG and VLDL in all patient groups in comparison with control groups (p≤0.05). It was found no significant differences in the concentration of serum TG and VLDL between each of post (short and long terms) groups in the group A (p≤0.05). But it was found a significant difference in the concentration of serum TG and VLDL between each of post (short and long terms) in the group B (p≤0.05). Also it was found a significant difference in the concentration of serum TG and VLDL between each of post (short and long terms) groups and control groups (p≤0.05). | The correlation between nitric oxide and each of (ALP, TP, TC, TG, LDL, VLDL, MDA and Cp) in these patient groups were positive. Whereas the correlation between nitric oxide and each of (AST, ALT, TSB, BD, InB, HDL and Alb) in these patient groups were negative. | The above reviewed results lead to conclusion that cholecystectomy causes variant alternations in serum hepatic function and lipid profiles and causes variant effects in serum oxidative stress. Also, age has no effect on each of (ALT, TSB, DB, InB, ALP, TP, TG, VLDL, NO, MDA, Cp and Alb), while age has effect on each of (TC, LDL and HDL). Besides, there are no effect of the period after cholecystectomy on all studied parameters except TG and VLDL.

تحوير فجوة طاقة ثاني اوكسيد التيتانيوم بواسطة تفاعلات الحالة الصلبة مع صوديوم بوروهيدريد والمنيوم ليثيوم هيدريد وتحديد فعالية التحفيز الضوئي == Modifying The Band Gap of Nano Titanium Dioxide By Solid State Reactions With Aluminum Lithium Hydride and Sodium Borohydride and Determining Their Photocatalytic Activity

Author name: سراج علي رحيم
Supervisor name: محسن عريبي الدخيلي | ابراهيم عبود فليفل
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: This study includes preparation of nanoparticles of titanium dioxide using sol-gel method and then, the band gap was modified by solid state reaction with (AlLiH4،NaBH4) reductive compounds. Modification reduced the band gap separating | energy levels between valance band (VB) and conduction band (CB), therefor; facilitating the transfer of excited electrons from (VB) to (CB). Absorption of the energy from incident photons having the same or larger energy than the energy of the | band gap promote the formation of the couple (electron - hole) . The resulting (e--h+) couple acts to produce (OH.) radicals. OH. radicals hav a high capability to destroy organic pollutants that adsorbed on surface of the photocatalytic TiO2. | The optical properties measured using UV-visible spectrophotometer (Absorbance (A), energy band gap (Eg) and absorption coefficient ( α ) . TiO2 and TiO2- solid state reaction showed clear blue shift of the absorption band gap which were (2.8ev, 2.7ev, 2.25ev, 2.0ev) to )TiO2- NaBH4(550 ) ,TiO2-NaBH4 (750 ) , TiO2-AlLiH4 (500 ) and TiO2 -AlLiH4 (750 )) respectively. The structure of prepared TiO2 nanopowders were identified using XRD, particle size distribution varied appreciably in comparison with crystallite size (D) calculated from Sheerer formula which was in a good accordant compared with ASTM results , the particle size and their distribution were characterized using (AFM) . To the surface forms and compositions diameters of nanoparticles)SEM) was implemented . The energy dispersive X-ray (EDX) microanalysis was utilized to investigate the chemical composition of the whole samples. | Photocatalytic reaction was studied by using UV-Vis spectrophotometry. | In photocatalytic reaction the effect of the catalyst on photocatalytic rate of decomposition of methylene blue dye through the use of catalyst TiO2 and TiO2- solid state reaction (TiO2 - NaBH4 (550 ,750 )) and (TiO2 - AlLiH4 (500 ,750 )) . Using constant weight of the catalyst and dye. The most effective weight was found (1*10-4 M). At best weight the influence of many factors on rate of decomposition of dye were studied the impact of change pH varies (4.5, 7.1 and 9.4) found that the highest percentage in the decomposition of the MB was in the acidic media than in neutral and then alkaline. The effect of temperature variation from (20, 30, 40ºC) and found that increased rate of decomposition with increasing the temperature of the MB. Activation energy (Ea) for each reaction was calculated by using the equation of Arrhenius equation between (5.73-11.31) kJ mol-1 . | A series of dark reactions with absorbance measurement by UV-Vis spectrophotometry, within different periods of time with the change of pH and temperature. The results indicate that no degradation of the methylene blue dye although all the factors affecting in photocatalytic present except UV-light .

تحضير تشخيص والخصائص الكهربائية لبعض للليكاندات الجديدة المستندة على 4.3.1 اوكسادايزول، 4.3.1 ثايادايزول و 4.3.1 ترايازول ومعقداتها

Author name: امل حسين نعيثل الزيدي
Supervisor name: محسن عريبي الدخيلي | ابراهيم عبود فليفل
General topic: Chemistry
Specific topic: Inorganic Chemistry
Degree: Doctorate
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: The thesis include preparation and characterization of some new derivations of, 1,3,4-thiadiazole ,1,2,4-triazole and 1,3,4-oxadiazole as ligands that describe blowThe new complexes were prepared from the reactions of ligands L1, L2, L3, and L4 with transition metal salts (CrCl3.6H2O, FeCl3, CoCl2.6H2O and NiCl2.6H2O). | The elemental analysis (CHN), Infrared (IR) Spectroscopy, Nuclear magnetic resonance spectroscopy (1H NMR), Mass spectra magnetic Susceptibility and flame atomic absorption were used to characterize the structural formula of these ligands and their complexes. | Based on the results of the analytical and spectral measurements of the prepared complexes in this study, and compare them with literature in relation to coordinate sites in ligand. We can suggest the following shapes for the complexes : | 1- With regard to L1 we can conclude that its tridentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of three of the chloride ions, the geometric shape can be proposed to be octahedral geometry. For nickel (II) Complex the ligand acts as bidentate with two chlorine ions, the geometry is tetrahedral geometry (weak field ligand). | 2-for L2 we can conclude that its tridentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of three of the chloride ions, the geometric shape can be proposed to be octahedral geometry. For nickel (II) Complex, the ligand acts as bidentate with two chlorine ions, the geometry is square plainer geometry (strong field ligand). | 3 -for L3 we can conclude that it's bidentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of two of the chloride ions, the geometric shape can be proposed to be tetrahedral geometry. For nickel (II) Complex, the ligand acts as bidentate with two chlorine ions, the geometry is square plainer geometry (strong field ligand). | 4 - For L4 we can conclude that it is bidentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of two of the chloride ions with two molecule of ligand, the geometric shape can be proposed to be octahedral geometry. For nickel (II) Complex, the ligand acts as bidentate with two chlorine ions, the geometry is square plainer geometry (strong field ligand). | The study also examined the electrical conductivity for both of L1, L3 and their complexes with (Co(III), Fe(III), and Cr(III)) in the presence and absence of iodine. | The study showed that both L1 and L3 are semiconductors and the electrical conductivity of L1 is greater than that of L3. The complexes of these ligands has significantly increased their electrical conductivity and Iron complexes are the most complex electrical conductivity complexes. | As for iodine doping of ligands and their complexes, it was found that iodine increases the conductivity of ligands while decreasing the conductivity of the complexes. However, despite the decrease in the conductivity of the complexes, the conductivity is still higher than those of the free ligands. | A theoretical study for ligands (L1 and L3) and their complexes by Gaussian 09 program and calculate the total energy , HOMO ,LUMO and energy gap for all the studied compounds were found semiconductor

التحقيق في اثار الحجامة الرطبة على بعض المؤشرات البايوكيميائيه في ذي قار محافظة / العراق == Investigation of The Effects of Wet Cupping Therapy on Some Biochemical Parameters in Thi - Qar Governorate/ Iraq

Author name: زهراء طالب مشلول
Supervisor name: محمد عجة عودة
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: This study was designed to determine the effect of cupping to treat or reduce a lot of blood variables such as diabetes, liver failure, lipid profile and status of Oxidative and antioxidant , where we have in this study to take blood samples from the volunteers before they activate cupping therapy and then we have to take more samples within 14 days and comparing the results obtained were as follows : The results of the blood glucose concentration decreased significantly (P≤0.05) post cupping when compared with a pre-cupping, while there is no significant decrease in the level of glucose in the blood serum of a group post cupping compared with the control group (P≥0.05 ). In addition, the group pre-cupping showed a significant increase (P≤0.05) in the glucose in the blood serum when compared with the two sets of post-cupping and the control group. It can be seen the results of MDA serum showed a decrease (P≤0.05) in the group post cupping, compared with a pre-cupping, while non-significant in the serum level of MDA in the group post cupping compared with the control group (P≥0.05). While the group pre cupping significant (P≤0.05) MDA in serum when compared with the two sets of post-cupping and control. Summary | XIV | Cp serum levels showed high significant increase (P≤0.05) in | serum Cp can be observed in the two groups pre and post cupping when comparing this with the control group, In addition, the total post-cupping has shown a significant decrease (P≤0.05) in serum Cp compared with a pre-cupping. | As well as the results showed Alb serum significantly increased (P≤0.05) in Alb serum can be observed in the two groups pre and post cupping when compared with the control group, as a group post the cupping showed that there was a significant decrease | (P≤0.05) in Alb serum compared with a pre cupping. | Liver function tests showed a significant decrease in the group post cupping, compared with a pre cupping (P≤0.05), while significant difference was observed liver enzymes levels (ALT, ALP and AST) in the serum can be observed in a post-cupping compared with the control group (P≤0.05). Moreover, the group pre-cupping showed a significant increase (P≤0.05) in levels of ALT, ALP, AST serum when the two groups to be compared with the postcupping and the control group. | Fat results in the serum showed little change, but did not reach the moral (P≥0.05) in the proportion of fat in the blood serum levels of lipoproteins among all groups studied. | In the end we can say that cupping is not used for treatment once and for all, but it's used to treat Alternatively, or in a more identification used to treat complementary.

طريقة كروماتوغرافية طيفية جديدة - لتقدير عقار اللوراتادين في بعض المستحضرات الصيدلانية == Anew Chromatographic - Spectrophotometric Method for Determination of Loratadine in Some Pharmaceutical Preparations

Author name: صفاء حكيم ناصر الغزاوي
Supervisor name: محمد تركي خثي
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
Abstract: Due to the medicinal significance of Loratadine, ethyl4-dihydro-11H benzo [5,6] cyclohepta [1,2-b] pyridin-11ylidene (-1-piperidinecarboxylate) has been devoted to this message To create a new chromatographic-spectral method for estimating the pure drug and the drug found in a number of its pharmaceuticals. | The letter included a detailed explanation of a new chromatographic-spectral method for estimating amounts of pure and commercial loratidine. The principle of this method is to break down the double bond present in the loratadine by the potassium permanganate oxidant factor of 0.05 molar and convert it into two ketone-containing compounds : 8-Chloro-5,6-dihydro-11H-benzo [5,6] cyclohepta [1,2-b The second compound is ethyl-4-oxopiperidine-1-carboxylate (B). It has been shown that the two compounds (A and B) can be separated by TLC, FTIR, separated and completely isolated by column chromatography technique. After the separation, the compound (A) was given a stable colorant complex with 4-amino acid benzoic acid ester, in a acidic medium, While the compound ( B ) did not give a stable complex. The results showed a study of changing the conditions of the process of analysis and separation of the two compounds and their diagnosis and the formation of the resulting complex and applications of the method and discussed with the use of different quantities of many types of acids and strong and weak rules and indicate their impact on the intensity of the complex complex color and the optimal conditions were selected for his way of work.

تخليق وتشخيص لبعض المركبات الحلقيه الغير متجانسه كالبيتا لاكتام والكاما لاكتام وفق تفاعل كانيكوزا == SYNTHESIS AND CHARACTRIZAITION OF SOME NEW HETROCYCLIC COMPOUNDS INCLUDING ? & ? LACTAMS BY USING KINUGASA REACTION

Author name: دعاء هادي محسن العطار
Supervisor name: محمود شاكر مكطوف | محسن عريبي الدخيلي
General topic: Chemistry
Specific topic: Organic Chemistry
Degree: Master
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
First pages:
Abstract: This study is concerned with the synthesis and characterization of the some β- lactams 3(a-f),as in (Table.2). These compounds 3(a-f) were prepared by reacting phenylactylene with the appropriate nitrones2(a-f), in the presence of triethylamine | in acetronitrel under nitrogen atmosphere at -10˚C. in moderate yield (50-70)% . The nitrones compound 2(a-f) were prepared by reacting aldehyde with appropriate N-phenyl hydroxyl amine 1 in the presence of Ethanol. | As in (Table.1) Also the N-phenyl hydroxyl amine 1 compounds were prepared by reduction of nitrobenzene with ammonium chloride in Zinc Powder in the presence of water.This study is concerned with the synthesis and characterization of mono-γ- | lactams and bis-γ-lactams These compounds were prepared by reaction phenylsuccinic anhydride with the appropriate schiff bases(imines), by using chloroform solvent and heated at temperature (51-61˚C) in moderate yields(70- 92)%, All this compound confirmed by using spectra data such as : , IR , 1H-NMR , 13CNMR , APT 13C-NMR , HSQC 1H-13C-NMR,Mass

التاثير الوقائي للخلاصة المائية لاوراق نبات الزريج STZ على الكبد واعتلال الخصوبة في ذكور الجرذان المصابة بالسكري بواسطة == Potential Role of Aqueous Extract From Chrozophora Tinctoria Leaves on Liver and Fertility Dysfunction in STZ Induced Diabetic Male Rats

Author name: منى حسون عبودي
Supervisor name: محمد عجة عودة
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Doctorate
University: University of Thi-Qar - College Of Science - Chemistry Department
Language: English
University location: Dhi Qar
First pages:
Abstract: This study was designed to investigate the pharmacological effects on air dried Chrozophora tinctoria (L.) Rafin plant samples as well as the responses of streptozotocin (STZ)-induced diabetic rats for the aqueous Chrozophora tinctoria (L.) Rafin leaves extracts. To achieve this aim, phytochemicals analysis were carried out by various standard assays and then antioxidant compounds contents in the three parts of the plant (leaves, stems, and roots) estimated by common spectroscopic methods. In addition, physiological, biochemical and histological parameters of (STZ) diabetic rats are evaluated too. Rats are distributed into five groups : Control, diabetic rats and three diabetic groups received orally different doses of (50, 70, and 90 mg/kg body weight (BW)) from the target extract for a period of 35 days. When the therapy is ended, blood samples, liver and testis tissues were taken and concentration of glucose, insulin, lipid profile, HbA1C, as well as the activity of ALT, AST, ALP, male sexual hormones were determined as well as liver and testis histology. In general, the results of this study show that the liver and testis tissue were damaged, serum ALP, AST ALT activities, HbA1C, lipid profile, T, LH, FSH, insulin and blood glucose levels were remarkable normalized. It was observed that the BW of diabetic control group is decreased. However the BW elevated slightly in the diabetic treated groups as well as serum insulin and male hormones. In addition, the extract improves the liver function and reduces lesions associated with diabetic state in STZ induced rats. Moreover, the effect of oral administration of Chrozophora tinctoria (L.) Rafin at a dose of 90 mg / kg body weight was more efficient than the 50 and 70 mg/kg body weight. Furthermore, the obtained results related that male reproductive system showed remarkable increased of sperm count, viability and motility after treatment with dose 70 mg/kg of body weight. Histological examination of the testis revealed improvement of spermatogenesis and Leydig cell proliferation with all doses of the extract. However, the histological features of the rats testis received 70 and 90 mg/kg, was found to be similar to the healthy group. The whole results indicated that the extract exhibited protective effect on liver tissues, as well as maintained the damage fertility in diabetic rats. These investigations explain its potentials as an antidiabetic, hepato protective agent, and promising therapeutic to recover male subfertility

تحضير وتشخيص مركبات حلقية غير متجانسة تحتوي على حلقات - 1,2,3ترايازول و - 1,3,4ثايادايزول == Synthesis and Characterization of New Heterocyclic Compounds Containing 1,2,3 - Triazole and 1,3,4 - Thiadiazole Rings

Author name: نور حميد عمران
Supervisor name: رياض جليل ناهي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: Al-Muthanna University - College Of Science - Chemistry Department
Language: English
University location: Muthanna
First pages:
Abstract: تم في هذه الرسالة تحضير وتشخيص و دراسة الاستقراية الحرارية لسلسلة جديدة من مركبات حلقية غير متجانسة تحتوي على 3,2,1-ترايازول وحلقة 4,3,1-ثايادايزول ومجموعة الايمين (قواعد شف). تضمن الجزء الاول من البحث تحضير مشتقات 3,2,1-التراياازول 53-57 باستخدام تفاعل الاضافة الحلقية بين الازايد والالكاين بوجود مركبات النحاس الاحادي كعامل مساعد. لذا تم تحضير سلسلة من مركبات الازايد الاروماتي 48-52 كمكونة الازايد المطلوب في تفاعل الاضافة الحلقية بينما تم استخدام حامض البروباينويك المتوفر تجاريا كمكونة الالكاين. ان استخدام حامض البروباينويك في هذا التفاعل يؤدي الى تعويض حلقة 3،2،1-التراياازول بمجموعة كاربوكسيل وبالتالي يمكن استغلالها في الكثير من التفاعلات لتحضير مركبات مشتقات جديدة لتطبيقات مختلفة. | بعد تحضير مشتقات 3,2,1-الترايازول، تم التركيز على استغلال مجموعة الكاربوكسيل في تحضير حلقة4,3,1- ثايادايزول متجمعة مع حلقة 3,2,1-التراياازول وذلك من خلال مشتقات الترايازول 53-57 المحضرة مع ثايوسيمي كاربازايد بوجود زيادة من POCl3 وبالتالي الحصول على سلسلة جديدة من المركبات الحلقية الجديدة تحتوي على4,3,1- ثايادايزول متجمعة مع حلقة 3,2,1-الترايازول في جزيئة واحدة 53-57. بسبب احتواء المركبات الناتجة على مجموعة امين معوضه مباشرة على حلقة الثايادايزول في الموقع C2, لذا تم استغلال هذه المجموعة لتحضير سلسه جديده من مشتقات قواعد شف وذلك بالتفاعل مع اثنين من الالديهايدات الاروماتية بارا برومو بنزالديهايد وبارا نايترو بنزالديهايد. | وتم تشخيص جميع المركبات المحضرة بمقياس الاشعة تحت الحمراء FT-IR ومطيافية الرنين النووي المغناطيسي ومطيافية الكتلة. | علاوة على ذلك تم دراسة السلوك الحراري للمركبات المحضرة بتقنية التحليل الحراري الوزني | TGA والتحليل الحراري التفاضلي الوزني .DTG | == This thesis describes the synthesis, characterization and thermal study of new heterocyclic compounds containing 1,2,3-triazole, 1,3,4-thiadiazole and imine moieties at the same molecule. Firstly, the copper (I) catalyzed azide-alkyne cycloaddition (CuAAC) was the method choice for the synthesis of the target 1,2,3-traizole derivatives 53-57. Thus, a series of p-substitution phenyl azides 48-52 was designed as azido components of this reaction which was synthesized via reaction of diazonium salts with sodium azide. The propiolic acid was chosen as an alkyne building block in CuAAC reaction. Importantly, choosing propiolic acid as a second moiety of CuAAC reaction is allowed to functionalize the target 1,2,3-triazole derivatives 53-57 with a carboxyl group. The latter, can be exploited in different reactions and applications. The main efforts are focused to exploit their carboxyl function groups for the combination of 1,2,3-triazole ring system with 2-amino-1,3,4-thiadiazole ring system. However, new series of heterocyclic compounds containing 1,2,3-triazole and 1,3,4-thiadiazole moieties at the same molecule was synthesized through condensation reaction between the synthesized 1,2,3-triazole derivatives 53-57 with thiosemicarbazide in the presence of POCl3. Furthermore, as the synthesised compounds 57-62 containing an amino function group attached into the C2 position of 1,3,4-thiadiazole ring, it was exploited for the synthesis of new heterocyclic compounds containing 1,2,3-triazole, 1,3,4-thiadiazole and imine moieties in one molecule. All the synthesized compounds were characterized by the FT-IR, NMR and Mass spectroscopies. For further investigations, the thermal behavior of the synthesised compounds was studied by TGA and DTG techniques

تحضير وتشخيص مشتقات جديدة ل 1،2،3 ترايزول - المحتوية على 4،1،3 اوكسادايزول - ومجموعة الازو == Synthesis and Characterization of New 1,2,3 - Triazole Derivatives Containing 1,3,4 - Oxadiazole and Azo Moieties

Author name: زينب كزار كويت راضي
Supervisor name: رياض جليل ناهي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: Al-Muthanna University - College Of Science - Chemistry Department
Language: English
University location: Muthanna
First pages:
Abstract: This thesis describes the synthesis, characterization and thermal study of new 1,2,3-triazole derivatives containing 1,3,4-oxadiazole and azo moieties. For the synthesis of the target 1,2,3-traizole derivatives 61-67, the copper (I) catalyzed azide-alkyne cycloaddition (CuAAC) was the method choice. Since the azide compounds being considered as a substrate for (CuAAC), a series of substituted phenyl azides was synthesized via reaction of diazonium salts with sodium azide, while the commercially available propiolic acid was chosen to be the alkyne function. Choosing of propiolic acid as an alkyne component of click reaction is allowed to functionalize the target 1,2,3-triazole derivatives with a carboxyl group function which can be exploited in different reactions and applications. Having the target 1,2,3-triazole derivatives 61-66, our efforts focused to exploit their carboxyl function groups for the synthesis of new heterocyclic compounds containing 1,3,4-oxadiazole moieties. A new series of compounds containing on 1,2,3-triazole and 1,3,4-oxadiazole moieties on the same molecule was synthesized through a condensation reaction between the synthesized 1,2,3-triazole derivatives 61-66 and semicarbazide hydrochloride followed by dehydro-cyclization step in the presence of POCl3. On the other hand, compound 67 was synthesized as an unnatural amino acid containing 1,2,3-triazole ring and is ready for different reactions such as diazonium salts formation. Thus, this unnatural amino acid was exploited in the synthesis of new three azo compounds following the standard procedure that is used in the synthesis of the azo compounds 74-73. The synthesized compounds introduce the 1,2,3-triazole and azo moieties on the same molecule thereby new applications can be reported. All synthesized compounds were characterized by the FT-IR, 1H-NMR, 13C-NMR and GC-MS spectroscopies. For further investigations, the thermal behavior of the synthesized compounds was studied by TGA and DTG techniques.

تحضير وتشخيص 4,1 - بس (اميدازول - 1 - يل مثيل) بنزين - سليكا ودراسة فعاليته كعامل مساعد == Synthesis and characterization of 1,4 - bis (imidazole - 1 - yl methyl) benzene - silica and its catalytic activity

Author name: نهلة غازي فهد
Supervisor name: قاسم محمد حلو
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: Al-Muthanna University - College Of Science - Chemistry Department
Language: English
University location: Muthanna
First pages:
Abstract: في هذه الدراسة تم استخلاص السيلكا من قشور الرز عن طريق غسل قشور الرز مرات عديدة بالماء المقطر، ثم عوملت مع محلول (1مولاري) من حامض النتريك، بعد ذلك احرقت في فرن بدرجة حرارة 800 درجة مئوية ، تم تحويل السليكا الناتجة الى سيليكات الصوديوم بعد ذلك تم مفاعلتها مع CPTES ينتج سليكا ذات مجموعة وظيفية --CH2Cl رمز لها بالرمز .RHACClتم تحميل الاميدازول المتفاعل مع كلوريد بارزاايلين على سطح .RHACClلتكوين العامل المساعد غير المتجانس رمز له .RHAPrIM تم تشخيص العامل المساعد بعدة تقنيات منها تحليل العناصر والتحليل الوزني الحراري TGA/DTA وتحليل امتزاز النتروجين ومطيافية الاشعة تحت الحمراء FT-IR وكذلك اطياف الرنين النووي المغناطيسي للحالة الصلبة لنواة ذرتي الكربون والسيليكون ( ( 29Si , 13C MAS NMRوكذلك المجهر الالكتروني الماسح SEM والمجهر الالكتروني النافذ.TEM طبقا الى نتائجCHN ،.EDXلوحظ زيادة نسبة الكربون اكثر مما هي عليه في RHACCl وبين التحليل كذلك وجود نسب من النتروجين والتي لم تكن موجودة سابقا في المركبRHACCl. اظهر تحليل الرنين النووي المغناطيسي للحالة الصلبة لنواة ذرة السيليكون29Si وجود ازاحات كيميائية تعود الى Q4،Q3 ، T3، T2 عند ازاحات كيميائية في الطيف حسب الادبيات. اما تحليل الرنين النووي المغناطيسي للحالة الصلبة لنواة ذرة الكربون13C اظهر حزما عند مواقع كيميائية مختلفة تعود لذرات الكربون في العامل المساعد المحضر. في حين بينت نتائج التحليل الحراري TGA/DTA امكانية استخدام العامل المساعد حتى 277 درجة مئوية دون ان يتفكك . وطبقا لصور المجهر الالكتروني النافذ TEM ظهرت دقائق ذات اشكال منتظمة وبحجم 5 نانومتر ، بعضها ملساء والاخرى كانت مسامية.درست الفعالية التحفيزية للعامل المساعدRHAPrIM في حمل ايون النتريت لتحضير حامض النتروز المستخدم في تحضير املاح الدايزونيوم . يعتبر حامض النتروز المادة الاساسبة لتحضير الاصباغ ، حيث حظرت اصباغ مختلفة عن طريق تفاعل الازدواج بين المركبات الاروماتية واملاح الدايزونيوم. شخصت الاصباغ المحضرة بواسطة تحليل العناصر، FT-IR واطياف UV-Vis . لوحظ تطابق النتائج العملية والمحسوبة لتحليل العناصر لمركبات الازو المحضرة. تم اعادة استخدام العامل المساعد عدة مرات و بثباتية عالية. == In this study, silica was extracted from rice husk via washing rice husk many time with distilled water, and then treated with 1.0 M of Nitric acid; finally, it was burned in an oven at 800 oC. The ash was converted to sodium silicate and reacted with chloropropyltriethoxysilane to form RHACCl. Imidazole with p-xylylene dichloride was loaded onto RHACCl in the form of p-xylylbisimidazole to form solid catalyst donated RHAPrIM. Various analytical techniques were well characterize the catalyst including CHN analysis, TGA/DTA, FT-IR, N2-adsorption desorption study, 29Si &13C MAS NMR spectra TEM, SEM and EDX. According to the CHN results, it was noticed that the carbon percentage increased from (11.70%) in RHACCl to (16.704%) in RHAPrIM; also the results were showed a present of nitrogen in RHAPrIM which was not present in RHACCl. Silicon solid-state nuclear magnetic resonance showed Q4, Q3, T3, and T2 chemical shifts at expected position. 13C spectrum showed different peaks at different chemical shifts related to the carbon structures of the organic moieties. Thermal analysis showed that the catalyst could be used safely up to 277 ºC. TEM images of RHAPrIM showed regularly shaped particles with an estimated size 5 nm. Some particle seems to be smooth in shape, while the others showed a porous shape. The catalytic activity of RHAPrIM was examined in-situ preparation of nitrous acid which was used in the preparation of diazonium salt. The RHAPrIM was used to produce nitrous acid via it’s reaction with nitrite ions. Nitrous acid is the key start materials for dyes preparation via diazonium salt. Coupling reaction of aromatic compounds was carried out with a diazonium salt to yield a mono azo dye. All dyes were characterized by elemental analysis, FT- IR, and UV-Visible spectra. Both calculated and found results of elemental analysis of prepared azo compound were match with each other. The catalyst was stable and regenerated within a simple experimental procedure

تحضير وتشخيص بعض مونيمرات وبوليمرت جديدة محتوية على حلقات غير متجانسة ودراسة خواصها الحرارية والفعالية البايولوجية == Synthesis and Characterization of Some New Monomers and Polymers Containing Heterocyclic Rings and Study Their Thermal Properties and Biological Activity

Author name: غادة مهدي كامل الزبيدي
Supervisor name: هلال مسعود عبد الله | ابتسام خليفة جاسم
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
University: University of Baghdad
Language: English
University location: Baghdad
First pages:
Abstract: يتضمن موضوع البحث تحضير مركبات حلقية غير متجانسة ثلاثية (الازردين و فنيل ازردين), خماسية (اوكسادايازول و ترايازول و تترازول), وخماسية ملتحمة (بنزوثايازول) والتي استخدمت لتحضير العديد من البوليمرات. | الجزء الاول : | يتضمن هذا الجزء تحضير مركب 2,3(1-ازردين)ماليك انهدريد[1] وبلمرته مع اثلين كلايكول و 1,3-بروبلين دايول و كليسيرول000الخ للحصول على رابطة استرية كما موضح بالشكل ادناه : | الجزء الثاني : | يتضمن هذا الجزء تحضير مركب 2,3(فنيل ازردين)ماليك انهدريد[12] وبلمرته مع اثلين كلايكول و 1,3-بروبلين دايول و كليسيرول000الخ للحصول على رابطة استرية كما موضح بالشكل ادناه : | الجزء الثالث : | يتضمن هذا الجزء تحضير مركب 3,2,ثنائي [2-مركبتو-5-يل-4,3,1-اوكسادايازول]1-ازردين [24] وبلمرته مع ثنائي كلوريدات الحامض للحصول على رابطة ثايواسترية كما موضح بالشكل ادناه : | الجزء الرابع : | يتضمن هذا الجزء تحضير مركب بنزوثنائي-2-امينوثايازول [29] وبلمرته مع ثنائي كلوريدات الحامض للحصول على رابطة امايدية كما موضح بالشكل ادناه : | الجزء الخامس : | يتضمن هذا الجزء تحضير مركب 4,1-ثنائي [3-مركبتو-4-(5-(بارا-فنيل)تترازولين)-5-يل-4,2,1-ترايازول] بيوتان [34] وبلمرته مع ثنائي كلوريدات الحامض للحصول على رابطة ثايواسترية كما موضح بالشكل ادناه : | * شخصت (المونمرات والبوليمرات) المحضرة باستخدام مطيافية FT.IR وUV/Vis و 1HNMR و 3CNMR وCHN كما قيست درجات انصهارها. | *درست اللزوجة و الصفات الحرارية لبعض البوليمرات المحضرة. | *كما تم تقييم الفعالية الحيوية لبعض البوليمرات المحضرة لتحديد امكانية استخدامها كمركبات ذات تطبيقات طبية. | == This work involves synthesis of different three (Aziridine, Phenyl azridine), five (Oxadiazole, Triazole, Tetrazole), and fused five (benzothiazole) member heterocyclic rings which used as a monomer for preparing many different polymers. | First part : | This part involves the synthesis of 2,3[1H-aziridine]maleic anhydride[1] and polymerized with ethylene glycol, 1,3-propylene diol, glycerol,…..etc. to get the polymers having ester linkage as shown below | This part includes the synthesis of 2,3[1-phenyl-aziridine]maleic anhydride[12] and polymerized with ethylene glycol, 1.3-propylene diol, glycerol,…..etc. to get the polymers having ester linkage as shown below This part includes the synthesis of 2,3-Bis[2-mercapto-5-yl-1,3,4-oxadiazole]1H-aziridine[24] and polymerized with diacid chlorides to get the polymers having thioester linkage as shown belowThis part contains the preparation of five member rings fused with benzene ring, its Benzobis-2-aminothiazole [29] and polymerized with diacid chlorides to get the polymers having amide linkage as shown belowIn this part, the compound 1,4- Bis[3-mercapto-4-(5-(p-substituted phenyl)tetrazolin)-5-yl-1,2,4-triazole]butane [37], [38] and polymerized with different diacid chlorides to get the polymers having thioester linkage as shown below In this part, the compound 1,4- Bis[3-mercapto-4-(5-(p-substituted phenyl)tetrazolin)-5-yl-1,2,4-triazole]butane [37], [38] and polymerized with different diacid chlorides to get the polymers having thioester linkage as shown below
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