Abstract: Novel series of 14 (urea and thiourea) derivative compounds were prepared from reaction of urea and thiourea with aromatic amine compounds (homocyclic and heterocyclic), in addition to preparation of 6 Schiff bases (C=N) compounds that were prepared from reaction of some derived compounds with benzyldehyde in this study. All the 20 prepared compounds were characterized according to F.T.I.R. spectra, purities were examined by T.L.C., and the melting points were measured to identify each of them.From November 2005 through March 2006, a sample of (urine and sera) from 200 patients suffering U.T.I. and urinary stone attending (Diwaniya Teaching Hospital, Pediatrics and Gynecology Teaching Hospital, Health Centers and Private Clinical Laboratories) in Diwaniya, another sample was collected from 100 healthy persons as a control group.The inhibition activity was measured for each of 9 commercially used antibiotics, and for the all prepared compounds in vitro against Proteus bacteria isolated from patients under this study and identified by valid laboratory methods (Api - 20E method).From (renal and bladder) 13 stones were collected from patients to detect the type of each stone by qualitative chemical analysis. Also the level of blood urea, serum uric acid, random blood sugar, serum creatinine and serum calcium, was measured for all samples in this study.This study shows the following results : Bacterial growth for Proteus and other kind of bacteria were found in 138 patients out of the 200 (69 %), while Proteus spp. was isolated from 23 representing by 16.66 % of Proteus spp. out of the 138 patients of U.T.I.. Results of biochemical tests showed that Proteus mirabilis was found in 21 isolates with 91.3 %, and Proteus vulgaris in 2 isolates with 8.7 %.Erythromycin was found to have the lowest inhibitory activity against Proteus spp. isolates with a percentage of resistance 86.9%, while Gentamycin have the highest inhibitory activity with a percentage of resistance 4.3 %. In bacterial sensitivity test among the 9 antibiotics was commonly used in this study.The prepared compounds showed inhibitory activity against growth of isolated Proteus spp. in (19 out of 20) compounds, [N - (5 - phenyl - 1,3,4 - thiadiazole) - 2 - ylthiourae] shows the highest inhibition activity with a diameter of inhibition zone 30 mm., while the [ N - pyridine - 4 - ylurea] shows no such activity in the same concentration, as compared with Gentamycin antibiotics which shows 18 mm diameter of inhibition zone.Struvite stones were commonest type of stones in patients with 61.5 %, followed by apatite carbonate stones with 30.7 % then mixed stones with 7.85 %.Statistical analysis shows a significant difference (P < 0.05) of the levels of blood urea, uric acid, serum creatinine and serum calcium for the patients when compared to that of control group. While no significant difference (P > 0.05) is observed or the R.B.S. level between the same groups.

محاكاة التحليل بالتنشيط النيتروني باستخدام طريقة مونتي كارلو وتطبيقه لنماذج بيئية == Simulation of Neutron Activation Analysis Using Monte Carlo Method and Application for Environmental Samples

Author name: ضياء شامخ زغير

Supervisor name: Hussain Al - Shahristani | Shahbaz A. Maki

General topic: Chemistry

Specific topic: Chemistry

Degree: Doctorate

University: Al-Nahrain University - College Of Science - Chemistry Department

Language: English

University location: Baghdad

First pages:

Abstract: تم تصميم ودراسة منظومتين للتحليل بالتنشيط النيتروني وفي كلا المنظومتين تم استخدام Am - Be كمصدر نيوتروني. احدى المنظومات استخدم فيها مصدرين من ال Am - Be مختلفي الفيض النيتروني تم محاكاتها نظريا لحساب توزيع الفيض النتروني على طول محور التشعيع باستخدام طريقة مونتي كارلو وحزمة برنامج Geant4 ذي خصائص البرمجة كائنيه المنحى . تمت مقارنة نتائج المحاكاة المستحصله للمشعع النيتروني البرافيني مع مشعع نيتروني مائي افتراضي وقد اظهرت النتائج ان توزيع الفيض النيتروني على طول محور التشعيع بالنسبة للمشعع المائي كانت اعلى منها للمشعع البرافيني . تم حساب الفيض النيتروني الحراري (تحت الكادميوم ) وفوق الحراري والسريع (فوق الكادميوم ) عمليا للمشعع البرافيني على طول محور التشعيع ومن ثم مقارنتها بالنتائج النظرية وكانت النتائج التي تم الحصول عليها متطابقة الى حد بعيد. استخدمت نفس هذه المنظومة لقياس تركيز النحاس في بعض المركبات وبتركيز ولغاية 10 ملغم، كما وتم تقديره في بعض المحاليل المائية المحضرة قياسيا بعد زيادة تركيزه.المنظومة الاخرى كانت لتحليل بالتنشيط النيتروني الاني وقد استخدمت بعد ان تم تضبيط جميع المعاملات الخاصة بها وتم استخدامها لقياس تراكيز كل من الزئبق والكوبالت والكادميوم حيث تم قياس تراكيز هذه العناصر بعد ترسيبها باستخدام كبريتيد الهيدروجين لزيادة تركيزها.تم تعيين محتوى الزئبق لمركبات كيميائية قياسية مختارة ولنماذج ماء بيئية مختلفة وكانت ظروف القياس 0,2 - 0,7 MeV منطقة الطاقة و15 دقيقة زمن القياس وكاشف نوع 3x3 NaI(Tl) . وكانت حدود الكشف 10 جزء بالمليون.تم تعيين محتوى الكادميوم لمركبات كيميائية قياسية مختارة ولنماذج ماء بيئية مختلفة وكانت ظروف القياس 0,35 - 0,8 MeV منطقة الطاقة و10 دقيقة زمن القياس وكاشف نوع 3x3 NaI(Tl) وكانت حدود الكشف 2 جزء بالمليون.تم تعيين محتوى الكادميوم لمركبات كيميائية قياسية مختارة ولنماذج ماء قياسية مختلفة وكانت ظروف القياس 0,1 - 0,3 MeV منطقة الطاقة و10 دقيقة زمن القياس وكاشف نوع 3x3 NaI(Tl) . وكانت حدود الكشف 100 جزء بالمليون. | Two neutron activation analysis systems were designed and studied. Americium - beryllium (Am - Be) was employed as a neutron source in both systems. Two different types of neutron sources (which differ in neutron flux) were used. One of them was used paraffin moderator which was theoretically simulated using Monte Carlo method by GEANT4 package program of objective oriented programming. Theoretical calculation results of neutron flux to the paraffin was compared with virtual water irradiators and these result showed the neutron flux distribution along the irradiator axes of water irradiator greater then paraffin irradiator. The thermal (under Cd) and fast (over Cd) neutron flux were calculated along the irradiation axis and compared to the experimental measurement. This comparison showed a good degree of agreement. This system (paraffin irradiator) was used to measure the copper content in some chemical compound and standard solutions after pre - concentrated by sulfide.Another system for prompt neutron activation analysis was optimized and used to measure the concentrations of mercury, cobalt and cadmium after their precipitation with H2S to concentrate them.The mercury content of various selected chemical compounds and environmental water sample after preconcentrated were determined. The optimization parameters of the measuring system were 0.2 - 0.7 MeV energy region, 15 min measuring time, and 3x3 NaI(Tl) detectors. The detection limit was 10 ppm. The cadmium content of various selected chemical compounds and environmental water sample after preconcentrated were determined. The optimization parameters of the measuring system were 0.35 - 0.8 MeV energy region, 10 min measuring time, and (3x3) NaI(Tl) detectors. The detection limit was 2 ppm.The cobalt content of various selected chemical compounds and standard solution after preconcentrated were determined. The optimization parameters of the measuring system were 0.35 - 0.8 MeV energy region, 10 min measuring time, and (3x3) NaI (Tl) detectors. The detection limit was 100 ppm.

تحضير ودراسة خواص مركبات بلورية سائلة كاطوار ثابـتـة في كروماتوغرافيا الغاز == Preparation and Characterization Of Liquid Crystalline Compounds as Stationary Phases in Gas Chromatography

Author name: مارتن جورج شليمون

General topic: Chemistry

Specific topic: Chemistry

Degree: Doctorate

University: Al-Nahrain University - College Of Science - Chemistry Department

Language: English

University location: Baghdad

First pages:

Abstract: تتضمن الاطروحة تحضير المركبات البلورية السائلة 4،4/ - بس - (4 - بروبوكسي بنزيليدين امينو)باي فنيل (2b) ، و2،5 - بس - [4 - (4/ بروبوكسي بنزيليدين امينو)فنيل] 1،3،4 اوكسادايازول (1f). تم تشخيص المركبات المحضرة، نوعيا باستخدام الطرائق الطيفية والمتمثلة بطيف الاشعة تحت الحمراء FTIR ، طيف الرنين النووي المغناطيسي1HNMR ، وباستخدام تحليل العناصر لكل من الكاربون، الهيدروجين والنيتروجين. كذلك تم دراسة الخواص البلورية السائلة للمركبات المحضرة باستخدام مسعر المسح التفاضلي ومجهر الضوء المستقطب المزود بمنصة تسخين، ولقد لوحظ ان هذه المركبات لها مدى ميزومورفي واسع مما يعطيها اهمية في استخدامها كاطوار ثابته في كروماتوغرافيا الغاز.لقد تم استخدم المركبين 2b و1f كاطوار ثابته بتحميلها على الساند الصلب كروموسورب وبنسب تحميل مختلفة (1%، 3%، 20%). تم تعبئة الاطوار الثابته في اعمده فولاذية، واستخدمت في فصل الهيدروكاربونات الاروماتية ( النفثالين، اسينافثين، اسينافثيلين، فينانثرين،انثراسين، والبايرين)، الكحولات (ميثانول، ايثانول، 2 - بروبانول، و1 - بروبانول)، وكذلك الايزومرات (اورثو، ميتا، بارا - زايلين). تم دراسة الخواص الكروماتوغرافيه للاعمدة المحضرة في درجات حرارة مختلفة، حيث استخدمت المديات (140 - 320) درجه مئوية للمركب 2b و(170 - 280) درجه مئوية للمركب 1f. تم اختبار ظروف الفصل للاعمده وذلك من خلال حساب عدد الصفائح المؤثرة في العامود ومعامل الفصل، ولقد لوحظ حدوث ظاهرة الطبخ الحراري بالنسبة للطور الثابت 2b مما سبب انخفاض في درجة الانتقال الحراري من الطور الصلب الى النيماتي، لذلك تم فصل الكحولات عند درجة الحرارة 180 درجه مئوية خلال العامود 20% 2b، وعند درجة الحرارة 240 درجه مئوية تم فصل الهيدروكاربونات الاروماتية في العامودين 1% و3% 2b. اما بالنسبة الى العامود 1f فقد تم الحصول على افضل فصل للهيدروكاربونات الاروماتية عند درجة الحرارة 220 درجه مئوية. كذلك تم حساب حجم الاحتجاز النوعي لكل من المواد المراد فصلها وفي كلا العامودين، وذلك لدراسة الخصائص الديناميكية الحرارية لهذه المواد في المركبات البلورية السائلة المحضرة كاطوار ثابته. لقد تم رسم اللوغاريتم الطبيعي لهذه الدالة مع مقلوب درجة الحرارة، وذلك لحساب الانثالبي (ΔH) والانتروبي (ΔS) لهذه المواد. تم ايضا حساب طاقة كبس الحرة (ΔG)، وقد لوحظ ان جميع القيم كانت سالبة مما يدل على ان عملية اذابة المحاليل في المركبات البلورية السائلة المستخدمة كاطوار ثابتة تحدث بصورة تلقائية.في هذه الدراسة تم حساب معامل الفعالية للمحاليل المراد فصلها وتحت ظروف التخفيف المتناهي، وكانت هذه القيم اصغر من واحد، مما يدل على ان هذه المحاليل تنحرف سلبيا عن سلوك المحاليل التي تعتبر كمحاليل مثالية. | This work involves the preparation of two liquid crystalline compounds, 4,4´ - bis - (4 - propoxybenzylidene amino)biphenyl (2b), and 2,5 - bis - [4 - (4´ - propoxybenzylideneamino)phenyl]1,3,4 - oxadiazole (1f). The prepared compounds were characterized qualitatively by using FTIR, 1HNMR, and elemental analysis (EA). The liquid crystalline properties of the synthesized compounds were verified using hot - stage polarizing microscope and differential scanning calorimetry (DSC). The prepared liquid crystal compounds have a wide mesophase range that gives useful properties to these compounds as stationary phases in Gas Chromatography (GC). Compounds (2b) and (1f) were prepared to be used as stationary phases by loading them separately on chromosorb W/HP 100 - 120 mesh size, as solid support with different loading ratios (1%, 3%, and 20%). The prepared stationary phases were packed through the stainless steal columns, and tested for separation of poly aromatic hydrocarbons PAHs (naphthalene, acenaphthene, acenaphthylene, phenanthrene, anthracene, and pyrene), alcohols (methanol, ethanol, 2 - propanol, and 1 - propanol), and positional isomers (o, m, and p - xylene).A chromatographic study of the interaction and elution characteristics of the studied analytes through the prepared columns was carried out at different column temperatures of, 140 - 320 ºC for 4,4´ - bis - (4 - propoxybenzylideneamino)biphenyl (2b) and 170 - 280 ºC for 2,5 - bis - [4 - (4´ - propoxybenzylideneamino) phenyl]1,3,4 - oxadiazole (1f). The best chromatographic conditions, efficiency, and selectivity of the columns for separation of PAHs, alcohols, and positional isomers were characterized by measuring the effective plate number of column (Neff.), resolution (Rs), and separation factor (α). It was found that the supercooling phenomenon has occurred with 2b column, which made a decrease in solid - nematic transition temperature. The best separation of alcohols was obtained at 180 ºC through 20% 2b column. PAHs could be separated through 3% and 1% 2b column at 240 ºC. The best chromatographic performance for separation of PAHs using 1f column was achieved at 220 ºC. This was related to the fact that the higher order of this liquid crystal occurred at these temperatures, which made the analytes interact more with the stationary phase. Specific retention volumes (Vg°) were calculated to study the thermodynamic behaviors of the analytes (solutes) on the liquid crystal stationary phases LCSPs (solution). From the plots of ln Vg° (mL.g - 1) versus 1/T (K - 1), the enthalpy (ΔH) and entropy (ΔS) of the solutions were measured. Gibbs free energy (ΔG) of the separated analytes at different temperatures was calculated. These values showed that the dissolution of the analytes on LCSPs were spontaneous. The study also included measurements of the activity coefficients at infinite dilution (γ∞). These values were < 1, which indicates a negative deviation of the solutions from ideality.

تحضير وتشخيص بعض المركبات الحلقية غير متجانسة مشتقة من بعض الامينات غير المتجانسة وتقييم الفعالية البايولوجية لبعض هذه المركبات == Synthesis and Characterization of New Heterocyclic Compounds Derived from Some Heterocyclic Amines and Evaluating of Biological Activity of Some Compounds

Author name: احمد ثامر سالم

Supervisor name: ابتسام خليفة جاسم | سوسن حارث شوكت

General topic: Chemistry

Specific topic: Chemistry

Degree: Doctorate

University: Al-Nahrain University - College Of Science - Chemistry Department

Language: English

University location: Baghdad

First pages:

Abstract: تحضير مركبات الثايوروليدينون, اميديزوليدينون واوكسازبين دايون من تفاعل قواعد شف مع كل من حامض الثايو خليك , الكلايسين وحامض الماليك اللامائي على التوالي2 - تحضير 1 - فنيل - 3 - هتر - 2 - يل يوريا وتايويوريا من تفاعل الهترو امين مع فنيل ايزوسيانات وفنيل ايزو ثايو سيانات على التوالي3 - تحضير1,3 - اوكسازوليدين - 4 - ون (7) و3 - فنيل - 2,3 - داي هيدرو ثايازول - 2 - يل هترو امين(8) و1,3 - اوكسازوليدين - 4 - اون من تفاعل مشتقات اليوريا والثايو يوريا (5.6) مع اثل كلورواسيتات وبارا فنيل يناسيل برومايد على التوالي.4 - تحضير 2 - كلورو هترو - 2 - يل اسيت امايد(10) من تفاعل الامين مع كلورو اسيتايل كلورايد.5 - تحضير اوكسازول - 2,5 - ثنائي الامين (11) ثايازول - 2,5 - ثنائي الامين (12) وثايوسمسكاربازايد (13) واست ازايد من(14) من تفاعل المركب (10) مع اليوريا والثايويوريا والثايوسمسكاربازايد والصوديوم ازايد على التوالي .6 - تحضير كارباما داثايونات (15) هترو - 2 - امينو استيلين (16) ومشتقات الفورم امايد (17) من تفاعل الامين مع كل من CS2 وبوبارجيل برومايد وحامض الفورميك على التوالي.7 - تحضير هيدرازينو فورم امايد من تفعل المركب (17 ) مع الفيل هيدرازين8 - تحضير ثنائي الثايولين من تفاعل الكارباماثايونات مع البارا فنيل فيناسيل برومايد.9 - تم تشخيص هذه المركبات بواسطة اطياف الاشعة تحت الحمراء والنين النووي المغناطيسي10 - تم تقييم الفعالية البايولوجية لبعض هذه المركبات المحضرة | 1 - preparation of thiazolidene - 4 - none (2) , imidazolidine - 4 - ones (3) , and oxazepine - 4,7 - diones (4) from schiff bases (1) by reaction with 2 - mercaptoacetic acid ,glycine and malic anhydride respectively .2 - preparation of 1 - phenyl - 3 - hetero - 2 - yl urea and thiourea from reaction of hetero amines with phenylisocyanate and phenylisothiocyanate respectively .3 - preparation of 1,3 - oxazolidine - 4 - one (7) ,3 - phenyl - 2,3 - dihydrothiazol - 2 - yl hetero amines (8) and 1,3 - oxazolidine - 4 - one (9) from the reaction of urea or thiourea derivatives (5,6) with ethylchloroacetate ,p - phenylphenacyl bromide respectively.4 - Preparation of 2 - chloro N - (hetero - 2 - yl)acetamide (10) from reaction of heterocyclic amines with α - chloroacetyl chloride .5 - Preparation of oxazole - 2,5 - diamines(11) Thiazole - 2,5 - diamine (12) , thiosemicarbazide (13) ,and acetazide derivatives (14) from the reaction of compound (10) with urea ,thiourea ,thiosemicarbazide and sodium azide respectively.6 - Preparation of carbamadithionate (15) ,hetero - 2 - aminoacetylene derivatives , and formide derivatives from the reaction of hetero amines with CS2 ,propargyl bromide and formic acid respectively .7 - Preparation of hydrazinoformamide (18) from reaction of heteroformamide (17) with phenyl hydrazine .8 - Preparation of dithiolene (19) by the reaction of carbamadithionate (15) with p - phenyl phenacyl bromide .9 - All prepared compounds are elucidated by some spectroscopic methods (FTIR,H NMR ,C13 NMR).10 - The biological activity of some prepared compounds are evaluated All reactions are shown in the following schemes

Author name: رجاء حسین فیاض

Supervisor name: اسعد عبود علي | فاطمة مھدي الجابري

General topic: Chemistry

Specific topic: Chemistry

Degree: Doctorate

University: University Of Basrah - College Of Education For Pure Sciences

Language: Arabic

University location: Basrah

First pages:

Abstract: Including preparation of six new symmetrical azodyes of selfa compounds ( sulfaguanidine , sulfanilamide and sulfadiazine , A1 - A3 respectively ) and ( mercuration of sulfaguanidine , sulfadiazine and sulfanilamide , B1 - B3 respectively ) by oxidative - coupling reaction of sulfa compounds and their mercuration with oxidizing agent ( 1,2 - nephthaquinone - 4 - methoxy ) . The color of prepared azodyes were orange to orange - redish with melting points ranges ( 275 - 312 oC ). The azodyes were characterized by C H N , FT - IR , H NMR and TG analysis. The electronic spectra of azodyes were showed max. wavelength range ( 440 - 460 nm. ).The acid - base properties were studied at pH values in the range of ( 0.7 - 12 ), the electronic spectra of azodyes were scanned at wavelength range of ( 350 - 600 nm. ) . The isopestic point of each dye were fixed and the protonation and ionization constants were determined by half - height method. The effect of solvents of different polarities on the azodyes spectra was also studied . From that spectra it was found that most of solvents no effect except for polar solvent like DMF ,which showed a light red shift ( that may be for the hydrogen bonding between dye and solvent ) . From the relation of max. wavelength and dielectric parameter of each dye , it was found that linearity or slightly deviation of linearity in case of polar solvent . That means the major effect is dielectric constant of the solvent The second subpart : The ability of using all prepared azodyes as acid - base indicators ( strong acid with strong base and weak acid with strong base ). The results were compared with that obtained from the recommended method . It was found that no significant observed between the two methods by using of relative error .The last subpart : Including complex formation between two of studied azodyes ( A1 & A3 ) with Ni2+ by forming 1 : 2 ( M : L ) complexes by aid of molar ratio method.The optimum conditions were studied which including ( the effects of , time , pH , sequence of addition and interferences ). The spectra of two complexes showed a red shift from their azodyes . The obeyness of Beer's law , molar absorbtivity coefficient , sandel resistivity , relative error , relation coefficient and detection limit were all determined . The effect of foreign ions with concentrations of ( 1 - fold , 5 - fold and 10 - fold ) on the absorbance of the complexes was also studied . The overall stability constants ( β1 & β2 ) of Niazodyes complexes were determined by using corresponding solutions method which including half - height method . The complexes were also characterized by C H N and FT - IR .Part two : Including simple , easy and sensitive spectrophotometric method for the microdetermination of sulfa and mercurated salfa compounds in aqueous solution and pharmaceutical compounds .This method depends on the oxidative - coupling between the reagent hydroxyl nephthaline - 4 - sulphonic acid in strong acid medium by forming colored imine - quinone dyes in max. wavelength ran ( 480 - 510 nm.). The optimum conditions which including ( volume of reagent , volume and kind of the oxidizing agent , volume and kind of the acid , sequence of additions , time effect and temperature effect ) . The electronic spectra of the dyes were carried on in the range of ( 350 - 600 nm.).This method was applied pharmaceutical compounds ( Tablets and Creams ) that containing sulfadiazine .It was found there are no significant difference between results of this method and the composition of the sulfa drugs , that observed from calculated relative rror.By the aid of C.H.N. , FT - IR and stoichiometry ( molar ratio method ) of forming the complexes, the chemical structure of the complexes Ni2+ and A1 & A3 dyes were suggested .