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تحضير متراكبات بوليمرية جديدة من البولي بروبلين ودراسة بعض خصائصها الميكانيكية والفيزيائية == Preparation of new polymeric Composites from Polypropylene and study of Some Mechanical and Physical Properties

Author name: كرار ذياب عبد الكاظم الزيادي
Supervisor name: عامر موسى جودة
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf

تحضير وتشخيص معقدات مزيج الليكاند لبعض العناصر الانتقالية == Preparation and Characterization of Some Transition Metal Mixed Ligand Complexes

Author name: ايمان جبار جاسم
Supervisor name: عبد الله محمد علي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf

تحضير ليكاندين جديدين وتطبيقهمافي استخلاص بعض الايونات الموجبة للعناصر الانتقالية من المحاليل المائية == Synthesis two new Ligands and their application in Extraction of some transition metal cation from aqueous solutions

Author name: فاتن خالد عبود
Supervisor name: شوكت كاظم جواد
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf

دراسة طيفية لايوني الكوبلت (II) والنحاس (II) باستعمال الكاشف العضوي الجديد 4-(4?- انتي بايرايل ازو ) بايروكالول == Spectrophotometric Study of Cobalt(II) and Copper(II) Ions by Using the New Organic Reagent 4-(4?-antipyriylazo) pyrogallol

Author name: امل سعدون مجيد
Supervisor name: حسين جاسم محمد
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf

تحضير ودراسة طيفية لمعقدات بعض العناصر الانتقالية مع الليكاند الجديدة ذ2-[(3-اسيتايل فنيل)ازو]-4،5-ثنائي فنيل اميدازو

Author name: ندى علي موسى
Supervisor name: عبد الله محمد علي حبيبان
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf

تحضير وتشخيص معقدات بعض العناصر الانتقالية مع ليكاندي ثايوسيميكاربازون جديدتين == Synthesis and Characterization of Some Transition Metal Complexes with Two New Thiosemicarbazone Ligands

Author name: ميثاق سعيد محمد
Supervisor name: عبد الله محمد علي حبيبان
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: تضمن البحث تحضير ليكاندين جديدتين من قواعد شف وذلك بتكاثف الثايوسيميكابازايد مع البنزوين واحدى معوضات الاسيتوفينون التي اعطت الليكاندين الاتيين. 1. بنزوين ثايوسيميكاربازون (L1 = BnTSC).2. بارا - بروبانال اسيتوفنيدين ثايوسيميكاربازون (L2 = p - PrAPTSC). شخصت اليكاندين بالطرائق الطيفية المتاحة باستعمال الاشعة فوق البنفسجية - المرئية والاشعة تحت الحمراء وقياس درجة الانصهار وكذلك التحليل العنصري الدقيق للعناصر. لقد استعملت هاتان الليكاندان في تحضير اثنا عشر معقد كيليتي جديد لكل من ايونات الكوبلت والنيكل والنحاس والخارصين والكادميوم والزئبق الثنائية التكافؤ وقد حضرت هذه المعقدات بعد تثبيت الظروف الفضلى من تركيز مولاري ونسبة مولية وذلك من دراسة اطياف الاشعة فوق البنفســجية - المرئية لمحاليـــل مزج هذه الايونات مع محاليل الليكاندين (BnTSC) و(p - PrAPTSC) كل على حده. شخصت المعقدات الصلبة بعد عزلها طيفيا بوساطة الوسائل الطيفية المتاحة كاطياف (UV - Vis) والاشعة تحت الحمراء (IR). وقد اظهرت محاليلها في الايثانول ازاحة حمراء مقارنة مع محاليل الليكاندين. وعند مقارنة اطياف الـ (IR) لهذه المعقدات مع اطياف الليكاندين الحرة فقد لوحظ تغيرات واضحة اذ اظهرت حزما جديدة لم تكن موجودة اصلا في اطياف الليكاندين في حين عانت حزم اخرى من تغيرات واضحة في الشكل والشدة والموقع وقد يعود السبب في ذلك الى حصول عملية التناسق بين الايونات الفلزية والليكاندين ، تبين منها ان الليكاند (BnTSC) سلكت كليكاند ثلاثية المخلب في حين سلكت (p - PrAPTSC) كليكاند ثنائية المخلب. وبينت نتائج التحليل الدقيق للعناصر (C.H.N) وحساب النسبة المئوية للايونات الفلزية في معقداتها توافقا كبيرا بين النسب المحسوبة نظريا وتلك النتائج المستحصلة عمليا. مما اعطى دعما للصيغ الجزيئية المقترحة. وقد تم استغلال نتائج قياسات (UV - Vis) لحساب النسبة المولية في تعيين ثوابت التكوين (الاستقرار) لهذه المعقدات. في حين استعملت التقنية المذكورة نفسها لمعرفة مدى استقرار المعقدات في محاليلها وبمرور الزمن. وبينت دراسة التوصيلية الكهربائية المولارية لمحاليل المعقدات المحضرة في هذا البحث في مذيبي ثنائي مثيل اوكسيد الكبريت وثنائي مثيل فوماميد وعند التركيز (1×10 - 3) مولاري وفي درجة حرارة المختبر بانعدام الصفة الايونية لهذه المحاليل. اما قياسات الحساسية المغناطيسية للمعقدات فقد بينت ان معقدات الكوبلت (II) والنحاس (II) ولكلا الليكاندين مضافا لمعقد النيكل (II) لليكاند (BnTSC) فانها تمتلك صفات بارامغناطيسية في حين اتصفت بقية المعقدات الكيليتية موضوع الدراسة بالدايامغناطيسية. من كل ما تقدم من نتائج مستحصلة التي تم التوصل اليها فقد تم اقتراح الاشكال الفراغية للمعقدات. | The research includes preparation of two new Schiff bases ligands drived from condensation reaction of thiosemicarbazide with benzoin and substituted acetophenone to give the following ligands : 1. Benzoin thiosemicarbazone (BnTSC = L1). 2. p - propanal acetopheneden thiosemicarbazone (p - PrAPTSC = L2). The identity of these ligands have been characterized by spectral methods (UV - Vis, IR) and another physical properties (m.p.) and elemental analysis. Twelve chelate complexes of two ligands with Co(II), Ni(II), Cu(II), Zn(II), Cd(II), and Hg(II) were prepared and characterized after fixing the optimum conditions of molar concentration and mole ratio using (UV - Vis) technique of mixed solutions of the above ions with (BnTSC) and (p - PrAPTSC ). Electronic spectra of prepared complexes in ethanolic solution showed batho chromic Shift compared with that of free ligands. Thr IR, spectra (using KBr disc) of these complexes showed some charges compared to those of free ligands. New bards were observed indicating that the ligand (BnTSC) is coordinated to the metal ion as atridentate ligand while the other ligand (p - PrAPTSC) coordinated as abidentate ligand. Micro elemental analysis for all complexes were made, the percentage of metal ions were determined using flame atomic absorption spectroscopy. Good agreement was obtained between the found and calculated values. The stability of the complexes in solution were tested by evaluation of (stability formation constants) by electronic spectrum. In addition to determined the stability of there complexes at different time. Conductivity measurement for (DMSO) and (DMF) solutions at (1×10 - 3M) has shown non ionic character for all chelate complexes. Magnetic susceptibility measurements of Co(II) and Cu(II) complexes of both ligands and Ni(II) chelate complex with (BnTSC) show that they are paramagnetic, but the rest complexes show diamagnetic properties. Finally from the observations the geometric structure of the synthesized complexes were suggested

دراسة تركيز الهبسيدين , حالات الحديد وبعض المتغيرات الكيموحياتية في مرضى متلازمة المبيض متعدد الاكياس

Author name: دعاء نعمــــة مســـلم الزامــــــلي
Supervisor name: هناء عداي علي السلطاني
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
Language: English
University location: Najaf
First pages:
Abstract: تعد متلازمة المبيض متعدد الاكياس ( PCOS ) واحدة من اشهر اضطرابات الغدد الصماء غير المتجانسة والاكثر تعقيدا للنساء في سن الانجاب. عادة ما تكون مرتبطة مع مقاومة الانسولين (IR) المرافق لفرط نسبة الانسولين في الدم كعملية تعويضية. الارتفاع المزمن لهرمون ( LH ) ومقاومة الانسولين هما الاكثر شيوعا لانحرافات الغدد الصماء والتي تضهر في متلازمة المبيض متعدد الاكياس.في الدراسة الحالية فان مستوى هرمون الهيبسيدين وحالات الحديد (Total Iron، Ferritin، TIBC، UIBC، %TS، TF) تم دراستها ومقارنتها مع العديد من العلامات الجسمانية من(العمر، الوزن، الطول، مؤشر كتلة الجسم، ونسبة الورك الى الخصر (WHR) والهرمونات (LH، FSH، TT، FT، SHBG، E2، Progesterone، Prolactin ) ومتغيرات مقاومة الانسولين التي تتضمن (مستوى السكر في حالة الصيامFBG، ونسبة الانسولين في حالة الصيامFIN ومقياس مقاومة الانسولين HOMA - IR) وبعض المتغيرات الكيموحياتية (الدهون الثلاثية، نسبة الكولسترول في الدم ، نسبة الكولسترول الجيد العالي الكثافة والكولسترول الضار الواطئ الكثافة) في مرضى متلازمة المبيض متعدد الاكياس ومجموعة الاصحاء. اضافة الى ذلك تم تقسيم مرضى (PCOS) الى عدة مجاميع طبقا للمعايير التالية : (وجود الشعرانية، وجود انتظام الحيض، وجود العقم الاولي والثانوي، وجود مقاومة الانسولين والحساسية للانسولين بالاعتماد على(HOMA - IR≥3 ) .تم اختيار ستون (60) مريضة مصابة بمرض متلازمة المبيض متعدد الاكياس (PCOS) تتراوح اعمارهم بين (15 - 42) سنة. تم تشخيص مرض (PCOS) من قبل طبيبة نسائية متخصصة في مركز الخصوبة في مستشفى الصدر التعليمي في النجف الاشرف خلال الفترة من (شهر ديسمبر 2014 الى شهر مايو 2015). كذلك اختيرت (30) امراة سليمة تتراوح اعمارهن بين (15 - 42) سنة. تم قياس المتغيرات الكيميائية (نسبة السكر في الدم في حالة الصيام، قياس تركيز TG، الكولسترول، HDL، Total Iron وTIBC باستخدام طرق طيفية. بينما تم قياس تراكيز كل من (نسبة الانسولين في حالة الصيام ، الهيبسيدين، Ferritin، LH، FSH، TT، SHBG وProgesterone، E2 وProlactin)باستخدام طريقة (ELISA). تم حساب مقاومة الانسولين (HOMA - IR) باستخدام المعادلة التالية (تركيز السكر في الدم في حالة الصيام × تركيز الانسولين في الدم في حالة الصيام / 22.5).في الدراسة الحالية وجد ان الزيادة في تركيز الانسولين في حالة الصيام (p=0.001) ، HOMA - IR (p=0.001) ، LH (p=0.001) ، ونسبة LH / FSH (p=0.001) وProgesterone (p=0.001) ، SHBG (p=0.001) ، TT وFT (p=0.001) ، E2 (p=0.001) ، Prolactin (p=0.001) ، الكولسترول ، HDL ، LDL والدهون الثلاثية (p=0.001 ) ، Total Iron ، TIBC ، Ferritin ، TS ٪ ، UIBC وTF (p=0.001) وهرمون الهيبسيدين (p=0.001) عندما قورنت مجموعة متلازمة المبيض متعدد الاكياس مع مجموعة الاصحاء. بينما اضهرت الدراسة الحالية عدم وجود تاثير لنقصان تركيز السكر في حالة الصيام ونسبة هرمون FSH (p>0.05) خلال المقارنة. وجد في الدراسة الحالية ان تغيير مستويات هرمون الهيبسيدين يعتمد بصورة رئيسية على حالات الحديد ومقاومة الانسولين . | Polycystic ovary syndrome (PCOS) is one of the most complex common and heterogeneous endocrine disorders of women in the reproductive age. It is frequently associated with insulin resistance (IR) accompanied by compensatory hyperinsulinaemia. Chronically elevated luteinizing hormone (LH) and insulin resistance are 2 of the most common endocrine aberrations seen in PCOS. In the present study, the level of serum hepcidin and Iron status(total iron, ferritin, TIBC, UIBC, TS%, TS.c) studied and compared with many descriptive (age, weight, height, BMI, hip/waist ratio (WHR) , hormonal (LH, FSH, total testosterone, Free testosterone, SHBG, E2, progesterone, prolactin and insulin resistance parameters including (FBG, fasting insulin, homeostasis model assessment of insulin resistance HOMA - IR) and some biochemical parameters (TG, Cholesterol, HDL, LDL) in PCOS and control groups. Furthermore, PCOS patients are sub grouped according to the following criteria : presence of hirsutism, presence of regularity of menstruation, presence of primary and secondary infertility, presence of insulin resistant and insulin sensitive state according to HOMA - IR≥3. Sixty (60) polycystic ovary syndrome patients (PCOS) of ages range between (15 to 42) year were recruited. PCOS was diagnosed in patient by the gynecologists of the Fertility Center in AL - Sadder Teaching Hospital in Najaf during the period from (December 2014 to may 2015), 30 healthy women of ages range between (15 to 42) year were included as a control group. Fasting blood glucose, TG, cholesterol, HDL, total Iron and TIBC concentrations were measured by spectrophotometric methods. Fasting insulin, hepcidin, ferritin, LH, FSH, total and free testosterone, sex hormone binding globulin, progesterone, E2 and prolactin levels were measured by enzyme linked immune - sorbent assay methods. Insulin resistance was estimated by( HOMA - IR) using the equation (Fasting blood glucose × fasting insulin/22.5) . In the present study Significant increase of the concentrations of fasting insulin (p=0.001) , HOMA - IR (p=0.001) , LH (p=0.001) , LH/FSH ratio (p=0.001) , progesterone (p=0.001) , SHBG (p=0.001) , total testosterone (TT) and free testosterone (FT) (p=0.001), E2 (p=0.001) , prolactin (p=0.001), cholesterol, HDL, LDL and triglycerides(p=0.001) , total Iron, TIBC, ferritin, TS%, UIBC and TF (g/L) (p=0.001) and hepcidin hormone (p=0.001) were obtained in the group of polycystic ovary syndrome patients group when compared with those of the control group. Fasting blood glucose and FSH showed no significance (p>0.05) were noticed during a comparable evaluation. In the present study Changes of Hepcidin levels are dependent directly on Iron status and insulin resistance

استخلاص نقطة الغيمة بالازدواج مع طريقة طيفية لاستخلاص وتقدير النيكل (??) والكوبلت (??) والبزموث (?I?) في نماذج مختلفة باستعمال مشتقي ازو مناسبين == Cloud point extraction coupled with spectroscopic method for separation, extraction and determination of Nickel( ?? ) , Cobalt( ?? ) and Bismuth ( I?? ) in different samples by use of suitable Azo - derivatives

Author name: احمد صادق عبد هاشم الحمادي
Supervisor name: شوكت كاظم جواد
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: Cloud point extraction methodology was used for separation, preconcentration and extraction cations for Bismuth(III) , Nickel(II) , Cobalt(II) as ion association complexes by two new laboratory prepared azo derivatives as complexing agents which are MIBSHA and AADAD as well as these new organic complexing agents studied spectrophotometricaly by UV - Vis spectroscopy and IR specrtrophotometry to confirm their structures and for the separation, preconcentration and extraction of the elements in this study which was performed as follows : 1 - Bismuth(III) Studies : At the beginning an experiment was conducted to determine the wave length of ion association complex of bismuth ion Bi(III) with new laboratory prepared complexing agent MIBSHA by UV - Vis, spectroscopy and the spectrum showed λmax=550nm. Under optimum conditions of extraction Bi(III), the study showed that pHex=9 was more stable for extraction and gave higher efficiency because at this acidic function, there exists the best coordination bounding between Bi(III) and MIBSHA in presence of 40 μg of Bi(III) as optimum concentration giving favorites thermodynamic equilibrium for complex formation and this method of extraction depends on using Non - ionic surfactant 1% Tritonx - 100. And experimental study showed that 0.5ml of this surfactant suitable for forming Cloud point layer (CPL) with higher density and smaller volume to give the best extraction efficiency for Bi(III) with high absorbance and distribution ratio (D). The extraction efficiency also increased with increasing MIBSHA concentration as linear relation because any increasing in MIBSHA concentration is mean increasing in ion pair complex concentration and suitability so increasing in the thermodynamic equilibrium partition to the CPL. And this reflects the sensitivity of new complexing agent MIBSHA in coordination binding and ion pair complex formation in addition to extraction CPE methodology which depends on heating. The experimental study shows that the optimum temperature of heating was (90°C) that gives higher extraction efficiency because it allow to reached the best thermodynamic equilibrium in Cloud point layer formation with good dehydration, as well thermodynamic data was ΔHex=0.145KJ mol - 1, ΔGex= - 73.786KJmol - 1and ΔSex=203.669Jmol - 1K - 1 whereas the low value of enthalpy for Demonstrate extraction to approach another ion of ion pair association complex, also the extraction method is entropic region, and the experimental study about the effect heating time was 20min was the optimum heating time which gives the higher extraction efficiency with high absorbance and distribution ratio D, as this time of heating helps to reach the optimum thermodynamic equilibrium of Cloud point layer formation CPLwith higher dehydration from other hand time of heating indicate the quantity of heat which162is help to dominate on the moving of micelles inside formation cloud point layer CPL with good properties of extraction. Stoichiometric study by using four spectrophotometric methods and the study revealed that the more probable structure of ion pair complex of Bismuth ion Bi(III) extracted was [1 : 1]+ anion [Bi(MIBSHA)]2+;2No3 - experimented study about synergism effect by using Tri butyl phosphate (TBP) and methyl isobutyl ketone (MIBK) show that the extraction efficiency for bismuth ion Bi(III) increased with the presence of TBP or MIBK in aqueous solution by the effect of TBP and MIBK participation in the complex formation of Bi(III) also the experiments showed that there is one molecule of TBP or MIBK enters in the structure of ion pair complex of Bi(III) as [Bi(MIBSHA)(TBP)]2+;2NO3 - ; [Bi(MIBSHA)(MIBK)]2+;2NO3 - and TBP or MIBK enter in the complex instead of water molecule in the hydration shell of Bi(III) and increase hydrophobicity of ion pair complex and increased rate of partitioning to the CPL. As well as this study involved experiments about interferences effects as well as electrolytes effect and these experiments illustrated interferences effect to decline extraction efficiency because these ions form ion pair complex with complexing agent MIBSHA , that means a decrease in complexing agent MIBSHA concentration to form ion pair complex with Bi(III) so that electrolytes affect by increasing extraction efficiency of Bi(III) by effect of increasing Dehydration and destroyed hydration shell of bismuth ion to increase the chances of binding with MIBSHA for more stable ion pair complex. Later, this method was used coupled with suitable spectrophotometric application in the separation and determination of bismuth (III) in different samples.2 - Studies about Nickel (II)For nickel ion Ni(II) extraction from aqueous solution as ion pair complex used new laboratory prepared complexing agent AADAD , the spectrophotometric study for ion pair complex on Ni(II extracted into CPL showed maximum absorbance peak at wave length λmax=585nm and through the experimental study to limit optimum conditions and effective parameters. The study demonstrated that the optimum pHex was (9) which gives the highest extraction efficiency for nickel ion Ni(II by use complexing agent AADAD, whereas at this pHex favorable binding was given to form ion pair complex of nickel ion Ni(II with high concentration and stability as well as the method CPE for extraction Ni(II needed 0.5ml of non - ionic surfactant 1% TritonX - 100 which is affected to reach favorable thermodynamic equilibrium for aggregation of micelles in the state CMC for CPL formation with good163properties for the ion pair complex extraction of Ni(II) as well this extraction efficiency appeared with the presence of 50μg Ni(II) in aqueous solution to reach the best thermodynamic equilibrium for ion pair complex formation. Increasing AADAD concentration showed the existence of linear relation with linear increase in absorbance and distribution ratio and linear increasing in concentration stability and partitioning to CPL ion pair complex of Ni(II whereas CPE methodology depends on the temperature of heating, the experiment showed that 80°C was the optimum temperature that gives the higher extraction efficiency of Ni(II with thermodynamic data ΔHex= 0.1126KJmol - 1 , ΔGex= - 58.19KJmol - 1 and ΔSex=165.16Jmol - 1K - 1 . These values prove that the ions of ion pair complex for Ni(II) extracted into CPL approached one another with a high gegree and the method of extraction was entropic in region. The experimental study about the effect of heating time showed that 15min was the best time of heating that allows to reach a higher extraction efficiency of CPE method. Time of heating indicates the kinetic side of extraction method as heating for 15min at 80°C gave the quantity of heating that hels to reach the favorable thermodynamic equilibrium for CPL formation stoichiometry showing the more probable structure of ion pair complex extracted for Ni(II) which was [Ni(AADAD)]+;No3 - but synergism effect study showed that by using TBP and MIBK showed increasing extraction efficiency of Ni(II) with the presence of TBP or MIBK in aqueous solution because substitution water in coordination shell of Ni(II) in ion pair complex and effect to increase hydrophobicity, stability and partitioning to CPL. Also, the study revealed that adding one molecule of TBP or MIBK in the structure of ion pair complex of Ni(II) such as [Ni(AADAD)(TBP)]+;NO3 - , [Ni(AADAD)(MIBK)]+;NO3 - . So the studies tackled the effect of interferences as cations and electrolytes on extraction efficiency, later on, we used this method in the extraction and spectrophotometric determination of Nickel (II) in different samples.3 - Studies about Cobalt (II)The experimental studies concerning the separation, preconcentration and extraction of cobalt(II) as ion association complex by using the same complexing agent used with nickel (II) AADAD according to Cloud point extraction methodology. The UV - Vis spectrophotometric studies about the ion association complex extracted showed that the maximum absorbance of the complex of wave length λmax=530nm. As well as the extraction method according to CPE method showed (pH=8) was the optimum acidic function for extraction giving the highest absorbance and distribution value D because this pHex the best164coordination bonding between cobalt ion Co(II) and complexing agent AADAD so that high partitioning of stable complex to cloud point layer CPL. Moreover, the experiments showed that 0.5ml of Non - ionic surfactant, very stable for giving higher extraction efficiency because this volume of surfactant helps to reach the favorable thermodynamic equilibrium of aggregation of micelles to form CPL with high density and small volume and the micelles in case one approaches the other with the best dehydration to be in high hydrophobicity with good partitioning of complex to CPL. And in this case giving higher extraction efficiency, also, this extraction efficiency obtained when 60μg of cobalt ion Co(II was in the aqueous solution to give the best thermodynamic equilibrium to formation high stability ion pair complex extracted into CPL quantitively effect of temperature study showed that 80°C was the best temperature of extraction according to CPE method because in this temperature the best CPL was formed by aggregation and using dehydration at CMC state happen good extraction as well as thermodynamic data for extraction Co(II) was ΔHex=0.1014KJmol - 1, ΔGex= - 60.658KJmol - 1, ΔSex=171.86Jmol - 1K - 1. These data showed from the small positive value of enthalpy of extraction , the ions of ion pair complex extraction when one approach another to increase stability of this complex as well the large positive value of entropy of extraction demonstrates the dependence of extraction according to CPE and entropy. Then this procedure being entropic in region. Time of heating as the experiment study showed is 15min and was stable to give higher extraction efficiency. Because heating the solution at fixed temperature and time mean the quantity of heating help kinetically to reach thermodynamic and kinetic equilibrium for formation CPL. Then giving higher extraction efficiency. Stoichiometry study revealed that the more probable structure of ion pair complex extracted was [Co(AADAD)]+;NO3 - . Synergism study show presence TBP or MIBK in aqueous solution effect to increase extraction efficiency of Co(II) according to CPE method. Because complexing agent AADAD was not able to saturated the coordination shell of Co(II) ion in complex formation then the empty coordination position and occupy with water molecule and decline extraction efficiency , but TBP or MIBK able to coordinate instead of water in coordination shell and increase extraction efficiency, as well the study showed one molecule of TBP or MIBK able to enter in complex formed such as [Co(AADAD)(TBP)]+;NO3 - or [Co(AADAD)(MIBK)]+;NO3 - . So that the studies involved the effect of interferences as cations and electrolytes on extraction efficiency , later we used this method for the extraction and spectrophotometric determination of cobalt (II) in different samples.

تحضير ودراسة الفعالية الحيوية لبعض مشتقات السلفايد والسلفون == Synthesis , Identification and Biological Activity for (Sulfide ,Sulfone) - Compounds

Author name: رشا نعمة حسين الجعباوي
Supervisor name: نغم محمود جواد الجمالي
General topic: Chemistry
Specific topic: Organic Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: Sulfone and Sulfide are important compounds due to their uses in industrial , artificial and pharmaceutical applications . They are characterized by their effectiveness against skin diseases and fungal what make them used as biologically important substances and preparatory studies have been extended to their derivatives. The research includes two sections : Section I : : contains preparing 19 compound which are (R1 - R19) in six parts : : - Part one : - includes preparing compound (R1) from the interaction of (Thio semicarbazide) with (Diethyl Terephthalate) interacting the resulted (R1) react with (10% Sodium hydroxide ) to prepare the compound (R2), interacting the resulted compound with (chloro ethyl acetate) to prepare the compound (R3) , and finally interacting the resulted compound with acetic acid and hydrogen peroxide to prepare compound (R4). Part two : - includes preparing compound (R5) by interacting compound (Sulfobenzoic anhydride) with (2 - amino - 5 - mercapto - 1,3,4 - thiadiazole) then the resulting interaction (R5) with( chloro ethyl acetate) to prepare the compound (R6) , and interacting the result with (acetic acid) and (hydrogen peroxide) to prepare compound (R7).Part three : - : includes preparing compounds (R8, R9, R10) by interacting (phenylene diamine) with (2 - mercapto acetic acid) to produce (R8) and reactance of this compound with Formaldehyde)) to form a compound (R9) and interacting the last compound (acetic acid) and (hydrogen peroxide) to prepare compound (R10). Part four : - includes interacting (2 - amino - 5 - mercapto - 1,3,4 - thiadiazol) with a compound formaldehyde)) to prepare the compound (R11) , interacting compound R11 and interacting the result with (Sulfobenzoic anhydride to produce compound (R12). Part five : - : includes preparing compounds (R13,R14, R15, R16) by interacting compound (Formaldehyde) with (2 - mercapto benzoic acid) to form (R13) , and interacting this result with ( Thio semicarbazide)) and (sodium hydroxide 10%) for the preparation of R14)), which through its interaction with (chloro ethyl acetate) is the preparation of the compound (R15 The oxidizing the resulted compound by (acetic acid) and (hydrogen peroxide) , gives (R16). Part six : - includes preparing compound (R17) by interacting( 2 - mercapto benzoic acid)) with(3 - chloro propanoyl chloride) and interacting the finally with (Thio semicarbazide) give (R18), which we can obtain011compound (R19) by interacting with (chloro ethyl acetate).All the prepared compounds have been following up the interactions enabled chromatography thin layer (TLC) for each prepared vehicles and characterized by (IR) spectrum NMR proton (1H.NMR), and a nice nuclear magnetic resonance of carbon (13C.NMR) and (C.H.N), and then measure the degree of fusion.Section II : This section includes the study of the biological inhibitory action to some of the prepared compounds on positive bacteria for dye Gram (Staphylococcus aureuse) and another negative bacteria for dye Gram (Escherichia Coli). All the compounds showed effect against both selected bacteria in the study.The Scheme below clarifies

تحضير مركبات الكبريت غير متجانسة الحلقة ودراسة الفعالية الحيوية لبعض منها == Synthesis Sulfur Heterocyclic Compounds and Study Biological Activity for Some its

Author name: انتصار عبيد سلمان الفتلاوي
Supervisor name: نغم محمود جواد الجمالي
General topic: Chemistry
Specific topic: Organic Chemistry
Degree: Master
Language: Arabic
University location: Najaf
Key words:
  • الثايازول، الثيادايازول
  • الثايازين
  • الثايادايازين
  • الثايازبين
  • الثيادايازبين
First pages:
Abstract: The compounds of heterocyclic that have the qualities of a great biological and pharmacological importance, where we see through the growing literature in Chemistry published research in this area significantly, so we decided to prepare new derivatives of them.In this study prepared (16) a new deriva????ve of sulfur heterocyclic compounds such as Thiazole, Thiadiazole Thiazine, Thiadiazine, Thiazepine and Thiadiazepine, and three other intermediate compounds to prepare Some of these derivatives, these compounds ((Five, Six and Seven - Membered Heterocycles))The research included two Section of study : The first section : included prepara????on (19) compounds (I1 - I19), by four parts : The first part : included preparation (I1) of benzil interaction with thiosemicarbazide and then the interaction of output with nitrous acid record spontaneously from mixing hydrochloric acid with sodium nitrite, to form a diazonium salt and then reactance this salt with (Acetyl acetone) to prepare azo compound (I2), and Then reactance output with thiourea, thiosemicarbazide, Thioacetamide and cysteine respectively for the preparation of compounds (I3 - I6).The second part : included reactance (diethyl terephthalate) with thiosemicarbazide, cysteine to prepare the compound (I7) and compound (I9), respectively, and then reactance outputs with Sulfobenzoic anhydride, thiosemicarbazide respectively to produce the compound (I8) and compound (I10), respectively. The third part : included reactance (1,3 - diphenylpropane - 1,3 - dione) with thiosemicarbazide to give the compound (I11) and then output reactance with benzaldehyde to give the compound (I12) and then output with reactance Sulfobenzoic anhydride to give the compound (I13). The fourth part : includes reactance (p - amino acetophenon)with nitrous acid record spontaneously from mixing hydrochloric acid with sodium nitrite, to form a salt of diazonium and then reactance this salt with diethyl mal Acetyl acetone to give compound (I14) and compound (I17), respectively, and then reactance thiosemicarbazide, benzaldehyde respectively, to give the compound (I15) and compound (I18), respectively, and then outputs reactance with Sulfobenzoic anhydride, thiourea to give compound (I16) and compound (I19), respectively. All interactions followed up by thin layer chromatography (TLC) for each prepared compounds and diagnosed by spectrum infrared (FT.IR) spectrum, proton nuclear magnetic resonance (1H.NMR), nuclear magnetic resonance of carbon (13C.NMR) and Elemental Analysis(C.H.N), and then measure the melting point. The second section : This section of the research included the study of the inhibitory action of the some of biological compounds against the gram - positive bacteria (Staphylococcus aureuse) and gram - negative bacteria (Escherichia coli) and all showed the effectiveness of the compounds against selected bacteria in the study type.

التشخيص الكيميائي والفولتامتري للبولي بيوتيلين سكسنيت الملدن بواسطة ايبوكسي (زيت النخيل)

Author name: حسن رحيم حمود الدحيدحاوي
Supervisor name: عماد عباس جعفر | هناء عداي علي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Najaf
First pages:
Abstract: في هذه الدراسة ، تم استخدم ايبوكسيي زيت النخيل EPO كملدن للبولي بوتيلين سكسينيت باستخدام الكلوروفورم كمذيب ، تم خلط ستة اوزان من PSPE وقد استخدم جهاز FTIR الطيفي لتحديد المجاميع الفعالة . كما وتم قياس الاستقرارية الحرارية والتحلل البيولوجي ، والخصائص المورفولوجية للخليط بواسطة جهاز التحليل الحراري الوزني TGA ، المجهر الالكتروني الماسح SEM وتقنية FTIR ، حيث اظهرت النتائج بان هناك بعض التاثر بين المركبين بوجود الاواصر الهيدروجينية التي تربط بين نهايات المجاميع الفعالة للبوليمر OH وبين حلقة الايبوكسي . مزيج الـ PSPE اظهر استقرار حراري عالي وتحسن في الخواص البيولوجية مقارنة مع الـ PBS النقي . كما اظهرت النتائج المورفولوجية للخليط ان EPO كان ذو قابلية امتزاجية جيدة مع PBS. تم تعديل قطب الكربون الزجاجي GCE مع طبقه رقيقة من (PSEP ) باستخدام طريقة محلول التبخر لانتاج القطب الجديد المعدل . PSEP/GC تم ايضا دراسة عمليات الاكسدة والاختزال لسداسي سيانيد الحديدات (II) باستخدام الـCyclic Voltammetry . وقد تبين ان ذروة الفصل ΔEpa - c ) ) بين قمم الاكسدة لايون فروسيانيد في محلول مائي هو 120 ملي فولت ، ونسبة التيار لقمم الاكسدة، IPA / IPC، كانت 1.6 لـ PSEP / GCE، مؤشرا انعكاسية وقابلية توصيلية جيدة للقطب المعدل. وبالتالي، فانه يمكن استخدامها لتحليل الجهد الكهروكيميائي . الخواص الفيزيائية للقطب المعدل PSEP / GCE تمثلت بالصلابة الجيدة، التصاق العالي على الاسطح المعدنية للقطب الالكتروليت الجامع ، بالاضافة الى الذوبانية والاستقرارية الجيدة للـPSEP على .GCE ايضا، الحساسية في ظل ظروف الـ cyclic voltammetry تعتمد بشكل كبير على تراكيز مختلفة من فروسيانيد ، الالكتروليت المستخدم ومعدل المسح . وقد لوحظ خلال معدلات مسح مختلفة بان قمم الاكسدة والاختزال للحديد / (III) الحديد (II) تمت بعملية معكوسة. | In this study, epoxidized palm oil (EPO) was utilized as a blended for poly butylene succinate (PBS) using chloroform as a solvent by solution casting process at six weight of PSEP. Fourier - transform infrared (FTIR) spectroscopy was used to identify the functional groups of PBS and PSEP blends. Thermal stability, biodegradable, and morphological properties of the blends were investigated by thermo gravimetric analyzer (TGA), and scanning electron microscope (SEM) technique. The FTIR spectra indicate that there are some molecular interactions by intra molecular hydrogen bond between PBS and EPO. All sets of PSEP blends show high thermal stability and significant improvement of biodegradable properties compared to pure PBS. Morphological results of PSEP blends show that EPO was good miscible with PBS. Aglassy carbon electrode (GCE) was modified with a poly butylene succinate - epoxidized palm oil (PSEP) film using a solution evaporation method to produce a new modified electrode PSEP/GCE. The redox process of K4[Fe(CN)6] during cyclic voltammetry was studied using the PSEP/GCE. It was found that the peak separation (∆Epa - c) between the redox peaks of ferrous cyanide ion in an aqueous solution is 120 mV and the current ratio of redox peaks, (Ipa/Ipc), is 1.6 for the PSEP /GCE, indicating good reversibility with good conductivity of the modified electrode. Hence, it can be used for voltammetric analysis. The physical properties of the modified electrode PSEP/GCE include good hardness, high adhesion to the metal surfaces of electrode collectors, solubility and good stability of the PSEP on GCE. Also, the sensitivity under conditions of cyclic voltammetry is significantly dependent on different concentrations of ferrous cyanide , the electrolyte used and the scan rate. At different scan rates, oxidation - reduction peaks of Fe(III)/Fe(II) were observed in a reversible process

تحضير وتشخيص ليكاندات قواعد شيف مشتقة من الترفثالديهايد ودراسة معقداتها مع بعض العناصر الفلزية == Synthesis And Identification of Schiff Bases Ligands Derived From Terephthaldehyde And Studying Its Complexes With Some Metal Elements

Author name: علي محمود علي
Supervisor name: محمد حامد سعيد | حسن ثامر غانم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: This thesis studies the synthesis of three new Schiff base ligand (L1 , L2 ,L3 ) derived from terephthaldehyde, the first ligand (L1) is produced by the reaction of terephthaldehyde with ortho - phenlenediamineat ( 1 : 2) molar ratio.The second ligand (L2) is produced by the reaction of terephthaldehyde with ortho - phenlenediamine at ( 2 : 1) molar ratio. The third ligand (L3) is produced by the reaction of terephthaldehyde with 2 - aminobenzothiazol at (1 : 1) molar ratio .These ligands are identified by using FT - IR and Uv - Vis spectroscopies,1H - NMR, massspectrometer and elemental analysis.These ligands are mixed with some metal chloride solutions Co(II), Ni (II), Cu(II) and Zn(II) by using absolute ethenolic solutions at (2 : 1) molar ratio to formtwelve complexes . These complexes are identified byanalytical andspectroscopic techniquessuch as elemental analysis andthe determination of the metalratio within its complex, recording infrared spectra,in addition to Uv - Vis by useing solvent DMSO (1x10 - 4M), the same solvent is used with molar conductance measurements for solutions of compounds at(1 x 10 - 3M)at room temperature, in addition to measuring the magnetic sensitivity of the complexes in solid state .This study has concluded that by using all the above techniques and experiments ,all these ligands' have acted as bidentate to form pentagonal and tetragonal metal cycles .Depending on the results of the study,octahedral structures of all the prepared ligands' complexes have been suggested.The following stereochemistriesreflect the complexes which are the subject of the study

تقدير البروتينات الدهنية والاجهاد التاكسدي في مصل المصابين بمرض حب الشباب == Evaluation of Serum Lipid Profile and Malondialdehyde in Patients with Acne

Author name: رنا عبد العالي الرفيعي
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
Language: English
University location: Najaf
First pages:
Abstract: The present study was conducted to verify the relevance of lipids and lipoproteins levels and their byproduct of oxidation, malondialdehyde (MDA) in acne patients. The design of the project included one hundred acne patients (47% males and 53% females)and 40 apparently healthy individuals (control group). Total serum cholesterol (TC), high density lipoprotein cholesterol (HDL - C), triglycerides (TG), low density lipoprotein (LDL - C), very low density lipoprotein (VLDL - C) and MDA levels were measured in acne patients and the control group.The results indicated significant (P≤0.05) elevations for TC, TG, LDL - C, VLDL - C and MDA levels in acne patients with respect to those of the control group. Sex differences were obtained as rises forTC, LDL - C and MDA (P≤0.05) in males when compared with thoseof the females. The linear regression analysis exhibited significantpositive correlation for TC (r = 0.68, P≤0.05) and LDL - C (r = 0.48, P≤0.05) with ages of the control group but not in the acne patients.Smoker acne patients demonstrated significant elevations for TC, TG, VLDL - C, LDL - C and MDA (P≤0.05) in comparison with those of the control group, while nonsmokers acne patients showed significant elevations for TC and LDL - C (P≤0.05) during a comparable evaluation. Married acne patients indicated significant increases for TC, TG, VLDL - C, LDL - C and MDA (P≤0.05) when compared with those of the control group, while non married acne patients illustrated significant elevations for TG, VLDL - C, LDL - C and MDA (P≤0.05). The influence of treatment was studied, the data stated significant elevation for TG and LDL (P≤0.05), in treated acne patients when compared with those of the control group, while untreated acne patients showed significant increases for TC, TG, VLDL - C, LDL - C and MDA (P≤0.05) in comparison with those of the control group.These results suggested that oxidative stress is involved in the pathogenesis of acne. We believed that this study is the first to deal with changes of serum lipid profile and oxidative stress in acne patients.

تحضير عوامل مساعدة من بعض اكاسيد الفلزات وتطبيقاتها في الاكسدة الحرارية والضوئية == Preparationof Catalysts From Several Metals Oxides and their Application in Thermal and PhotoOxidation

Author name: فاطمة علاوي عبد السجاد
Supervisor name: موسى عمران كاظم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Najaf
First pages:

دراسة الاطياف الاهتزازية والفعالية البايولوجية لبعض القلويدات == A study of the vibrational spectra and the biological activity of some alkaloids

Author name: ايمان عبد الوهاب عبد الله الكويتي
Supervisor name: عبد الرزاق عبد الجليل العيسى | حسين عبد الكاظم عبد الحسين
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Najaf
First pages:
Abstract: The present study was conducted to extracts several alkaloids and their potency on the contraction of smooth’s Rat intestine .to achieve these aims : (Okra, Potato, Cilca ,Pomegranate, Sweet melon, Water melon, Eggplant , pumpkin , Quince , Oaks, Apple, Broad been ,Cauliflower ,Cinnamon ,spinach) were subjected to extraction by petroleum ether and ethanol.HPLC and Mayer’s test revealed significant amounts of pelletierin from punica granatum,lupanine from spinacia oleracea,sinaxalen from brassica oleracea,jasmonoyl tyrosine alkaloid from vica faba ,solanidine from solanum tuberosum and solanine from solanum melongena,in the enrolled plants.The amounts of these alkaloids were (0.22,0.015,0.043,0.036,0.041,0.031) mg/g Respectively .The interaction of alkaloids (0.1) g/L and the contraction of smooth muscle in rat was examined by IR spectroscopy. with the data exhibited stretching band of (C - N) bond in the rang of (1215 - 1020),as described in the literatures .The wave number of the stretching bands of (C - N)in alkaloids were found to be inversely proportional with the molecular weight of alkaloids .Alkaloids were found to elicit Rat intestinal strain according to the order Pelletierine>Lupanine>Sinaxalen>Jasmonoyltyrosine> Solanidine>Solanine.These results suggest the involvement of (C - N) bonds in alkaloids during the induction of smooth muscle contraction.

فصل واغناء بواسطة الاستخلاص بنقطة الغيمة والتقدير الطيفي لـ (??) Mg و(??) Zn و(??) Hg في نماذج تحليلية == Separation and Preconcentration by Cloud Point Extraction and Spectrophotometric Determination for Mg(??), Zn(??) and Hg(??) in Analytical Samples

Author name: فارس حــميد حــيدر الــحيدري
Supervisor name: شوكت كاظم جواد
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: استخدمت تقنية استخلاص نقطة الغيمةCloud point Extraction (CPE) في فصل واستخلاص واغناء كل من ايون الخارصين(II) والمغنيسيوم(II) والزئبق(II) من المحاليل المائية بالازدواج مع طرق طيفية لمطيافية(UV - Vis spectroscopy) لتقدير هذه العناصر قيد الدراسة وذلك باتباع تقنية تكوين معقد الترابط الايوني او المعقد الكيلتي لايون الخارصين(Zn2+)، مع كاشف عضوي جديد محضر مختبريا هو(AIBSNB)، واما كل من ايون المغنيسيوم(Mg2+)، وايون الزئبق(Hg2+) فقد استخلص وفق مبدا التمذوب(solvation) باستخدام(2,4 - dimythyl pentane - 3 - one) للمغنيسيوم(Mg2+)، و(Acetophenone) بالنسبة للزئبق(Hg2+).بينت الدراسة ان ايون الخارصين استخلص على هيئة معقد ترابط ايوني (Ion association complex) او معقد مخلبي(Chelate complex) بالارتباط مع الكاشف (AIBSNB) الجديد والمحضر مختبريا والذي اجريت له دراسة طيفية بمطيافية فوق البنفسجية - المرئية (UV - Vis spectroscopy) ومطيافية تحت الحمراء (IR - spectroscopy) وكذلك التحليل الدقيق للعناصر وقد اثبتت الدراسات الطيفية وتحليل العناصر صحة التركيب المقترح للكاشف العضوي الجديد(AIBSNB) كما ان الدراسة الطيفية للمعقد المستخلص للخارصين(II) مع الكاشف العضوي(AIBSNB) بمطيافية(UV - Vis spectroscopy) اثبتت ان الطول الموجي لاعظم امتصاص للمعقد كان(λmax=380nm)، وقد اوضحت الدراسات لاستخلاص الخارصين(II) ان قيمة الدالة الحامضية المثلى لعملية الترابط وتكوين المعقد المستخلص كانت(pHex=9) عند وجود(50µg) من ايون الخارصين (Zn2+) في 10mL من المحلول المائي. وقد اثبتت التجارب العملية ان استخلاص ايون الخارصين على هيئة معقد ترابط ايوني او مخلبي وفق تقنية استخلاص نقطة الغيمة (CPE)يحتاج الى تسخين عند درجة حرارة(90ºC) ولزمن مقداره(15دقيقة)،فقد اظهرت الدراسة قيم الدوال الثرموديناميكية لاستخلاص الخارصين(II) هي(Sex=+155.9400 J mol - 1K - 1∆)، (Gex= - 56.4830 kJ mol - 1∆)، (Hex= +0.1242 kJ mol - 1∆)، كما تبين ان (0.5mL) من المادة النشطة سطحيا (surfactant) (TritonX - 100 1%) كانت هي الافضل في عملية الاستخلاص حيث تكون طبقة نقطة الغيمة(CPL) ذات الكفاءة العالية للاستخلاص. كما شملت الدراسة تحديد التركيب الاكثر احتمالا للمعقد المستخلص لايون الخارصين، وذلك باتباع اربعة طرق طيفية من اجل ذلك وقد اشارت هذه الطرق الى ان المعقد المستخلص كان له التركيب [Zn(AIBSNB)]+;NO3─ او [Zn(AIBSNB)+(NO3)─] كما ان دراسة توليف المذيب(Synergism) لاستخلاص الخارصين(Zn2+) بينت ان هناك مشاركة لجزيئة واحدة من كل من(TBP) و(MIBK) في تكوين المعقد المستخلص لايون الخارصين(Zn2+) يرافقه زيادة كبيرة في كفاءة الاستخلاص. وقد تضمنت الدراسة توضيح اثر بعض المتداخلات وكذلك الاملاح الالكتروليتية وتاثيرها على كفاءة استخلاص ايون الخارصين(Zn2+)، كما استخدمت طريقة الاستخلاص هذه في اجراء عمليات فصل وتقدير الخارصين في نماذج بيئية وحياتية مختلفة.تمت عملية استخلاص وتقدير ايون المغنيسيوم(II) وايون الزئبق(II) باستخدام طريقة استخلاص نقطة الغيمة (CPE) وباستعمال المادة النشطة سطحيا (surfactant) (1% TritonX - 100) ووفق تقنية التمذوب(solvation)، وباستعمال مركب(2,4 - DMP) (2,4 - dimythyl pentane - 3 - one) ، كعامل استخلاص (Extractant) للمغنيسيوم(II)، وكذلك(Acetophenone) كعامل استخلاص للزئبق(II) وقد اشارت الدراسة الى ان الصنف المستخلص لايون المغنيسيوم(II) كان له اعلى قمة امتصاص عند(λmax=249nm)، اما الصنف المستخلص لايون الزئبق(II) كان له اعلى قمة امتصاص عند(λmax=293 nm). بينت عملية استخلاص كل من ايون المغنيسيوم(Mg2+) وايون الزئبق(Hg2+) وفق مبدا التمذوب(Solvation) تحتاج الى استخدام عامل التمليح (Salting out Effect) وقد استخدم(KNO3) كعامل تمليح وقد اعطى اعلى كفاءة استخلاص لايون المغنيسيوم(Mg2+) عند(0.5M) اما اعلى كفاءة استخلاص لايون الزئبق(Hg2+) كانت عند تركيز عامل التمليح(KNO3) بمقدار(0.08M) وبوجود(50µg) من كل من ايون المغنيسيوم(Mg2+) وايون الزئبق(Hg2+) حيث ان هذا التركيز لايون(Mg2+) و(Hg2+) يعطي افضل توازن ثرموديناميكي لتكون الصنف المستخلص لايون(Mg2+) وكذلك(Hg2+) وفق مبدا التمذوب (Solvation). كما تضمنت الدراسة استخدام انواع مختلفة من عوامل التمليح وبتراكيز مختلفة، حيث تبين ان كفاءة استخلاص المغنيسيوم(Mg2+) والزئبق(Hg2+) وفق مبدا التمذوب (Solvation) يختلف باختلاف نوع عامل التمليح واكثر من تاثره بتركيز عامل التمليح. كما ان تقنية استخلاص نقطة الغيمة(CPE) لفصل الصنف المستخلص لايون المغنيسيوم(Mg2+) وايون الزئبق(Hg2+) اوضحت انها تحتاج الى تسخين لدرجة حرارة (90ºC) لايون المغنيسيوم(Mg2+)، و(85ºC) لايون الزئبق(Hg2+) وبزمن تسخين مقداره(15دقيقة) لكلا الايونين وعند وجود(0.5mL) من المادة النشطة سطحيا(surfactant) (TritonX - 100 1%) لكلا الايونين ايضا. كما شملت الدراسة استخدام عدد من عوامل الاستخلاص المختلفة وبيان تاثيرها على كفاءة الاستخلاص لايون المغنيسيوم(Mg2+) وايون الزئبق(Hg2+) وفق مبدا التمذوب(Solvation)، مركب(Acetophenone) هو الافضل والاكفا في استخلاص ايون المغنيسيوم(Mg2+) وايون الزئبق(Hg2+) على حد سواء وقد اشارت طريقة استخلاص نقطة الغيمة (CPE) لفصل واستخلاص واغناء كل من المغنيسيوم (Mg2+) والزئبق (Hg2+) وفق مبدا التمذوب (Solvation) ان قــــــــــيم الـــــــدوال الـــــثرموديناميكية لــــــــــعملية الاســـــــــــتخلاص كانت(Sex= +173.2830 J mol - 1K - 1∆)، (Gex= ─ 63.1314 kJ mol - 1∆) (Hex= +0.2295 kJ mol - 1∆) لايون المغنيسيوم (Mg2+) اما لايون الزئبق (Hg2+) فقد كانت الــــــــــدوال الـــــــــــــــــثرموديناميكية للاستخلاص هي (Sex= +202.6789 J mol - 1 K - 1∆) ، (Gex= ─ 72.4139 kJ mol - 1∆) ، (Hex= + 0.14521 kJ mol - 1∆) وقد طبقت هذه التقنية في استخلاص وتقدير(Mg2+) والزئبق(Hg2+) في نماذج بيئية وحياتية مختلفة. | Absract By used of cloud point extraction method for sepration, extraction and preconcentration for Zn(II), Mg(II) and Hg(II) from aqueous solutions copuled with spectrophotometric UV - Vis methods to determenation . these elements in environmenteal and vital sampels, with using of laboratory prepared new organic reagent (AIBSNB) for extraction Zn2+ as complex but Mg2+ and Hg2+ extracted by CPE method according to solvation technique by (2,4 - dimethyl pentan - 3 - one) (2,4 - DMP) for Mg2+ and (Acetophenone) for Hg2+.The study show extracted Zinc ion Zn2+ as ion association complex or cheleate complex after coordinat biding with organic reagent (AIBSNB), which is new laboratory prepared and the spectroscopic stadies for this new organic reagent demonstrate the true suggestion of it is structure, as well as spectrophotometric study for complex of this organic reagent with Zinc ion Zn2+ extracted to CPL in CPE method show maximum absorbance wave length was λmax=380nm. The study of extraction Zn2+ appear pH=9 was the optimum acidic function for aqueous phase in presence 50μg Zn2+ in 10mL aqueous solution and the experiments for extraction Zn2+ as ion association complex or chelate complex according to CPE method need heating the solution to 90ºCfor 15mintes time of heating. And the thermodynamic data for extraction was (∆Sex=+155.94 J mol - 1K - 1), (∆Gex= - 56.483 kJ mol - 1), (∆Hex=+0.1242 kJ mol - 1), whereas the study show (0.5mL) of surfactant (1% TritonX - 100) was the optimum concentration of non ionic surfactant to formation cloud point layer (CPL) as second aective phase for extracted complex of Zn2+, in addition to the study ivolved determine the more probable structure of complex extracted by used foure spectrophotometric studies which was appeared the complex extracted for Zn2+ was[Zn(AIBSNB)]+;NO3 - or [Zn(AIBSNB) - (NO3 - )], so that synergism study show there is aparticipate for one molecule of TBP or MIBK in the formation of complex Zn2+ extracted with increasing in extraction efficiency for Zn2+ . from the other hard used this method for separation and determination Zn(II) in envirommental and vital samples.But extraction and determination megnesium(II) and mercury(II) by CPE methodology with using of nonionic surfactant 1% TritonX - 100, and according to solvation technique by use of (2,4 - dimethylpentan - 3 - one)(2,4 - DMP) as extractant for Mg(II) so Acetophenoe as extractant for Hg(II).The study was show the extracted species for megnesiumion Mg2+ has maximum absorbance at wave length λmax=249nm and extracted species for mercury ion Hg2+ has maximum absorbance at wave lengthλmax=293nm, as well as extraction Mg2+ and Hg2+ according to this method (solvaton) needed salting out then used KNO3 as salting out and giving higher extraction efficiency at 0.5M KNO3 for extraction Mg2+,but for extraction Hg2+ used 0.08M KNO3 to giving higher extraction efficiency in pressence 50μg Mg2+ and Hg2+ each one alone. As optimum concentration ,whereas this quantity from metal cation help to reached farorable thermodynamic equilibrium for formation extracted spesies for Mg2+and Hg2+according to solvation method. Also this study demonstrate different salting out and different concentration, and show extraction efficincy for Mg2+and Hg2+according to solvation method differ by kind of salting out more than it is concentration, as well extraction the species of Mg2+ and Hg2+ by CPE method reached high efficiency by heating at 90ºC for Mg2+ and at 85ºC for Hg2+ with heating time 15 minutes for both ion in precence (0.5mL) of 1% TritoX - 100 so that study the effect of different extractant on extraction efficiency of Mg2+ and Hg2+according to solvation method.Thermodynamicaly extraction of thes ion by solvation method show thermodynamic data was(∆Sex=+155.94 J mol - 1K - 1), (∆Gex= - 56.483 kJ mol - 1), (∆Hex=+0.1242 kJ mol - 1), for Mg but for Hg2+thermodynamic data was (∆Sex=202.6 J mol - 1K - 1), (∆Gex= - 72.4138 kJ mol - 1), (∆Hex=0.1421 kJ mol - 1), this study involved determination Mg(II) and Hg(II) in different samples according to solvation method by CPE technique.

حماية الفولاذ الكاربوني المستعمل في افران معمل اسمنت الكوفة من التاكل == Protection of Carbon Steel used in Kufa Cement Plant Kilns from Corrosion

Author name: علي كاظم هادي الشماع
Supervisor name: سعد عزيز حسن حسوة
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: يتناول موضوع الرسالة دراسة تاكل الفولاذ الكربوني(ST37 - 2)في محلول حامض الكبريتيك ذوالتركيزين(5x10 - 3M,2.5x10 - 6M)ومحلول هيدروكسيدالصوديوم(3.5x10 - 6 M) في المدى الحراري التجريبي من(303الى333)كلفن وباستعمال جهاز المجهاد الساكن (potentiostat ) وبدا مسح الجهد لمدة 20 دقيقة بعد غمر الانموذج من الفولاذ الكربوني في محلول التاكل بدءامن - 300 ملي فولت ومتابعة التفاعل لحين بلوغ الجهد +300 ملي فولت مقابل قطب الكالوميل المشبع وكان معدل تغير جهد المجهاد الساكن مع الزمن يصل الى30ملي فولت لكل دقيقة واستعمل هذا المعدل لتسجيل كثافة التيار بصورة مستمرة مع تغير الجهد.ولقد تم ايجاد كثافات تيار التاكل, جهود التاكل وكذلك خطوط ميل تافل الكاثودية والانودية من منحنيات الاستقطاب في محاليل التاكل. واظهرت النتائج العملية الى انزياح جهود التاكل الى قيم اكثر سالبيه مع ارتفاع درجة الحرارة, كما وازدادت كثافات تيار التاكل عموما مع ارتفاع درجات الحرارة مشيرة الى زيادة سرعة التاكل مع زيادة درجة الحرارة .الاجزاء المستقيمة لخطوط تافل الكاثودية والانودية انزاحت دوما بصورة متوازية لبعضها البعض.حافظت خطوط تافل على خطيتها وبقي مقدار التغير في ميلها طفيفا في كل الدرجات الحرارية التجريبية وهذا دليل على عدم حصول تغيير في ميكانيكيات التفاعلات الكاثودية والانودية مع تغير درجة الحرارة, وامكن الاستدلال من قيم ميل خطوط تافل على ان تعادل ايونات الهيدروجين على المواقع الكاثودية وذوبان الفلز من المواقع الانودية هي الخطوات السائدة والمقررة لسرع التفاعلات التي حدثت على السطوح البينية لكل من الكاثود/ محلول والانود / المحلول . واستنتجت معلومات الدينمية الحرارية لعملية التاكل من قيم جهود التاكل اذﹾ بينت النتائج عموما امكانية حدوث تفاعلات التاكل ورافق تكوين نتاجات التاكل تغيرات في كل من انثالبي وانتروبي التاكل. كما بينت المعلومات الحركية على حدوث تاثير التعويض في تفاعل التاكل، وكما اشارت قيم كل من الطاقة الحرة والانتروبي لعملية التاكل في الاوساط المختلفة الى ان تفاعل التاكل يكون تلقائيا مصحوبا بزيادة في قيم الانتروبي ضمن الظروف التجريبية .اما قيم دوال الدينمية الحرارية لعملية تثبيط التاكل وباختلاف الصبغات المستعملة في الدراسة فكانت مختلفة اعتمادا على طبيعة المثبط اذ تراوحت قيم كل من انثالبي الامتزاز وانتروبي الامتزاز بين الموجبة والسالبة اما طاقة جبس الحرة لعملية الامتزاز فكانت موجبة لجميع المثبطات.اما بالنسبة لكفاءة التثبيط فكانت كمايلي : ا - صبغة الـ (Murexide) اظهرت اعلى كفاءة تثبيط في الوسط 2.5x10 - 6 M H2SO4 اذ تجاوزت .998%عند استعمال تركيز 5 ppmوضمن المدى الحراري التجريبي333 - 303 K . ب - صبغة الـ (Sudan III) اظهرت اعلى كفاءة تثبيط 99.6% في الوسط 2.5x10 - 6 M H2SO4 عند استعمال تركيز 150 ppm وبدرجة حرارة 313 K . ت - صبغة الـ (Carmine) اظهرت اعلى كفاءة تثبيط 99.4% في الوسط 2.5x10 - 6 M H2SO4 عند استعمال تركيز 25 ppm وبدرجة حرارة 333 K . ث - صبغة الـ (Leishman) اظهرت اعلى كفاءة تثبيط في الوسط 2.5x10 - 6 M H2SO4 عند استعمال تراكيز 50,25,5 ppm وبدرجة حرارة 333 K اذ بلغت 99.5%.وبصورة عامة امكن استنتاج اعلى كفاءة تثبيط للاصباغ الاربعة في محاليل التاكل وضمن المدى الحراري التجريبي وكمايلي : محلول 10 - 3 M H2SO4) x5Murexide ˃ Leishman ˃ Sudan III ˃ Carmine (محلول 10 - 6 M H2SO4) x2.5Leishman ˃ Sudan III ˃ Carmine ˃ Murexide (محلول 10 - 6 M NaOH) x3.5Leishman ˃ Sudan III ˃ Carmine ˃Murexide (تم استعمال مجهر الالكتروني المسحي في دراسة التركيب البلوري لعينة الفولاذ الكربوني (ST37 - 2) بعد تعرضه للتاكل بغياب اية صبغة وعند وجود تركيز 50 ppm من كل صبغة من الصبغات الاربعة قيد الدراسة وبدرجة حرارة40oC وفي محلول حامض الكبريتيك ذو التركيز 2.5x10 - 6M H2SO4 كانموذج للفحص المجهري ، وتبين من الدراسة المجهرية ان التاكل الذي يصيب الفولاذ الكربوني ST37 - 2 هو من النمط الذي يصيب الحبيبات البلورية الاوستنيتية والفريتية التي يشتمل عليها الفولاذ الكربوني، فضلا عن تاكل الفواصل البلورية | The subject of this thesis concerned with the investigation of the polarization behaviour of the carbon steel (ST37 - 2) specimen in (5x10 - 3 M H2SO4 ,2.5x10 - 6 M H2SO4 and 3.5x10 - 6 M NaOH ) solutions over the temperature range(303 - 333 K).The potential scan about 20 minute after the specimen immersion in the solutions beginning at - 300mV and proceed through to +300mV verses a saturated calomel electrode .Four dyes (Carmine , Murexide , Leishman and Sudan III ) dyes were used as corrosion inhibitors at concentrations ranging from (5to150 ppm).The corrosion current densities iCorr , corrosion potentials ECorr ,the cathodic and anodic Tafel slopes have been derived from the polarization curves of the carbon steel specimen in the studied solutions with and without dyes. An attempt was made to estimate on theoretical treatments the thermodynamics functions of corrosion of carbon steel (ST37 - 2). The kinetics of corrosion and inhibition of the carbon steel specimen have also been studied by measuring the corrosion rates in presence and absence of dyes (inhibitors) at several temperatures in the experimental temperature range. In general the results of the corrosion experiments showed a shift of the corrosion potentials towards more negative values with the rise of temperatures.The corrosion current densities generally increased with the rise of temperature reflecting the increasing rate of carbon steel (ST37 - 2) specimen corrosion with increasing temperature .The linear sections of the cathodic Tafel lines shifted almost to each other ,and a similar behaviour was found for the linear sections of the anodic Tafel lines .The Tafel lines maintained their linearity and slope at all experimental temperatures suggesting no alterations in the mechanisms of the cathodic and anodic reactions with the variation of temperature .The values of the Tafel slopes suggested that the proton discharge at the cathode and the metal dissolution at the anode were the prevailing rate determining - steps of the reactions which occurred at the cathode /solution and anode / solution interfaces .The measured corrosion potentials and current densities enabled a thorough investigation of the thermodynamic and kinetic aspects of the carbon steel (ST37 - 2) corrosion in the studied solutions. Thermodynamics of carbon steel (ST37 - 2) specimen corrosion have been deduced from their corrosion potentials and the resulting data showed the generally the feasibility of the corrosion reactions and that the formation of the corrosion products was accompanied by the variation of the enthalpy values between negative and positive values and increase of the entropy values of corrosion with variation of temperature . The kinetic data showed the operation of a compensation effect in the corrosion reaction of carbon steel(ST37 - 2) . Also thermodynamics of the dyes adsorption process (inhibition process) in different temperatures were calculated ,the resulting data shows the values of enthalpy and entropy of adsorption ranged between positive and negative values while the values of Gibbs free energy of the adsorption process were positive for all dyes. As for the inhibition efficiency was found as follows : A. Murexide dye was acted as good inhibitor in 2.5 x10 - 6 M H2SO4 and showed the highest inhibition efficiency reach to 99.8% when using concentration of 5 ppm of dye and within the temperature range 333 - 303 K. B. Sudan III dye showed the highest inhibition reach to 99. 6% in 2.5 x10 - 6 M H2SO4 concentration when 150 ppm of dye used and at temperature of 313 K. C. Carmine dye showed the highest inhibition efficiency reach to 99.4%in2.5x10 - 6MH2SO4when using 25 ppm of dye and at temperature of 333 K. D. Leishman dye showed the highest inhibition efficiency in 2.5 x10 - 6MH2SO4at dye concentrations of 50,25,5 ppm and at temperature of 333 K . In general the tendencies of the four dyes for corrosion efficiency followed the orders : 5x10 - 3 M H2SO4 ) Murexide ˃ Leishman ˃ Sudan III ˃ Carmine ( 2.5x10 - 6 M H2SO4) Leishman ˃ Sudan III ˃ Carmine ˃ Murexide (Leishman ˃ Sudan III ˃ Carmine ˃Murexide ( 3.5x 10 - 6 M NaOH) Electronic scanning microscopy was used to study the Crystal structure of a carbon steel(ST37 - 2)specimen after being subjected to corrosion in the absence of dye and presence in a concentration of 50ppm of each dye and at temperature of 40oC and in a solution of sulfuric acid with a concentration of 2.5 x10 - 6 M H2SO4 as a sample for microscopic examination, the microscopic study found that corrosion of carbon steel (ST37 - 2)is of the style of the Austenitic and ferritic Crystal grains as well as crystal boundary corrosion

تقنية استخلاص نقطة الغيمة لفصل واغناء المغنيسيوم (II) والخارصين (II) والنيكل (II) على هيئة ايونات سالبة وتقديرها طيفيا في نماذج بيئية وحياتية مختلفة == Cloud Point Extraction Method For Separation And Preconcentration of Mg 2+,Zn 2+,Ni 2+as Anions And Their Spectrophotometric Determination In Environmental And Vital Samples

Author name: اباء عدنان عزوز المحنه
Supervisor name: شوكت كاظم جواد
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: قد استعملت تقنية CPEعلى مدى واسع من التطبيقات في اغناء وفصل واستخلاص العديد من المركبات البايلوجية والدوائية والمركبات العضوية والعديد من الايونات الفلزية على هيئة معقدات سالبة اوموجبة في محاليلها المائية.وتعد من التقنيات المهمة والسهلة والرخيصة والصديقة | Cloud point extraction CPE methodology is wide spread used for applications to separation or Preconcentration and extraction of many medic mental or biological compounds as well as organic compounds and several metal ions as negative or positive and neutral complexes for aqueous solutions, as well as this method considers an easy, cheap and important technique and one application of green chemistry with high sensitivity which isn’t use organic solvents. This study is an application for CPE methodology for extraction, separation and preconcentration of magnesium (II), zinc (II) and nickel (II) from aqueous solutions as anions coupled with spectrophotometric method for determination these metals in different vital and environmental samples. And the major thought of this study is to change the metal ion to anion complex in aqueous solutions, and then extracted as ion pair association complexes after combination with large suitable complexing agent and using surfactant as additional phase to extract ion pair association complexes formed and in this study surfactant TritonX - 100 was used. This study include extraction of Mg (II) as anion complex with Oxine [Mg (OX3) - ] after combination Mg2+with Oxine produced from 8 - hydroxy qunoline in basic solution NaOH, afterward formed ion pair association complex with Rhodamin - B.The first step in this study is the definition (?max ) for ion pair association complex formed and extracted spectrophotometricaly. The study show ?max was 648 nm according to mechanism below : Mg2+ + 3 OX - Mg (OX) 3 - Rhb+; Cl - + Mg (OX) 3 - [Rhb+; Mg (OX) 3 - ] + Cl Cloud point extraction CPE method is one of indirect method of extraction to submit to thermodynamic equilibria which is control extraction method.This study demonstrate (50µg/10 mL) giving best extraction with higher activity as well as this method need 0.08 M 8 - HQ for extraction, as well as 0.5 M NaOH to produce Oxine from 8 - HQ as well as need 1×10 - 4 M Rhodamine - B for favorable activity of extraction. Extraction of zinc (II) according to CPE method, by using PANN as new complexing agent prepared in this study to produce ion pair association complex in HCl media after change Zn2+ to ZnCl3 - , ZnCl4= , spectrophotometricaly show ?max = 414 nm for ion pair association complex formed and extracted. According to equilibria below : PANN + 2 HCl [2H - PANN] 2+; 2Cl - PANN + HCl HPANN+; Cl - Zn2+ +3 HCl - ZnCl3 - + 3H+ Zn2+ + 4 HCl ZnCl4= or HZnCl4 - + 3H+ or 4H+ HPANN+; Cl - + ZnCl3 - HPANN+; ZnCl3 - + Cl - HPANN+; Cl - + HZnCl4 - HPANN+; HZnCl4 - + Cl - [2H - PANN] 2+; 2Cl - +ZnCl4= [2H - PANN] 2+; ZnCl4= +2Cl - Hydrochloric acid HCl media play a major rule for change metal cation Zn2+ into anion complex ZnCl3 - or ZnCl4= , then study demonstrate 1M was optimum concentration of HCl giving higher activity of extraction Zn2+ with (20µg/10 mL). Extraction of nickel (II) according to CPE method by used DB18C6 with mechanism of extraction below : Ni2+ + 3H+Cl - NiCl3 - + 3H+ Ni2+ + 4 H+Cl - NiCl4=+ 4H+ Na+Cl - + DB18C6 [NaDB18C6] +; Cl - [NaDB18C6]+; Cl - + NiCl3 - [NaDB18C6] +; NiCl3 - + Cl - [NaDB18C6]+; Cl - + HNiCl4 - [NaDB18C6] +; HNiCl4 - + Cl - Higher activity of extraction was by use of 0.5 M HCl, 0.25 M NaCl, Ni2+ (50µg/10 mL) as well 1×10 - 4 M DB18C6. With study the effect of crown ethers and cryptand kinds. Which include thermodynamic and applications for spectrophotometric determination of these metals in different samples.

تحضير ودراسة السلوك البلوري السائل ل الفا - بيتا (4 - n - الكوكسي - 6,5,3,2 - رباعي مثيل - 4? - اوكسي - ازوبنزين) ايثان == Preparation And Study The Behavior of The Liquid Crystalline ? - ? (4 - N - Alkoxy - 2,3,5,6 - Tetra Methyl - 4 - Oxy - Azobenzene) Ethan

Author name: نور محمود عبد الحسين التميمي
Supervisor name: ساجدة هادي رضا
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: تضمنت هذة الدراسة تحضير مشتقات حلقية غير متجانسة مثل 2 - امينو - 4 - فنيل ثيازول(2 - Amino - 4 - phenyl thiazol)، والاوكسازبين(Oxazepine)، والتريازول(triazol)، والاميدازوليدين(Imidazolidine). ابتداءا من (2 - Amino thiazol) و(Acetophenon) كمركبات اساس | This Study include synthesis of some heterocyclic derivatives such as (2 - amino - 4 - phenyl thiazol) , (oxazepine) ,(tetrazole) and (Imidazolidine) ,starting from (2 - amino thiazol) and (acetophenon) This Work is divided in to three Parts : Part one : Include Foure StepsThe first step include synthesis of 2 - amino - 4 - phenyl thiazol from (acetophenon),(thiourea ),(Iodine) ,while second step repersents the formation of Azo derivatives of (2 - amino - 4 - phenyl thiazol) ,while third step includes the formation of schiff base derivatives through reaction of azo compound with (3 - hydroxybenzaldehyde) The fourth step includes the reaction of prepared shiff base with compound (? - alanine) These steps are explain in diagram (1)Diagram No.1Part two : Includes two stepsFirst step includes the formation of schiff base derivatives of (2 - amino thiazol) through reaction of (2 - amino thiazol) with several compound , while second step includes reaction of several compounds with prepared schiff base to formate five and seven ring Theses steps are explain in diagram(2) Diagram No.(2)Part Three : Includes two stepsThe first step includes reaction of (acetylaceton) and (isatine) with (2 - amino thiazol) to formate new schiff base , while second step includes reaction several compound with prepared schiff base to formate five and seven ring.These steps are explain in Digram (3) Diagram No.3The sequence of reaction steps are followed up by (TLC) technique , and by busing solvents (methanol and benzene(1 : 4)) and ethyl acetate.All compounds are identified by (FT : IR) ,and some compounds by H1 - NMR and (C.H.N.S)

تحضير الكاشفين DPIDBSA وMBDPI واستعمالهما في الدراسة التحليلية للايونات Co(II) , Ni(II) , Cu(II) بالطرق الطيفية == The Preparation And Use of The Two Reagents DPIDBSA And MBDPI In An Analytical Study of Ions Co(II) , Ni(II) , Cu(II) By Spectroscopic Methods

Author name: زينب جاسم خضير الربيعي
Supervisor name: سامي وحيد راضي الحسناوي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: تم تحضير مركبات دايمرات ازوبلورية سائلة بالصيغة الاتية : no.on n = 2 - 7و تشخيصها بالطراق الطيفية المتمثلة بطيف الاشعه تحت الحمراء وطيف الرنين النووي المغناطيسي للبروتون بالاضافة الى التحليل العنصر الدقيق وقد تبين من خلال التحليل الطيفي والتحليل العنصري | A new series of liquid crystal compound has been synthesized : no.on n=2 - 7 The identification of this new series had been done by IR and HNMR spectra in addition to C.H.N analysis. By using a hot stage polarizing microscope, it was found that the members n=2,3 show pure nematic phase and members n=4 - 7 show smectice (sc ) in addition to nematic phase. The effect of the number of carbon atoms on the side chains of the these compounds with TN - I shows odd - even effect transition temperatures was recognized. The TN - Sc show odd - even odd effect. The brodeniris groups (CH3) in terminal benzene rings decrease the transition temperature and has less effect on dimenshing the liquid crystalline properties than the monomers.

استخدام تقنية كروماتوغرافيا الغاز باستعمال اطوار سائلة ثابتة لدراسة كفاءة فصل بعض مركبات الازو المشتقة من الباراكريزول == Use Gas - Chromatography Technique By Using Stationary Liquid Phases For Study of Separation Efficiency For Some Azo Compounds Derivative From P - Cresol

Author name: وداد ابراهيم يحيى خزاعل
Supervisor name: قاسم كاظم الاسدي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: حضر كاشفين عضويين جديدين هما2 - [3 - Acyl methyl phenyl )azo] - 4,5 - diphenyl imidazol (3 - AMePADPI) 1 - [(2 - Pyridyl azo)] - 2 - naphthol (PAN) وقد استخدما في فصل واستخلاص والتقدير الطيفي لعناصر النحاس(II)، النيكل(II)والبلاديوم(II) على هيئة ايونات موج | Synthesized two organic reagent was 2 - [(3 - Acyl methyl phenyl)azo] - 4,5 diphenyl imidazole (3 - AMePADPI) and 1 - [(2 - pyridyl azo)] - 2 - naphthol (PAN), which is used for separation , extraction and spectrophotometric determination Copper(II) ,Nickel(II) and Palladium(II) as Cations according to solvent extraction method ,dependence on measurement absorbance of ion pair complex extracted at ?max as well Calculation distribution ratio (D). This Study include limitation of optimum conditions for Complex formation and extraction such as pHex. and the experimental shows optimum pH for extraction Copper(II) with (3 - AMePADP) (pHex=8) and (pHex=9) with (PAN) but for Nickel was(pHex=11) with both organic reagent as well (pHex=9) for palladium (II) with both organic reagents. The study about metal ions concentration effect on extraction methods demonstrate 40µg Cu2+ suitable concentration giving higher absorbance for ion pair complex extracted to organic phase and higher distribution ratio (D) with both organic reagent , also for Nickel(II) was 80µg Ni2+ with (3 - AMePADP) and 50µg Ni2+ with (PAN) , but for palladium(II) was 20µg Pd2+ with(3 - AMePADPI) and 15µg Pd2+ with (PAN). Kinetic energy has important role in extraction. method according to Solvent extraction , and this study show effect shaking time of two immiscible phase on qualification `of extracted and illustrate 15 min was suitable shaking time for Copper(II) and Nickel(II) with both organic reagent and 5 min for palladium(II) with both organic reagent to obtaining higher absorbance of ion pair complex extracted to organic phase and distribution ratio (D). Organic solvent effect study appear there is not any linear relation between dielectric constant (?) of organic solvents and distribution ratio (D) that’s is mean there is not any effect for polity of organic solvent on extraction method but there is an effect for organic solvent structure which is participate in the structure of ion pair complex extracted by formation ,Tight ion pair or loose ion pair as well experiment result illustrate dichloro methane organic solvent (DCM) was the best organic solvent in extraction Copper(II) ,Nickel(II) and Palladium(II) by organic reagent (3 - AMePADPI) and PAN. Study about determination more probable structure of ion pair complex extracted (stoichiometry ) by performance four spectrophotometric method for extraction Cu2+ , Ni2+ and Pd2+ by (3 - AMePADPI) and PAN under optimum conditions and all experiment show the structure of ion pair complex extracted was (1 : 1) (metal : ligad) [Cu(3 - AMePADPI)]2+SO42 - . , [Cu(PAN)]+HSO4 - .[Ni(PAN)]+Cl - . [Ni(3 - AMePADPI)]2+2Cl - . [Pd(3 - AMePADPI)]2+2Cl - . , [Pd(PAN)]+Cl - . Declination of distribution ratio (D) frequently by reason of the organic reagent not gratify the coordination shell of metal ion and in this case water molecule participate to saturate the coordination shell and increase partition the complex to aqueous phase and increase dissociation of complex and decrease distribution ratio(D) as well probable to formation ion pair complex in structure of [M(L)]n+(OH) where M=Cu2+ , Ni2+ and Pd2+ and L = (3 - AMePADPI) or PAN this complex favorite partition to aqueous phase and decrease distribution ratio. Thermodynamic study include Temperature effect on extraction efficiency the experimental results demonstrate the reaction was exothermic for Copper(II) with both organic reagent (3 - AMePADPI) and PAN but the Complextion reaction of Nickel(II) and Palladium(II) with organic reagent (3 - AMePADPI) and PAN endothermic reaction , after calculation thermodynamic data ?Hex , ?Gex , ?Sex show entropy values was high that is mean complexation reaction is entropic in region. The study about Interferences effect on extraction method of Cu2+ , Ni2+ and Pd2+ by (3 - AMePADPI) and PAN to clarify metal cations of first group in periodic table Li+ , Na+ and K+ giving enhancement in distribution ratio in arranging Li+ >Na+>K+ by reason of high affinity of these ions to water and the thickness hydration shell increase with diameter decrease , this properties these ions being to contribute to destroy hydration shell of Cu2+ , Ni2+ and Pd2+ and increase chances of association with organic reagent and increase distribution ratio (D) , but metal cations of second group in periodic table Mg2+ , Ca2+ has more charge density than metal cation of first group and has less thickness in hydration shell and the effective behavior on extraction method was less , but anions able to participate in electrostatic combination with cation complex and giving different effects by differ in molar volume , stereo structure and charge density. The study about synergism by used tributyl phosphate (TBP) and Methyl iso butyl Ketone (MBK) in the extraction the experimental results shows TBP and MIBK giving enhancement in distribution ratio (D) by participate molecular of these solvents in the structure of ion pair complex extracted install f water molecular in coordination shell of metal cation as well as the results show there is one molecular of TBP or MIBK participate in ion pair complex extraction [Cu(MIBK)(PAN)]+HSO - 4 , [Cu(MIBK)(3 - AMePADPI)]2+SO42 - [Cu(TBP)(PAN)]+HSO - 4 , [Cu(TBP)(3 - AMePADPI)]2+SO42 - [ Ni (MIBK)(PAN) ]+Cl - , [ Ni (TBP)(3 - AMePADPI)]2+ 2Cl - [ Ni (MIBK)(PAN) ]+Cl - , [ Ni (TBP)(3 - AMePADPI)]2+ 2Cl - [Pd(MIBK)(PAN)]+Cl - , [ Pd(MIBK)(3 - AMePADPI)]2+2Cl - [Pd(TBP)(PAN)]+Cl - , [ Pd(TBP)(3 - AMePADPI)]2+2Cl - The study about of effect of ethanol in aqueous solution on extraction method of metal in aqueous solution on extraction method of metal cation Cu2+ , Ni2+ and Pd2+ by (3AMePADPI) and PAN the results show foundation of ethanol in aqueous solution with metal cations giving increase in distribution ratio and this increasing continue until reached optimum concentration of ethanol after this value distribution ratio (D) decrease. This study include used organic reagent (3AMePADPI) and PAN for spectrophotometric determination of Copper(II) ,Nickel(II) and Palladium(II) in different environmental and vital samples.

تحضير وتشخيص مركبات خماسية وسباعية غير متجانسة الحلقة لمشتقات الامينو بنزوثيازول == Synthesis And Identification of Five And Seven Membered Ring Heterocyclic Compounds of Amino Benzothiazole Derivatives

Author name: علي فتاح ناصر الحسيني
Supervisor name: فائز عبد الحسين عبد الرماحي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
Abstract: تضمن الجزء الاول من البحث تحضير اربعة كواشف عضوية جديدة هي مشتقات ازو لمركب الباراكريزول وقد تم تشخيص الكواشف المحضرة من خلال اطياف الاشعة فوق البنفسجية - المرئية (UV - Vis) فضلا عن قياس اطياف الاشعة تحت الحمراء IR)) وتم اجراء قياسات نسب العناصر الدقيق ( | The first part of this study included perpetrating four new organic reagents which are derivatives of P - cresol. Its identification was done by UV - Vis spectrophotometer, IR and C. H. N. Depending on the results, we found the correspondence between the theoretical calculation and the experimental ones with a way to suggest the final structures of the prepared reagents. The purity of these reagents was tested through thin layer chromatography.The prepared reagents are : 1. 2[(4 - Methyl phenyl )azo] - 4 - Methyl phenol (MePAMP)2. 2[(4 - Chloro phenyl )azo] - 4 - Methyl phenol (CPAMP)3. 2[(4 - Methoxy phenyl )azo] - 4 - Methyl phenol (OMePAMP)4. 2[(4 - Nitro phenyl )azo] - 4 - Methyl phenol (NPAMP)The second part deals with the study of chromatographic behavior of organic prepared reagents dissolved in ethanol according to gas chromatography on stationary liquid phases as capillary columns with different polarities as zebron (FFAT) which is characterized with high polarity, silica fused (BP10) with a medium polarity and poly phenyl siloxine (OV - 5) that appears with low polarity.Gas chromatography was equipped with a flame ionization detector (FID) and the nitrogen as carrier gas with flow rate 30cm3min - 1 at different column temperatures ranged 100C increments depending on columns maximum operation temperature, column inlet temperature and detector temperature were higher than the separation column (25,50) 0C respectively.This investigation attempts to find the optimum conditions for the sequential separation were defined for the azo compounds of all capillary columns such as injection, applied pressure inlet of column, gas flow rate as well as the conditions of the efficient separation.The order of elution and resolution of compounds on various stationary liquid phases were normal chromatographic behavior which is decrease in specific retention volumes with increase of column temperature through the relationship between logarithm of specific retention volume for the studied compounds against reciprocal of absolute column temperature which is observed generally linear relation for all compounds on different liquid phases by using (Clausius - Clapeyron) , then calculate the thermodynamic parameters ?H0 , ?S0 and ?G from the slope and intercept respectively the negative values of partial molar enthalpy ?H0 of solutions indicate to highest interaction between liquid phases and separated compounds. The results show that the zebron (FFAT) consider the high negative value of ?H and the reaction was exothermic, on other hand the highest negative value of ?s means less random of solutes on some liquid phase , so it was more selective towards to prepared azo derivatives of p - cresol. Also calculated separation factor (RS),number of theoretical plate (N), equivalent highest of one theoretical plate (HETP) respectively for mixture of studied compounds on various liquid phases.The precision and accuracy of the prepared organic reagent (MePAMP) from 0.06% to 1.44% for (CPAMP) from 0.91% to 1.5%, (OMePAMP) from 0.03% to 1.42% and finally for (NPAMP) from 0.06% to 1.6%

دراسة الية تفاعلات بعض الهيدروكاربونات مع جذر الهيدروكسيل الحر بطريقة نظرية دالية الكثافة == Astudy of the Mechanism of Some Hydrocarbons Reactions with ? ?Hydroxyl Radical by Density functional Theory

Author name: نادية عزت مهدي الكرباسي
Supervisor name: عباس عبد علي دريع الصالحي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:

الاستخلاص والتقدير الطيفي لايونات (II)Pb(II)، Cd(II)، Ni في نماذج مختلفة بتقنية نقطة الغيمة == Extraction andSpectrophotometric titration of Pb 2+ , Cd 2+, Ni 2+ cations in Different Samples by Cloud point Technigue

Author name: جـيـهان رزاق مـسـلــم اللـهـيـبــي
Supervisor name: شوكت كاظم جواد
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:

تقدير وفصل الرصاص (II) والكادميوم (II) والمنغنيز (VII) في النماذج البيئية والحياتية المختلفة باستعمال كواشف عضوية == Determination and Separation Lead(II),Cadmium(II) and Manganese(VII) in Environmental and Vital Samples by Using Organic Reagents

Author name: غصون جواد عباس شبع
Supervisor name: شوكت كاظم جواد
General topic: Chemistry
Specific topic: Analytical Chemistry
Degree: Master
Language: Arabic
University location: Najaf
First pages:
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