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الفصل الكروموتوكرافي لبعض الاحماض الامينية بواسطة طريقة كروموتوكرافيا السائل العالية الاداء باستعمال طور ثابت جديد == Chromatographic Separation of Some Amino Acids by High Performance Liquid Chromatography Method Using A New Stationary Phase

Author name: علي عباس رسول
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: New stationary phase for high performance liquid chromatographyhas been prepared by the reaction of Neutral red solution with Weaklyacidic cation exchanger resin . The stability of the new attachedfunctional group on the resin was studied against different solvents suchas benzene, ethanol, acetonitrile, acetone, methanol, chloroform, andpetroleum ether as well as NaOH and HCl solutions. The new preparedresin was found stable and no depletion of the Neutral red moiety fromthe resin was noticed with the above materials .The FTIR analysis hasconfigured the attachment of Neutral red on the resin as well as thephysical appearance of the new resins.The new stationary phase has been packed into stainless steel column. The pKa value for new resins has been calculated. The pKa for Weakly acidic - Neutral red resins were 7.15. The chromatographic performance of the packed column was characterized. The number of plate numbers N, height equivalent of a theoretical plates H, capacity factors Ḱ, selectivity factors α, and peaks asymmetry, and Resolution RRsR were measured by analyzing different analytes on the new columns using different mobile phase compositions and flow rates.These parameters were measured from analysis of some amino acids such as Histidine, Phenylalanine, Tryptophan, and Tyrosine. The analysis of amino acids using Weakly acidic - Neutral red column has performed using %10 acetonitrile in buffer phosphate as mobile phase.The average value of plate numbers N was (316.59) . The plate heights H was averaged (0.085) cm , capacity factors Ḱ were ranged from (1.8 - 2.86). Separation factors α were ranged from (0.21 - 1.17), and peak asymmetry value were range from (0.99 - 1.09). Resolution RRsR were ranged from (0.93 - 3.77).IIThe analysis of amino acids using a new stationary phase has performed using buffer phosphate as mobile phase . The average value of plate numbers N was (234.79) , plate heights H was (0.107)cm , capacity factors Ḱ were ranged from (1.13 - 4.73) , separation factors α were ranged from (0.23 - 1.22) , peak asymmetry value were range from (1.10 - 1.18) and resolution were (0.93).R.S.D were ranged from(0.04 - 1)% , recovery were ranged from (93.8 - 97.12)% , The relative errors were ranged from ( - 2.88 - - 6.2) % .Calibration curves for all analyzed compound were linear from their detection limits to at least 50 ppm with correlation coefficient ranged from(0.9991 - 0.9996).The detection limits were ranged from(0.05 - 0.25) ppm at signal to noise ratio of three or more.

هرمونات الغدة الدرقية والكورتيزول والبرولاكتين ومؤشر كتلة الجسم لدى مرضى السكري من النوع الثاني == The Profile of Thyroid Hormones, Cortisol, Prolactin and Body Mass Index in Patients with Diabetes Type 2

Author name: محمد صفاء شوكت النجار
Supervisor name: سلمان علي احمد
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Diabetes is a group of disorders that produce elevated levels of blood glucose. The two main forms of diabetes are type 1and type 2. The cause of diabetes was associated with some endocrine hormones and obesity. This study was focused on diabetes type 2 and its effects on thyroid hormones (TSH, T3, T4), prolactin and cortisol and with body mass index. To achieve this aim 68 diabetic patients type 2 with ages of 35 - 70 years and 34 healthy people with ages of 35 - 70 years (control group) were enrolled. These hormones (TSH, T3, T4, PRL and Cortisol) were estimated by an enzyme immunoassay method with final fluorescent detection (MiniVidas).The results demonstrated significant increase of T4 (p<0.05), Cortisol (p<0.05) levels, and significant decrease of TSH (p<0.05) levels. A non significant increase was shown in prolactin (p>0.05) levels, and non significant decrease in T3 (p>0.05) levels.Obesity is the most important modifiable risk factor in the pathogenesis of type 2 diabetes, however, racial factors seem to be important in the relationship between body mass index and glucose in patients with diabetes type 2.The linear regression analysis revealed significant negative correlation (r= - 0.310, p<0.01) in cortisol levels with BMI, and significant positive correlation in fasting serum glucose (r=0.293, p<0.05) and TSH (r=0.275, p<0.05) levels with BMI in patients with diabetes type.The linear regression analysis revealed significant negative correlation (r= - 0.249, p<0.05) in cortisol levels with fasting serum glucose, and positive correlation in TSH (r=0.258, p<0.05) levels with fasting serum glucose in patients with diabetes type 2.The linear regression analysis revealed significant negative correlation (r= - 0.469, p<0.05) in T4 levels with Cortisol levels in patients with diabetes type 2.

عمود فصل جديد لتقنية الكروماتوكرافيا السائلة عالي الاداء (HPLC) == New column for high performance Liquid chromatography (HPLC)

Author name: احمد مرزة حمزة
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: New stationary phases for high performance liquid chromatography has been prepared by the reaction of Bromophenol blue salt solution with Amberlite CG - 400 (ClP P) resin . The stability of the new attached functional group on the resin was studied against different solvents such as benzene, ethanol, acetonitrile, acetone, methanol, chloroform, and petroleum ether as well as NaOH and HCl solutions. The new prepared resin was found stable and no depletion of the Bromophenol blue moity from the resin was noticed with the above materials .The FTIR analysis has configured the attachment of Bromophenol on the resin as well as the physical appearance of the new resins.The new stationary phase has been packed into stainless steel column.The resin capacity of newly prepared resin has calculated. The resin capacity for the Amberlite - bromophenol blue salt was found to average 5.27 meq./g which is more than the Amberlite resin, 3.95 meq./g.The chromatographic performance of the packed column was characterized. The number of plate numbers N, height equivalent of a theoretical plates H, capacity factors Ḱ, selectivity factors α, and peaks asymmetry, and Resolution RRsR were measured by analyzing different analytes on the new columns using different mobile phase compositions and flow rates.These parameters were measured from analysis of some amino acids such as Histidine, Phenylalanine, Tryptophane, and Tyrosine. The analysis of amino acids using Amberlite - Bromophenol blue column has performed using %10 acetonitrile in water as mobile phase.The average value of plate numbers N was192.085. The plate heights H was averaged 0.089 cm , capacity factors Ḱ were ranged from 1.8 - 2.42. Separation factors α were ranged from 0.86 - 1.3 , and peak asymmetry value were range from 1.02 - 1.98 . Resolution Rs were ranged from 0.92 - 4.15 . R.S.D were ranged from(0.06 - 0.10)% , recovery were ranged from (95.84 - 96.88)% , The relative errors were ranged from ( - 3.12 - - 4.64) % . Calibration curves for all analyzed compound were linear from their detection limits to at least 50 ppm with correlation coefficient ranged from 0.9989 - 0.9996. The detection limits were ranged from 0.05 - 0.25 ppm at signal to noise ratio of three or more.

علاقة الهرمونات الجنسية بصورة الدهون المصلية والاجهاد التاكسدي في عقم الرجال

Author name: ذو الفقار غانم محمد المحنه
Supervisor name: سلمان علي احمد
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
Language: English
University location: Baghdad
First pages:

دراسة نظرية لبعض معقدات المغنيز (III) الحاوي على ذرتي النيتروجين والاوكسجين == Theoretical Studies for some Manganese (III) Complexes Containing Oxygen and Nitrogen Atoms

Author name: احمد عبد الستار علي
Supervisor name: مثنى عبد الجبار شنشل | ایاد حمزة جاسم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Reactive oxygen species (ROS) are small, highly reactive, oxygen containing molecules that are naturally generated in small amounts during the body’s metabolic reactions and can react with and damage complex cellular molecules such as fats, proteins, and DNA. Superoxide dismutase (SOD) represents an essential defense system against oxygen - derived free radicals, specifically superoxide (O2• - ). Superoxide can initiate a series of free radical reactions that yields other oxygen radicals, which together are thought to actas inflammatory mediators and induce cellular damage. The presence of natural superoxide dismutase (SOD), Catalase (CAT), and Glutathione Peroxidase (GPx) is to perform as defense systems against the cells damage which caused by superoxide compounds. These various enzymes allow to founding a widely area of treatment of many diseases.In our thesis, a series of ten Schiff - bases manganese (III) complexes which is previously prepared have been designed and build as SOD and CAT mimetics. The complexes along with the known Mn - Salen [(C1 : a known drug used as standard against superoxide anion (O2 - ) (SOD - mimetic activity) and hydrogen peroxide (H2O2) (CAT - mimetic activity)], have been characterized using the Gaussian 03 program (2003). The results show the following : 1. The manganese (III) ion in these complexes is surrounded by two nitrogen atoms of the Schiff - base, and two oxygen atoms and metal ion above the basal plane toward the anion (Cl - ).2. The behavior of building complexes is different in the oxidationreduction reactions.3. Some complexes which have mixed ligands (heteroligands), show to have better activities than that of the same ligands (homoligands).4. Some complexes get high mimetic enzyme activity in one reaction (SOD - mimetic or CAT - mimetic activities), but low mimetic enzyme activity in the other reactions.5. The activities of both C2 and C7 complexes are higher than that of C1 complex in both reaction types (SOD - mimetic and CAT - mimetic activities).6. The activities of (C4, C9, C10) complexes are higher mimetic enzyme than that of C1 complex as superoxide dismutase. 7. The activities of (C3, C5, C6, C8, C11) complexes are higher mimetic enzyme than that of C1 complex as Catalase.8. The calculation of geometrical shapes of building complexes were achieved by calculate the bond frequencies and force constant, the results indicate that all the building complexes have square pyramidal shape.

تحضير بعض قواعد شف كمثبطات لانزيم اليوريز ودراسة تاثيرها على بكتيريا المتقلبات Proteus M == Preparation of some Schiff bases as Urease inhibitors and study their effect on Proteus mirabilis bacteria

Author name: احمد حسين علي التميمي
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: The current study involves preparation number of cysteine derivatives by the reaction of cysteine with different aromatic aldehydes forming the following Schiff bases : "2 - (4 - bromobenzylideneamino) - 3 - mercaptopropanoic acid, 2 - (4 - hydroxybenzylideneamino) - 3 - mercaptopropanoic acid, 2 - (4 - (dimethylamino)benzylideneamino) - 3 - mercaptopropanoic acid and 2 - (4 - chlorobenzylideneamino) - 3 - mercaptopropanoic acid".The new prepared derivatives were identified by using spectroscopy (FTIR) and measuring their melting points.The biological activities against Proteus mirabilis were estimated using well - diffusion method around the plate then the antibacterial activities were estimated.The effects of the prepared compounds on urease activity were studied. The results showed good effect in urease inhibition. All the prepared compounds showed competitive inhibition since the value Vmax was the same and Km increased.Finaly, Vmax, Ki, Km and i % values of the enzyme was calculated using line weaver Bruk equation.It is noticed from enzymatic and biological studies that Schiff bases compounds are strong inhibitors of the urease enzyme where the(2 - (4 - (dimethylamino)benzylideneamino) - - 3mercaptopropanoic acid ) inhibition force was (Ki=0.0043 M) which is the highest inhibition force comparing with the other prepared compounds.The percentage of inhibition (%i) was equal to (96.77%).

مقارنة التشخيص والتحاليل الحياتية لانزيم الفوسفاتيز القاعدي في الاكياس المائية المتكونة من جنس Echinococcus Granulosus ومصل دم الانسان

Author name: مريم فضيل ناصر
Supervisor name: سلمان علي احمد
General topic: Chemistry
Specific topic: Analytical Biochemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: Hydatidosis, a zoonitic parasitic disease, is one of the most important economic and health problem in Iraq and many other countries in the Middle East. It is caused by Echinococcus Multilocularis and Echinococcus granulosus, the larval stage of which is localized in the liver, lungs and other visceral organs of intermediate hosts such as sheep, goats and cattle.Human are considered to be an accidental intermediate host, either by eating improperly disinfected vegetables or by close contact with dogs. The mature form lives in the ileum of candies as its definitive hosts, where it leads to an asymptomatic infection .Serology or immunodiagnostic tests are the most useful techniques for the detection of hydatid cysts in human patients.Objectives : One of the reasons why Echinococcus granulosus cysts are described as a public health problem is the lack of effective chemotherapy.Reviewing the literature bears in mind the possibility of an effectual and successful chemotherapeutic treatment in the early stages of cyst development, as indicated by many reported studies. Thus, the major problem in the management of Hydatid disease seems to be related to the lack of an efficient routine diagnostic test capable of identifying asymptomatic patients at early stages of the disease. Consequently, the need for a consistent diagnostic test, applicable for mass screening in hyperendemic regions, has become mandatory.Much attention has been focused on the multilocularis species which represent the major type affecting western countries. These cumulative efforts have recently evolved a commercially available and reliable immunodiagnostic test for the specific diagnosis of Alveolar ehinococcus. Unfortunately, the test fails to identify most of the patients suffering from cystic echinococcosis, caused by the closely related echinococcus granulosus.Hence, this will detract from the valuablity of the test in districts, where echinococcus granulosus is well known as the main endemic type, including Iraq, and necessitating the requirement for further studies with regard to echinococcus granulosus.The present study was conducted to estimate the kinetic parameters and biochemical characteristics of alkaline phosphatase in fertile and sterile cyst membranes from patients with hepatic cystic echinococcosis. The raised alkaline phosphatase serums of patients suffering cholestasis caused by gallstones were used as a representative alternate to Human liver - type alkaline phosphatase. Comparisons were aimed to reveal whether these two cyst membranes enzymes are different from each other and from the Human liver - type alkaline phosphatase.Subject and methods : In this study two samples were used, the cyst and human serum.Hydatid cysts were obtained from six hepatic cystic echinococcosis patients attending The Red Crescent Private Hospital, Baghdad, for surgical intervention from January 2007 through August 2008. Based on ultrasonographic examination, only two were identified as fertile, three were sterile and one patient with calcified cyst.Fasting venous blood samples were acquired from patients with professional diagnosis of gallstones, attending the above hospital for surgical treatment. Serum was separated, 5&#39; - nucleotidase activity was measured to confirm that the raised alkaline phosphatase activity is mainly due to liver isoenzymeCollected serum samples were pooled and divided into aliquots, stored at - 2 C until further analysis.The present study was measurement of alkaline phosphatase activity in serum and cyst homogenate according to the method of kind and king.Kinetic studies will involve the affinity of these enzymes to their substrate, as well as the effect of other factors including hydrogen ion concentration (pH) and temperature. Heat inactivation and the effect of specific inhibitor, namely L - phenylalanine, are also to be examined on the activity of the three alkaline phosphatase enzymes.Results : 1.Different alkaline phosphatase activity were observed in fertile cysts while there was no alkaline phosphatase activity in hydatid cyst homogenated from sterile cysts and still not able to be detected even when larger volume of the hydatid cyst homogenated sample were used for the estimation and can be explained that by the presence or the absence of fresh protoscoleces in fertile or sterile hydatid cyst, respectively. Because of this statement it can be differentiate between the sterile & fertile cyst.By the results of the biochemical characterization of alkaline phosphatase, there were different Km values, optimum pH and optimum temperature for each hydatid cyst homogenated & human - liver type.The heat - sensitive specifically showed that the echinococcus granulosus alkaline phosphatase was more heat resistance than echinococcus multilocularis & liver - type enzyme.The respond of different human alkaline phosphatse isoenzymes to L - phenylalanine have been shown to varied from low sensitive (liver and bone) to highly sensitive (placental and intestinal). Thus, the wide range of IC50 observed herein, can be ascribed to the presence of isoenzymes other than liver type in the serum samples enrolled in this study. No inhibitory effect was observed on alkaline phosphatase from hydatid cyst homogenate.Conclusion : Considering present findings along with the following discussion, the following conclusions might be derived : Echinococcus granulosus Alkaline Phosphatase serve as a marker of cyst viability.The different characteristic of alkaline phosphatase from hydatid cyst membrane revealed that echinococcus granulosus Alkaline phosphatase is distinct from human isoenzymes more specifically from liver alkaline phosphatase isoenzyme.

دراسة امتزاز وامتصاص بعض الملوثات العضوية على ثنائي اوكسيد التتانيوم == Sorption study of Some Organic Pollutants on Titanium Dioxide

Author name: قيس محمد عبد الحسين
Supervisor name: خلود عبد صالح السعدي
General topic: Chemistry
Specific topic: Physical Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: The subject of this thesis involves studying the possibility removed of four organic compound by TiO2. These organic compounds (considered as pollutants) which are; Birlliant blue (dye), polyvinyl alcohol (PVA), Linear alkyl benzene sulfonate (LAS) and Lambdacyholothrin as (pesticides). The thermal and photo - stability were studied and the results showed that all pollutants are stable in temperature range about (288 - 318) K, and stable against UV - linght in the wave length range (290 - 320) nm.Titanium dioxide successed in removing; 95 - 54% of dye, 6.2% of PVA, 13.19% of LAS and failed in removeing pesticides.UV - Vis absorption spectrophotometric technique was used to follow the pollutants concentration before and after adsorption process and after different periods of time, since the sorption isotherms were obtained by obeying Langmiur and Freundlich adsorption isotherms, with R2 (1 - 0.9993) for dye, R2 (0.9992 - 0.9574) for PVA, R2 (0.9503 - 0.9813) for LAS.The dye adsorption isotherms take S - shapes which related to a strong interaction between dye and TiO2 with thermodynamic values DH = +(5.962 - 26.57)J, DG = - (966 - 999)J, DS = +(3.45 - 9.1906)J.The thermodynamic parameters were studied by using the sorption process of the three pollutants on TiO2 of different temperatures ranging (293 - 318)K, and from the sorption isotherms the values of DH, DG, and DS for PVA DH = - (133.4 - 212.83)J, DG = +(78 - 157.4)J, DS = - (500)J, LAS DH = +(53.14 - 66.14)J, DG = - (1.21 - 1.38)kJ, DS = +(4 - 14)J. The sorption process of dye and LAS a positive DH values, negative DG values and positive DS values, which indicates the spontaneous absorption process, which for the negative DH values, positive DG values and negative DS values are due to the non spontaneous adsorption process for PVA. The kinetic study of pollutants sorption on TiO2 was studied depending on three kinetic equations : 1 - Lagergren equation : it was used to obtain the order of the sorption process, and the results showed a good obey with R2 = (0.9477 - 0.9995) for dye, R2 = (0.956 - 0.9942) for PVA, R2=(0.9948) for LAS, to this equation, which indicates that the sorption processfollowed a pseudo - 1st order kinetics, and from the linear Lagergren equation for the pollutants sorption the rate constants of sorption were calculated at different temperatures, and the activation energy for the sorption process was also calculated which reached 39.011 kJ.mol - 1 for sorption of dye.2 - Morris - Weber model : was employed and it gave a good match with the straight linear equation with R2 = (0.98 - 0.994) for dye, R2=(0.9892) for PVA, R2 = (0.9989) for LAS. This relation indicates that the diffusion process was so obvious, and it involvesthe transport of pollutant from the bulk solution into the TiO2 surface, which is considered the rate - limiting step. 3 - Reichenberg model : was employed and it gave a good linear relationship between Bt and time with acceptable correlation coefficient R2 = (0.9891) for dye, R2 = (0.9306) for PVA, R2 = (0.9776) for LAS.This relation indicates that the rate limiting mechanism is the absorption and the sorption process involving three steps : absorption, adsorption and desorption).

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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