علوم - دكتوراة
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Item REMOVAL OF REFINED PETROLIUM PRODUCTS POLLUTING DAMA DAMA RED SEA PORT, USING NATURAL ZEOLITE(2017) OBAID BASHEIR ISMAIL AHMEDABSTRACT This study was done Dama Dama Sea Port for exporting refined petroleum products. It lies 24 Kilometers South of Port (polluted )and Kaleneib area 25 Kilometers South of Port Sudan (unpolluted) Test Dama Dama Kaleneib Water temp. during summer 29-25 oC 25-21 oC Water temp. during winter 23-19 oC 15-19 oC Air temp. during summer 38- 35 oC 36-30 oC Air temp. during winter 26- 24 oC 23 -21oC PH 8.8 -8.4 8.6-8.4 Salinity 35% -37 % 35.5 % - 36.5% B.O.D 4.78 -5.03 mg/L 1.67 -3.18 mg/L C.O.D 1.81-2.23 mg/L 0.419-0.756 mg/L D.O 2.37 -4.59 mg/L 4.45 -5.54 mg/L Oil content in sediment Nil -1.3% Nil -0.006% The treatment of the polluted samples was done in two ways:- Chemical treatment using different kinds of natural zeolite taken from different sites in the Sudan i.e. (Doka, Algalabat, Biouda desert, Nuba Mountains)and industrial zeolite made by mixing different ratios of clay, trona and feldspar of different grains size and ignited at different temperatures 1200 oC to yield different kinds of industrial zeolites. The treatment was done by passing polluted sea water through adsorption column packed with different kinds of zeolites three times to select the most efficient zeolite in adsorbing petroleum hydrocarbon pollutants . The second method of treatment was biological by making a culture of Bacteria, Fungi and Algae which is know to decompose the hydrocarbon matter that pollute marine environment but the results obtained from this kind of treatment is poor when compared to previous method (zeolite treatment ). The physical and chemical properties of the polluted water were investigated before and after the treatment with the best type of zeolite (Biouda desert zeolite) .The results showed a clear decrease in pollutants which is 75.6% and a noticeable improvement in the chemical and physical properties of the polluted sea water. The chemical composition of Biouda desert zeolite which has the highest adsorptive properties was investigated using XR-F method and was found to be (Gonnardite 66% and stellerite 34% ) having the chemical formula (Na2 Ca4 Si6O16.7H2O ) and it was found to be the best sample for removing refined petroleum pollutant from Sea water . ملخص الدراسه - اجريت هذه الدراسه باخذ عينات من ماء البحر من موقعين على ساحل البحر الاحمر:- - الموقع الاول هو ميناء دما دما لتصدير منتجات البترول المكرره وتقع على بعد 24 كيلو متر جنوب بورتسودان والمياه فى هذا الموقع ملوثه بمنتجات البترول المكرره . - الموقع الاخر هو منطقة كلانيب الواقعه على بعد 25 كيلو متر جنوب بورتسودان ومياه هذه المنطقه خالى من الملوثات البتروليه والجدول يمثل نتائج تحليل المياه في المنطقتين دمادما وكلانيب علي التوالي . 25-21 م0 29-25 م0 درجة حرارة المياه خلال الصيف م0 19- 15 م0 23 - 19 درجة حرارة المياه خلال الشتاء 36- 30 م0 38- 35 م0 درجة حرارة الهواء خلال الصيف م0 23-21 26- 24 م0 درجة حرارة الهواء خلال الشتاء 35.5 -36.5 % 35-37 % درجة الملوحه 8.6-8.4 8.8-8.4 PH ملجم/لتر 4.78-5.03 ملجم/لتر 4.78-5.03 الاكسجين الحيوى المذاب ملجم/لتر 0.419-0.756 ملجم/لتر 1.81-2.23 الاكسجين الكيميائى المذاب ملجم/لتر 4.45-5.54 ملجم/لتر 2.37-4.59 الاكسجين المذاب فى الماء صفر- 0.006% صفر-1.300% كمية المواد البتروليه فى الرواسب وتعكس النتائج السابقه الفرق فى الخصائص والاختلافات ناتجه عن تلوث مياه منطقة دما دما بالمواد البتروليه وخلو مياه منطقة كلانيب من هذه الملوثات . وتمت معالجة مياه منطقة دما دما الملوثه بطريقتين . 1- المعالجه فى الطريقه الاولى تمت بامرار المياه الملوثه خلال اعمدة الفصل المحتويه على انواع من الزيوليت الماخوذه من مناطق مختلفه بالسودان (منطقة دوكه , القلابات ,صحراء بيوضه وجبال النوبه وتمت المعا لجه بامرار المياه الملوثه خلال اعمدة الفصل المعباه بالانواع المختلفه من الزيوليت ثلاث مرات لاختيار الزيوليت ذو الكفاءه الاعلى والامثل لفصل المواد البتروليه عن الماء . وكانت النتائج المتحصل عليها تعكس بوضوح ان الزيوليت الطبيعى الما خوذ من صحراء بيوضه هو الاحسن. اما طريقة المعالجه الثانيه فهى طريقة حيويه وذلك باستزراع عينات معينه من البكتريا والفطريات والطحالب المحلله للمواد الهيدروكربونيه الملوثه للبيئه البحريه لكن هذه الطريقه كنت نتائج ازالة الملوثات بها متدنيه عند مقارنتها بالطريقه السابقه (طريقة الزيوليت ) وتمت دراسة الخواص الكيميائيه والفيزيائيه للمياه الملوثه قبل وبعد المعالجه بافضل نوع من الزيوليت (زيوليت صحراء بيوضه ) وعكست النتائج المتحصل عليها تدنيا واضحا فى درجة تلوث المياه بنسبة75.6% وتحسن واضح فى الخواص الفيزيائيه والكيميائيه لمياه البحر الملوثه بعد المعالجه بالزيولايت الزيوليت الطبيعى الما خوذ من صحراء بيوضه هو الاحسن . بعد ذلك تم تحليل عينه بيوضه ذات الخواص الامتزازيه الجيده لايجاد تركيزها الكيميائى وذلك باستخدام تقنية الاشعه السينيه وباختبار شرائح من العينه بالما يكروسكوب الالكترونى ووجد ان العينه تتكون من (قناردايت بنسبة 66% واستلرايت 34% ولها تركيب . ..(Na2CaAl4Si6O16.7H2O) كيميائى ووجد ان هذه العينه هى احسن واكفأ عينه لازالة الشوائب البتروليه الملوثه لمياه البحر .Item Synthesis of Chalcones with Mannich Side Chain(Al Neelain University, 2011) ANWAR ELBUSHRA MOHAMMED NORELJALEELNineteen new compounds (chalcone with Mannich side chain) were synthesized in this work, together with their intermediates. Aminomethylation of vanillin was achieved by reaction of formaldehyde with various amines (pyrrolidine, piperidine, moropholine, N-methylpiperazine, and N- ethylpiperazine) in dioxane to obtain 4-hydroxy-3-methoxy-5-pyrrolidinomethyl- benzaldehyde (1), 4-hydroxy-3-methoxy-5-piperidinomethylbenzaldehyde (2) 4- hydroxy-3-methoxy-5-morpholinomethylbenzaldehyde (3), 4-hydroxy-3-methoxy-5- N-methylpiperaznomethylbenzaldehyde (4), 5-N-Ethylpiperazinomethyl-4-hydroxy- 3-methoxybe-zaldehyde (5) respectively. These intermediates were reacted with 4- methoxyacetophenone to obtain chalcones with Mannich side chain : 4-Hydroxy-3,4'- dimethoxy-5-pyrrolidinomethylchalcone (6), 4-hydroxy-3,4'-dimethoxy-5- piperlidinomethylchalcone (7), 4-Hydroxy-3,4'-dimethoxy-5-morpholinomethyl chalcone(8),4-hydroxy-3,4'-dimethoxy-5-N-methylpiperazino-methylchalcone (9) , 5- N-ethylpipera-zinomethyl-4-hydroxy-3,4'-dimethoxychalcone (10) The chalcones : 4-hydroxy-4'-methoxychalcone and 4-hydroxy-4'- methoxychalcone were prepared by reacting 3-hydroxy or 4-hydroxybenzaldehyde with 4-methoxyacetophenone . The aminomethylation of chalones was done by reaction with formaldehyde and suitable amines (dimethylamine, pyrrolidine, piperidine, moropholine, N-methylpiperazine, and N-ethylpiperazine) in acetonitrile to obtain 3-hydroxy-4'-methoxy-4-dimethylaminochacone (12), 3-hydroxy-4'- iii methoxy-4-pyrrolidinomethylchalcone (13), 3-hydroxy-4'-methoxy-4-piperlidino- methylchalcone (14), 3-Hydroxy-4'-methoxy-4-morpholinomethylchalcone (15), 3- hydroxy-4'-methoxy-4-( N-methyl-piperazino methyl)chalcone(16),3-hydroxy-4'- methoxy-2,4-bis-(N-methylpiperaz-inomethyl)chalcone (17) and 4-(N- ethylpiperazinomethyl)-3-hydroxy-4'-methoxychalcone(18),4-hydroxy-4'-methoxy- 3,5-bis-dimethylaminomethylchalcone (20), 4-hydroxy-4'-methoxy-3,5-bis- pyrrolidinomethylchalcone (21), 4-hydroxy-4'-methoxy-3,5-bis-piperdinomethyl chalcone (22), 4-hydroxy-4'-methoxy-morpholinomethylchalcone(23), 4-hydroxy-4'- methoxy-3,5-bis-morpholinomethylchalcone(24), 4-hydroxy-4'-methoxy-3,5-bis-N- methylpiperazinomethylchalcone (25), 3-(N-ethylpiperazinomethyl)-4-hydroxy-4'- methoxychalcone (26) 3,5-bis-(N-ethylpiperazinomethyl)-4-hydroxy-4'-methoxy chalcone (27) The final products were purified by thin layer and column chromatography. They were identified along with their intermediates by spectroscopic methods: UV, IR, NMR spectroscopy ( 1 H, 13 C, ABT, COSY, NOESY, HSQC, HMBC) and Mass spectrometryItem Determination and Characterization of Tannin Material Extract From Three Common Acacia Species in Sudan(Al Neelain University, 2009) AYMAN AHMED AL-KHDIR ALI JACKNOONThis research is dealing with the analysis and comparative studies of tannins of three common Acacia species of Sudan. Since vegetab1e tannins are important for leather industry, A. nilotica and A. seyal samples were collected from Sunut forest in Khartoum State while A. tomentosa, samples were collected from the shmbata Forest. Bark samples From collections of the three acacia species ,were extracted with distilled water, 80% methanol and 70% acetone ;two sets of extraction were made, one by boiling, and the other by shaking the samples in the respective solvent for eight hours at room temperature. Although the amount of material extracted by these two procedures did not differ greatly , 70% acetone was a more efficient solvent than either water or 80% methanol. Qualitative analysis showed that the fruits (garad) contain tannins materials, flavinoid coumarins, and quantitative analysis showed that the fruits (pods) contain a higher percentage of tanning materials, that can be used commercially, barks contain XIII low tannin content compared with fruits. Also it was found that the unripe fruits give the highest percentage of the tannins content. Rotary system (with extraction changing in size of powder, rate of solvent to the fruits weight, and solvent temperatures), enabled access to extracts with high concentration when using crushed fruits, water at 70°C and ratio of (3:1) of water to fruits weight. Sodium fluoride and a mixture of oxalic acid and sodium sulphite showed high efficiency as antifungal reagents. With the mixture of acid - sulphite was found to be the best bleaching agent compared with sodium fluoride The amount of tannins present in the bulk samples was determined by folindenis method for total phenolic materials, followed by precipitation with hide-powder. The difference between the amount of phenolic materials present before and after addition of hide-powder represent the amount of tannins present. The extracts of the bark of A. nilotica A. seyal and A. tomentosa, contain (80.45% ,59.9% and 33.5%) tannins respectively. The amount of iron content of the extracts and samples of Acacia species was determined since the Iron hinders the process of retanning leather of Iron content was determined by atomic absorption spectrophotometry. The iron content of bark extracts of A nilotica, A tomentosa and A seyal is 0.0044%, 0.0040% and 0.0029% respectively. In contrast, the iron content of bark extract of the three species of Acacia had lower percentage compared to that of Mimosa (0.00475%), which is imported from Kenya. The tannins of a mixture of powder of Acacia nilotica and bark of the acacia seyal were identified by using thin layer chromatography (TLC), ultraviolet and infrared spectroscopy. Comparisons of the absorption spectra and TLC of the reference tannins and some phenolics with that of a mixture extracts revealed the presence of both condensed and hydrolysable tannins, since it consists of catechin, tannin and gallic acids. The leaching materials were powdered using spray drier. They exhabited excellent properties, when used for tannage of leather. Better physical and chemical properties of leather were achieved compared with leather tanned using mimosa powder.