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تحضير ودراسة طيفية وحرارية لمعقدات بعض العناصر الإنتقالية مع ليكانـــــد 4- (2- بريديل آزو)- ريزورسينول
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لقد حضر في هذا البحث عدد من المعقدات الجديدة لبعض ايونات العناصر الانتقالية وهي كل من Fe(II) , Fe(III) , Co(II) , Ni(II) , Cu(II) و Zn(II) مع الكاشف العضوي -4 ( -2 بريديل آزو ) ريزورسينول المعروف ب (PAR) . حيث تم التحضير بعد تثبيت الظروف المثلى من دالة حامضية وتركيز مولاري بوساطة أطياف الاشعة فوق البنفسجية – المرئية لمحاليل مزج الايونات الفلزية مع محاليل الكاشف العضوي اعلاه ولمدى واسع من الدالة الحامضية والتركيز المولارية الخاضعة لقانون لامبرت – بير وقد تباينت ظروف التحضير بتابين الايونات الفلزية المدروسة . إذ تم تحضير ثلاثة معقدات لكل من آيوني النيكل (II) ومعقدين لآيون الكوبلت (II) ومعقدين لكل من الحديد (II) و (III) والخارصين (II) بأختلاف ظروف التحضير . كما تم التعرف على تراكيب هذه المعقدات عن طريق ايجاد النسبة المولية للفلز : الليكاند من خلال الدراسات الطيفية لمحاليل معقدات الفلزات المذكورة آنفا وذلك بأستخدام طريقة النسب المولية وقد تراوحت هذه النسب ما بين 1:1 أو 2:1 . وبعد تنقية المركبات الصلبة الناتجة درست بوساطة أطياف الاشعة فوق البنفسجية – المرئية حيث أظهرت أطياف محاليلها في الميثانول ازاحة حمراء لوحظت في منطقة الطيف المرئي لجميع المعقدات . كما درست بوساطة اطياف الاشعة تحت الحمراء إذ سجلت تغييرات واضحة لاطياف المعقدات نسبة الى طيف الليكاند الحر . ولوحظ ظهور حزم جديدة لم تكن موجودة في طيف الليكاند تدل على الاتباط الثنائي او الثلاثي السن لليكاند بالآيون الفلزي . إذ أنه من المتوقع ان تكون مواقع الارتباط لليكاند من خلال اوكسجين مجموعة الهيدروكسيل اورثو لحلقة الريزورسينول ( بعد ان تفقد بروتونها) ونيتروجين مجموعة الآزو القريبة من حلقة الريزوسينول ونيتروجين حلقة البريدين إذ تتكون حلقتان خماسيتان مستقرتان مما تعطيان استقرارا عاليا لهذه المعقدات . كما تم اجراء التحاليل الدقيقة لعناصر (N , H , C) لهذه المعقدات وتم تعيين النسب المئوية للأيونات الفلزية باستخدام مطيافية الامتصاص الذري اللهبي كما تم تعيين نسبة عنصر الكبريت وآيون الكلوريد بأستخدام طرق تحليلية مختلفة . وقد أظهرت نتائج هذه التحاليل جميعاً تقاربا للنسب المئوية المستحصلة مع النسب النظرية المحسوبة للصيغ التركيبية المقترحة لهذه المعقدات. أما دراسة التوصيلة الكهربائية لمحاليل المعقدات المحضرة في مذيبي الميثانول وثنائي ميثل فورم امايد فقد أظهرت ان المعقدات لا تمتلك صفات آيونية . كذلك فقد شملت الدراسة أيضا اجراء التحاليل الحرارية TGو DTG لليكاند الـ PAR وللمعقدات المحضرة جميعاً . وقد أثبتت هذه التحاليل وجود جزيئة ماء تبلور واحدة في جميع المعقدات ومن النسب المئوية للفقدان في الوزن التي سجلتها المنحنيات الحرارية ومقارنتها مع النسب المحسوبة نظريا فقد تم التوصل الى ان الخط العام للتحلل الحراري تضمن تكون جذور حرة للريزورسينول والبريدين مع تحرر غاز النيتروجين أثناء عملية التحلل . اما المواد الصلبة المتبقية من نواتج فهي أما العناصر او اكاسيد العناصر لكل معقد . واخيرا فقد دعمت النتائج أعلاه باجراء تحاليل طيف الكتلة الذي أثبت بما لايقبل الشك الصيغ الجزيئية المقترحة المحضرة . وتعتبر الدراستان الاخيرتان ( التحلل الحرارية وأطياف الكتلة ) الاولى من نوعها التي تجرى على ليكاند الـ PAR ومعقداتها الفلزية .

Publication Date
Fri Jun 30 2023
Journal Name
حوليات أداب عين شمس
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Thu Mar 31 2022
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Wed Jun 28 2023
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Wed Mar 18 2020
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