Sintesis dan karakterisasi kompleks Gadolinium (III) dengan ligan 1,3,5-Benzenatrikarboksilat (H3BTC) menggunakan metode Solvotermal

ABSTRACT:

Gadolinium is a rare earth metal element which is very strong paramagnetic because it has seven valence electrons and has an outer energy level of 4f which is partially filled with electrons. It has a characteristic energy level that induces excitation in the luminescence process. Apart from that, gadolinium also has pores that can be used as gas storage. The ligand used in the synthesis is the 1,3,5-Benzenatricarboxylate (H3BTC) ligand. The H3BTC ligand is more widely used as a ligand in complex formation because of the ability of its carboxylic group to form coordinating covalent bonds with metals and hydrogen bonds with other compounds, such as H2O. H3BTC is a highly symmetric carboxylic acid and can be used as a building block in supramolecular synthesis because it has the potential to create distinctive shapes through hydrogen bonds. The H3BTC ligand reacts with the gadolinium ligand to form a complex compound that is paramagnetic. When gadolinium binds first to one water molecule before binding to the H3BTC ligand. The presence of these water coordinates will make gadolinium more effective in reducing toxicity.

Gadolinium(III) complexes with H3BTC ligands were synthesized using the solvothermal method with temperature variations of 80, 100, 120oC. The mole ratio used is metal: ligand (1:2). The synthesized product will be characterized using Powder X-Ray Diffraction (P-XRD) to determine the crystal structure and Scanning Electron Microscopy (SEM) to determine particle size, morphology, and elemental composition of compounds.

The product synthesized by the solvothermal method at temperatures of 80, 100, and 120oC is in the form of white powder. The average masses of the products obtained at temperatures of 80, 100, and 120oC are 0.2012 grams, 0.2035 grams, and 0.2105 grams, respectively. The mass of the product obtained increases with higher synthesis temperatures. Powder XRD analysis indicates that each identified Gd-BTC complex has a tetragonal crystal system with space group P4122. The most effective synthesis temperature is 100 degrees Celsius, exhibiting a crystallinity degree of 98.84% and a crystal size of 11.60 nm. Higher synthesis temperatures result in increased crystallinity. However, excessively high temperatures lead to excessively rapid and random movements, causing irregular crystal growth and a decrease in crystallinity degree. SEM characterization results illustrate that each complex has a microroad morphology with varying morphology sizes. Higher synthesis temperatures yield longer particle lengths and smaller particle diameters. EDS characterization reveals that the percentage composition of Gd-BTC elements identified differs from the theoretical composition percentages.

ABSTRACT:
Gadolinium is a rare earth metal element which is very strong paramagnetic becauseit has seven valence electrons and has an outer energy level of 4f which is partially filled withelectrons. It has a characteristic energy level that induces excitation in the luminescenceprocess. Apart from that, gadolinium also has pores that can be used as gas storage. Theligand used in the synthesis is the 1,3,5-Benzenatricarboxylate (H3BTC) ligand. The H3BTCligand is more widely used as a ligand in complex formation because of the ability of itscarboxylic group to form coordinating covalent bonds with metals and hydrogen bonds withother compounds, such as H2O. H3BTC is a highly symmetric carboxylic acid and can be usedas a building block in supramolecular synthesis because it has the potential to create distinctiveshapes through hydrogen bonds. The H3BTC ligand reacts with the gadolinium ligand to forma complex compound that is paramagnetic. When gadolinium binds first to one water moleculebefore binding to the H3BTC ligand. The presence of these water coordinates will makegadolinium more effective in reducing toxicity.Gadolinium(III) complexes with H3BTC ligands were synthesized using thesolvothermal method with temperature variations of 80, 100, 120oC. The mole ratio used ismetal: ligand (1:2). The synthesized product will be characterized using Powder X-RayDiffraction (P-XRD) to determine the crystal structure and Scanning Electron Microscopy(SEM) to determine particle size, morphology, and elemental composition of compounds.The product synthesized by the solvothermal method at temperatures of 80, 100, and120oC is in the form of white powder. The average masses of the products obtained attemperatures of 80, 100, and 120oC are 0.2012 grams, 0.2035 grams, and 0.2105 grams,respectively. The mass of the product obtained increases with higher synthesis temperatures.Powder XRD analysis indicates that each identified Gd-BTC complex has a tetragonal crystalsystem with space group P4122. The most effective synthesis temperature is 100 degreesCelsius, exhibiting a crystallinity degree of 98.84% and a crystal size of 11.60 nm. Highersynthesis temperatures result in increased crystallinity. However, excessively hightemperatures lead to excessively rapid and random movements, causing irregular crystalgrowth and a decrease in crystallinity degree. SEM characterization results illustrate that eachcomplex has a microroad morphology with varying morphology sizes. Higher synthesistemperatures yield longer particle lengths and smaller particle diameters. EDS characterizationreveals that the percentage composition of Gd-BTC elements identified differs from thetheoretical composition percentages

مستخلص البحث:

جلادولينيوم هو أحد عناصر اللوغان األرضية النادرة القوية جدا ألنه حيتوي على سبعة إلكرتوانت تكافؤ وله مستوى طاقةخارجي يبلغ4fمملوء جزئيا ابإللكرتوان، وله مستوى طاقة مميز حيفز اإلاثرة يف عملية التأللؤ. ابإلضافة إىل ذلك، حيتوي اجلادولينيومأيضا على مسام ميكن استخدامها لتخزين الغاز. الربيطة املستخدمة يف التوليف هي الربيطة١،٣،٥-كسيالتبنزينرتيكاربو(BTC3H.)تستخدم روابطBTC3Hكروابط يف تكوين معقد نظرا لقدرة جمموعاهتا على نطاق واسعكسيالت على تكوينالكربوكبات أخرى، مثلروابط تسامهية منسقة مع املعادن وروابط هيدروجينية مع مرO2HينتميBTC3Hكسيليةإىل أمحاض كربوكوحدة بناء يف التخليق فوق اجلزيئي ألنه لديه القدرة على إنشاء أشكال مميزة من خالل الروابط متناظرة للغاية وميكن استخدامهاهليدروجينية.كبات اجلادولينيوممت تصنيع مر(الثالث)املعقدة مع روابطBTC3Hابستخدام طرق الذوابن احلراري مع تغريات يفدرجات احلرارة تبلغ٨٠،١٠٠،١٢٠درجة مئوية. نسبة الشامات املستخدمة هي املعدن: ليجند(٢:١). سيتم متييز املنتجاتكبة ابستخدام حيوداملرمسحوق األشعة السينية(P-XRD)لتحديد البنية البلورية واجملهر اإللكرتوين املاسح(SEM)لتحديدكبكيب األويل للمرحجم اجلسيمات والشكل املورفولوجي والرت.املنتجات اليت مت تصنيعها بطريقةسولفوثريمال مع تغريات يف درجات احلرارة من٨٠و١٠٠و١٢٠درجة مئوية يفكتلة من املنتجات عند درجات حرارة شكل مسحوق أبيض، حصلت على متوسط٨٠،١٠٠،١٢٠درجة مئوية على التوايلمن٠.٢٠١٢gram؛٠.٢٠٣٥gram؛٠.٢١٠٥gramكتلة املنتج اليت مت احلصول عليها أكثر وأكثر مع زايدة درجة .حرارة التوليف. أظهر حتليل مسحوقXRDكبكل مر أنGd-BTCمت حتديده على أنه حيتوي على نظام بلوري رابعي الزواايمع جمموعة الفضاءP٤١٢٢كانت درجة حرارة التوليف األكثر فعالية هيو١٠٠درجة مئوية بدرجة تبلور٩٨.٨٤٪ وحجم بلورة١١.٦٠اننومرت.كلما زادت درجة حرارة التوليف، زاد طول اجلسيمات وأصغر قطر اجلزيئات. تظهر نتائج توصيفEDSأنالنسبة املئوية لتكوين عنصرGd-BTCاحملددة ختتلف عن النسبة املئوية لتكوين العنصر يف احلساابت النظرية