scholarly journals Zeolite Encapsulated Fe-poprhyrin for Catalytic Oxidation with Iodobenzene Diacetate (PhI(OAc)2)

2017 ◽  
Vol 57 (4) ◽  
Author(s):  
Gholamreza Karimipour ◽  
Maryam Rezaei ◽  
Davoud Ashouri
Keyword(s):  
Electron Microscopy ◽  
Sem Analysis ◽  
X Ray Diffraction ◽  
Nay Zeolite ◽  
X Ray ◽  
Diphenylacetic Acid ◽  
Ft Ir ◽  
Homogenous Catalyst ◽  
Epoxidation Of Cyclohexene ◽  
Scanning Electron

<em>meso</em>-Tetrakis(3-pyridyl)porphyrinatoiron(III) chloride encapsulated on NaY Zeolite [Fe(T-3-PyP)@NaY] was synthesized as a heterogeneous “ship-in-a-bottle” type catalyst and characterized by Fourier transform infrared (FT-IR), atomic absorption (AA), diffused reflectance UV-Vis (DR UV-Vis), X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis. The catalytic activity of Fe(T-3-PyP)@NaY was examined for the epoxidation of cyclohexene by PhI(OAc)<sub>2</sub> in CH<sub>3</sub>CN/H<sub>2</sub>O (5:1) and compared to that of Fe(T-3-PyP) as a homogenous catalyst. We found that the heterogeneous catalyst Fe(T-3-PyP)@NaY was stable and reusable for several times, and provided a mild condition and exhibited high activity and selectivity in the oxidation of alkenes to epoxides(16-94%). As representative examples for the use of Fe(T-3-PyP)@NaY/ PhI(OAc)<sub>2</sub> in organic oxidations, oxidation of 4-nitrobenzylalcohol to 4-nitrobenzaldehyde (97 %), oxidative dehydrogenation of diethyl 4-(2,6-dichlorophenyl)-2,6-dimethyl- 1,4-dihydro-3,5-pyridinedicarboxylate to the corresponding pyridine (100 %), diphenylacetic acid to benzophenone (64 %) was achieved.

scholarly journals A Novel Strong Cyan Luminescence Emission of Tb2O3 Particles

2021 ◽  
Author(s):  
Fatma Unal
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Ammonium Carbonate ◽  
Precipitation Method ◽  
X Ray Diffraction ◽  
Terbium Oxide ◽  
X Ray ◽  
Ft Ir ◽  
Pl Emission ◽  
Scanning Electron

Abstract Terbium oxide (Tb2O3) particles (NPs) were synthesized by precipitation method using ammonium carbonate as precipitation agent. Effects of precursor molarity (0.1, 0.15 and 0.2 M) on photoluminescence (PL) behaviour of the NPs were investigated. The presence of the Tb2O3 phase was confirmed by X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR) analyses. Morphological investigations of the produced powders were made by Field Emission Gun-Scanning Electron Microscopy (FEG-SEM). It showed that the morphology of Tb2O3 particles transformed from the nanograin chain to bundles morphology of rod-like as the amount of precursor molarity increased. Emission spectrum were investigated by Photoluminescence (PL) Spectroscopy. All the Tb2O3 particles exhibited the strongest peak at 493 nm ascribed to 5D4-7F6 (magnetic dipole (MD), C2) transition. The increase in the number of C2 sites released from the MD transition with the increase of the precursor molarity caused a negative increase in the b* (yellowness/blueness of the emission) value in the CIE diagram, indicating that the colour shifted to the blue region. The Tb2O3 particles produced by the precipitation method exhibited novel strong cyan colour and the PL emission intensity increased with increasing molarity.

The Characterization of Bovine Bone-Derived Hydroxyapatite Isolated Using Novel Non-Hazardous Method

2020 ◽  
Vol 45 ◽  
pp. 49-56
Author(s):  
Aniek Setiya Budiatin ◽  
Samirah ◽  
Maria Apriliani Gani ◽  
Wenny Putri Nilamsari ◽  
Chrismawan Ardianto ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Extraction Method ◽  
Bovine Bone ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Novel Method ◽  
Scanning Electron

Bovine bone is a considerable source for the production of hydroxyapatite. The recent study reported a novel method to extract hydroxyapatite from bovine bone without producing hazardous residue. The bovine bones were cut and boiled in the opened chamber followed by boiling in pressurized tank. The bones were then soaked into 95% ethanol. Calcination was then conducted in 800°C, 900°C and 1,000°C, for 2 hours. The result was then grinded and sieved. The powder then was characterized using Fourier transform infrared (FT-IR), Scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD) to measure the purity of hydroxyapatite. It is concluded that the hydroxyapatite derived from this process showed 100% purity, resulting 35.34 ± 0.39% w/w from the wet bone weight and 72.3% w/w from the dried weight. The present extraction method has been proven to yield high amount of pure hydroxyapatite as well as reducing the use of hazardous reagent.

Synthesis of Triethynylborazine-Polyhydromethylsiloxane Copolymers and its Ceramization

2013 ◽  
Vol 774-776 ◽  
pp. 629-633
Author(s):  
Ji Feng Jiang ◽  
Kang Kang Guo ◽  
Ya Ping Zhu ◽  
Fan Wang ◽  
Hui Min Qi
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Nuclear Magnetic Resonance ◽  
Fourier Transform ◽  
Thermogravimetric Analysis ◽  
X Ray Diffraction ◽  
Hydrosilylation Reaction ◽  
X Ray ◽  
Ft Ir ◽  
Scanning Electron

Triethynylborazine-polyhydromethylsiloxane copolymers (TEB-PHMSs) were prepared through hydrosilylation reaction between -C≡CH attached to boron and ≡Si-H. The structures of TEB-PHMSs were characterized by Fourier transform Infrared (FT-IR) and Nuclear Magnetic Resonance (NMR) spectroscopy. Their cure behavior were examined by Differential Scanning Calorimeter (DSC) and FT-IR, and then thermostability and ceramization of cured TEB-PHMS were investigated by Thermogravimetric analysis (TGA), pyrolysis-GC-MS, X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The results indicated that TEB-PHMSs could be cured and converted into an outstanding thermostable SiBCN ceramics.

Synthesis, Characterization and Magnetism of Nanosized Copper Ferrite

2008 ◽  
Vol 368-372 ◽  
pp. 604-606 ◽  
Author(s):  
Wei Zhong Lv ◽  
Zhong Kuang Luo ◽  
Bo Liu ◽  
Xiang Zhong Ren ◽  
Hong Hua Cai ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Thermal Analysis ◽  
Copper Ferrite ◽  
Sonochemical Method ◽  
Thermal Gravimetric ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir ◽  
Scanning Electron

Copper ferrite powders were successfully synthesized by sonochemical method. The resultant powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), FT-IR, differential thermal analysis-thermal gravimetric (DTA-TG), differential scanning calorimetry (DSC) and VSM. The particle saturation magnetization (Ms) is 66 emu/g and an intrinsic coercive force (iHc) is 2100 Oe when the precursor calcined at 950 °C for 15 h.

scholarly journals FT-IR φασματοσκοπική μελέτη ασθενειών των οστών

2016 ◽  
Author(s):  
Στυλιανός Κυριαζής
Keyword(s):  
Electron Microscopy ◽  
Reactive Oxygen Species ◽  
Scanning Electron Microscopy ◽  
Oxygen Species ◽  
X Ray Diffraction ◽  
Cross Link ◽  
X Ray ◽  
Ft Ir ◽  
Ros Reactive Oxygen Species ◽  
Scanning Electron

Οι παθήσεις των οστών και η θεραπεία τους σχετίζονται άμεσα με την γνώση των βλαβών που προκαλούν οι ασθένειες σε μοριακό επίπεδο των βιολογικών μορίων, ιστών και υγρών του σώματος. Μέχρι σήμερα, πολλές από τις ασθένειες δεν μπορούν να αντιμετωπιστούν μη επεμβατικά, επειδή δεν έχουν παρασκευασθεί φάρμακα τα οποία θα μπορούσαν να επιδιορθώσουν τις βλάβες. Δυστυχώς, μέχρι σήμερα, η συνήθης αντιμετώπιση των περισσότερων ασθενειών είναι η χειρουργική αφαίρεση του τμήματος του οστού που έχει φθαρεί. Η γνώση επομένως των βλαβών οι οποίες προκαλούνται από τις ασθένειες θα μπορούσε ενδεχομένως να οδηγήσει στην ανάπτυξη φαρμάκων και την εξέλιξη της μη επεμβατικής αντιμετώπισης αυτών των ασθενειών .Στην παρούσα μελέτη χρησιμοποιήθηκαν μη καταστρεπτικές μέθοδοι, όπως η υπέρυθρη φασματοσκοπία με μετασχηματισμό Fourier (Fourier Transform Infrared, FT-IR) και ηλεκτρονιακό μικροσκόπιο σάρωσης (Scanning Electron Microscopy, SEM) και περίθλαση ακτίνων Χ (XRD, X-Ray Diffraction).Για την μελέτη λήφθηκαν δείγματα φλοιώδους και σπογγώδους οστού, καθώς και χόνδρου οστού από 42 ασθενείς ηλικίας 31 έως 87 ετών, οι οποίοι υποβλήθηκαν σε χειρουργική αντιμετώπιση. Από αυτά 15 προήλθαν από ασθενείς με αναπτυξιακή δυσπλασία του ισχίου, 1 από αγκυλοποιητική αρθρίτιδα του ισχίου, 4 από έκτοπη οστεοποίηση του ισχίου, 3 λόγω οστεονέκρωσης της μηριαίας κεφαλής, 1 από ρευματοειδή αρθρίτιδα του γόνατος, 2 έπειτα από χαλάρωση ολικής αρθροπλαστικής γόνατος, 4 έπειτα από χαλάρωση ολικής αρθροπλαστικής ισχίου και 2 από ψωριασική αρθρίτιδα (ισχίου και γόνατος) και 10 καρκινικά. Τα δείγματα δεν υπέστησαν καμία επεξεργασία πέραν της αφαίρεσης των προσμίξεων αίματος και λιπαρών συστατικών του εξωτερικού περιβάλλοντος του οστού. Τα υπέρυθρα φάσματα έδειξαν σημαντικές διαφορές μεταξύ των υγιών οστών και των οστών τα οποία προήλθαν από τα δείγματα των ασθενών. Οι μεταβολές ήταν συνάρτηση της ασθένειας αλλά και των συστατικών του εκάστοτε οστού. Γενικά διαπιστώθηκε ότι σε κάθε περίπτωση το οξειδωτικό στρες συμμετέχει σε κάποιο από τα στάδια της ανάπτυξης της ασθένειας. Κατά το οξειδωτικό στρες παράγονται ελεύθερες ρίζες (ROS, reactive oxygen species) οι οποίες οδηγούν σε υπεροξείδωση των λιπιδίων και φωσφολιπιδίων των μεμβρανών των κυττάρων και κατά συνέπεια στην καταστροφή των κυττάρων. Από τις μειώσεις των εντάσεων και τις μετατοπίσεις των απορροφήσεων τάσης των ομάδων νΟΗ και νΝΗ στην περιοχή του φάσματος από 4000-3000 cm-1 φαίνεται ότι ο υδροξυαπατίτης χάνει τις ομάδες -ΟΗ, ενώ οι δεσμοί υδρογόνου οι οποίοι συγκρατούν την α-έλικα των κολλαγονούχων πρωτεϊνών μεταβάλλουν την έντασή τους. Αυτό επιβεβαιώνεται από τις μετατοπίσεις των ταινιών των Amide I και Amide II των πρωτεϊνών προς μικρότερες συχνότητες στην περιοχή 1700-1500 cm-1, ως αποτέλεσμα της καταστροφής της α-έλικας. Το φαινόμενο αυτό είναι περισσότερο έντονο στην περίπτωση των χόνδρων. Η ταινία περίπου στα 3080 cm-1, η οποία συνδέεται με την ολεφινική ομάδα (v=CH) επιβεβαιώνει την επίδραση των ελευθέρων ριζών στα στάδια της ασθένειας. Η αύξηση των εντάσεων των ταινιών των μεθυλ (vCH3) και μεθυλενομάδων (vCH2) στην περιοχή 3000-2850 cm-1 συνδέεται με την αύξηση του λιπόφιλου περιβάλλοντος, ως αποτέλεσμα της επίδρασης του οξειδωτικού στρες και τον σχηματισμό αμυλοειδών πρωτεϊνών. Η ταινία στα 1743 cm-1 η οποία αποδίδεται σε σχηματισμό αλδεϋδικών ομάδων συνδέεται με το οξειδωτικό στρες και επομένως με την φλεγμονή. Σε ασθενείς οι οποίοι εμφάνιζαν χρόνια φλεγμονή η ένταση της ταινίας είναι αρκετά υψηλή. Τα υπέρυθρα φάσματα έδειξαν την καταστροφή του υδροξυαπατίτη των οστών και την μετατροπή του σε άλατα του φωσφορικού ασβεστίου, προσδίδοντας επομένως μεγαλύτερη σκληρότητα και ευθραυστότητα στο οστό. Η καταστροφή του βιολογικού υδροξυαπατίτη επιβεβαιώθηκε με XRD ανάλυση.Οι SEM αναλύσεις έδειξαν την καταστροφή των πρωτεϊνών του οστού. Από την ανάλυση της εικόνας φάνηκαν οι θέσεις διασταυρούμενων (cross-link) και διακλαδούμενων (branch-link) πολυμερισμών. Οι θέσεις αυτές αποτελούν δραστικά σημεία σχηματισμού φωσφορικών αλάτων, τα οποία μειώνουν την αντοχή των οστών. Επίσης επιβεβαιώνουν την επίδραση των ελευθέρων ριζών.Η έκτοπη οστεοποίηση φαίνεται να μην είναι αποτέλεσμα της δράσης των οστεοβλαστών, αλλά της αδυναμίας λειτουργίας του ATP στον φυσιολογικό κύκλο λόγω ισχαιμικών επεισοδίων που επικρατούν στην περιοχή ανάπτυξης του οστού. Αυτό επιβεβαιώθηκε από την σύγκριση των φασμάτων έκτοπου οστού και επασβεστωμένης αορτικής βαλβίδας. Τέλος, στον σχηματισμό των αμυλοειδών πρωτεϊνών αποδίδουμε την αντίσταση στην θεραπευτική αγωγή και ακτινοθεραπεία των οστών.

Preparation of Nanosized Barium Ferrite Spinel by a Sonochemical Method

2008 ◽  
Vol 368-372 ◽  
pp. 607-609
Author(s):  
Bo Liu ◽  
Wei Zhong Lv ◽  
Zhong Kuang Luo ◽  
Xiang Zhong Ren ◽  
Hong Hua Cai ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Barium Ferrite ◽  
Sonochemical Method ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ultrasound Radiation ◽  
Ft Ir ◽  
Scanning Electron ◽  
Ferrite Spinel

Nanosized barium ferrite spinel particles were prepared with the aid of ultrasound radiation by a precursor approach. A precursor was got by sonicating an aqueous solution of BaCl2, Fe (NO3)3·9H2O and urea firstly. Nanosized BaFe2O4 particles with a size of ca.40nm were prepared after the precursor was heated at 950 °C for 15 h. The nanosized barium ferrite particles and the precursor were characterized by powder X-ray diffraction, scanning electron microscopy, FT-IR and differential scanning calorimetry.

Effects of La0.5Sr0.5CoO3 sol concentration on the microstructure and dielectric properties of Ba0.6Sr0.4TiO3 films prepared by sol-gel method on Ti substrate

2012 ◽  
Vol 1494 ◽  
pp. 253-258
Author(s):  
Dan Jiang ◽  
Songwei Han ◽  
Xuelian Zhao ◽  
Jinrong Cheng
Keyword(s):  
Electron Microscopy ◽  
Dielectric Properties ◽  
Sol Gel ◽  
Sem Analysis ◽  
X Ray Diffraction ◽  
Gel Method ◽  
X Ray ◽  
Sol Gel Method ◽  
Bst Films ◽  
Scanning Electron

ABSTRACTBa0.6Sr0.4TiO3 (BST) thin films were deposited on La0.5Sr0.5CoO3 (LSCO) buffered Ti substrates. Both BST and LSCO were prepared by sol-gel method. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis were used to investigate the effect of LSCO sol concentration on the crystallinity and surface morphology of the films. The results show that with the increase of LSCO sol concentration, BST films show variation of the structure and dielectric properties. BST films for LSCO of 0.2 mol/L exhibit a better crystallinity and improved dielectric properties, with the tunability, dielectric constant and tanδ of 30%, 420 and 0.028 respectively.

From Layered Ni(OH)2 Thin Films to Ni(so4)0.3(OH)1.4 Nanobelts through so42- Inserting in Colloid-Based Route

2011 ◽  
Vol 295-297 ◽  
pp. 1548-1553
Author(s):  
Zhi Yong Jia
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Large Scale ◽  
Ph Value ◽  
Shape Evolution ◽  
X Ray Diffraction ◽  
Weak Base ◽  
X Ray ◽  
Ft Ir ◽  
Scanning Electron

The single-crystalline nanobelts of monoclinic Ni(SO4)0.3(OH)1.4have been synthesized on a large scale through a convenient, low-temperature hydrothermal method. The influences of reaction time, pH value, concentration of ammonia on the phase and shape evolution of nanobelts were systematically investigated. It was found that the initial layered Ni(OH)2 thin films as intermediates could be split and converted into the monoclinic Ni(SO4)0.3(OH)1.4nanobelts through SO42-ions inserting process. The formation mechanism of nanobelts involved in the inserting process and the corresponding drive force have been investigated in detail by means of X-ray diffraction (XRD), and scanning electron microscopy (SEM), FT-IR spectra and pH value analyses. In addition to, we have also found that the ammonia molecules acted as both weak base and ligand agent was crucial to the controlling nucleation and inserting process in the formation process of nanobelts.

scholarly journals Synthesis of Zeolite NaA from Low Grade (High Impurities) Indonesian Natural Zeolite

2014 ◽  
Vol 14 (2) ◽  
pp. 138-142 ◽  
Author(s):  
Asalil Mustain ◽  
Gede Wibawa ◽  
Mukhammad Furoiddun Nais ◽  
Miftakhul Falah
Keyword(s):  
Electron Microscopy ◽  
Natural Zeolite ◽  
Synthesis Method ◽  
Sem Analysis ◽  
Low Grade ◽  
Framework Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Zeolite Naa ◽  
Scanning Electron

The zeolite NaA has been successfully synthesized from the low grade natural zeolite with high impurities. The synthesis method was started by mixing natural zeolite powder with NH4Cl aqueous solution in the reactor as pretreatment. The use of pretreatment was to reduce the impurities contents in the zeolite. The process was followed by alkaline fusion hydrothermal treatment to modify the framework structure of natural zeolite and reduce the SiO2/Al2O3 ratio. Finally, the synthesized zeolite was calcined at 600 °C for 2 h. The final zeolite product was characterized by X-ray fluorescence (XRF), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that the morphology of the zeolite NaA was cubic shape as observed by SEM analysis and the synthesized zeolite NaA with pretreatment gave less impurity than without pretreatment.

scholarly journals Synthesis and some properties of compounds Cu2PrSb3S7 and Cu2ErSb3S7

2020 ◽  
Vol 64 (11) ◽  
pp. 13-17
Author(s):  
Reyhan M. Agayeva ◽  
Keyword(s):  
Electron Microscopy ◽  
Eutectic Point ◽  
Sem Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dissolution Zone ◽  
Concentration Interval ◽  
Microhardness Testing ◽  
Physicochemical Methods ◽  
Scanning Electron

The phase equilibrium in systems of CuSbS2 – PrSbS3 and CuSbS2 – ErSbS3 has been studied by physicochemical methods (Differential thermal analysis – DTA, X-ray diffraction phase analysis, Scanning Electron Microscopy – SEM analysis and microhardness testing) and their T-x diagrams were drawn. It was determined that both systems are quazibinary and characterized by formation of Cu2LnSb3S7 -type (Ln = Pr, Er) compounds. Cu2PrSb3S7 melts congruently at 1050 K and is the phase with unstable content. Its dissolution zone changes within concentration interval of 32-37 mole% of PrSbS3. Cu2PrSb3S7 divides the system into two sub-systems: CuSbS2-Cu2PrSb3S7 and Cu2PrSb3S7-PrSbS3. Both of sub-systems are eutectic. The coordinates of the eutectic point are like following: 15 mole % PrSbS3, T = 740 K and 50 mole % PrSbS3, T = 790 K. Cu2ErSb3S7 melts at 920 K by decomposition. At 725K between Cu2ErSb3S7 and CuSbS2 compounds in content of 15 mole % of ErSbS3 is formed eutectic balance. 4 mole % of solid solution is formed on base of CuSbS2. Both compounds are crystallized by naffildite-type structure in the form of rhombic syngonia (Cu2PrSb3S7 – a = 1.444; b = 2.146; c = 0.3995 nm; z = 4; Cu2ErSb3S7 – a = 1.430; b = 2.128; c = 0.380 nm; z = 4; stereogroup Pbnm or Pbn21).

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