scholarly journals Polyol-mediated synthesis of size-controlled copper nanoparticles under microwave irradiation

Author(s):  
Anh Trần Thị Kiều ◽  
Trung Đặng Bảo

In this research, well-dispersed zero-valent copper nanoparticles (CuNPs) were successfully synthesized from a well-defined complex of [Cu(OH)(TMEDA)]2Cl2 in neat glycerol via a polyol method, under microwave irradiation (MW) assistance. The as-prepared CuNPs were thoroughly characterized by means of various techniques such as inductively coupled plasma mass spectrometry (ICP-MS), Ultraviolet-visible spectroscopy (UV-vis), X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses, evidencing the formation of the spherical nanoparticles with the range of 3.24.2 nm in mean diameter. In addition, the size control of obtained CuNPs was examined via reaction time, thereby showing that the formation of CuNPs conformed to the model of “mono-dispersion”.

Materials ◽  
2019 ◽  
Vol 12 (19) ◽  
pp. 3267
Author(s):  
Gigliola Lusvardi ◽  
Francesca Sgarbi Stabellini ◽  
Roberta Salvatori

(1) Background: valuation of the bioactivity and cytocompatibility of P2O5-free and CeO2 doped glasses. (2) Methods: all glasses are based on the Kokubo (K) composition and prepared by a melting method. Doped glassed, K1.2, K3.6 and K5.3 contain 1.2, 3.6, and 5.3 mol% of CeO2. Bioactivity and cytotoxicity tests were carried out in simulated body fluid (SBF) solution and murine osteocyte (MLO-Y4) cell lines, respectively. Leaching of ions concentration in SBF was determined by inductively coupled plasma mass spectrometry (ICP-MS) and optical emission spectrometry (ICP-OES). The surface of the glasses were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques. (3) Results: P2O5-free cerium doped glasses are proactive according to European directives. Cerium increases durability and retards, but does not inhibit, (Ca10(PO4)6(OH)2, HA) formation at higher cerium amounts (K3.6 and K5.3); however, cell proliferation increases with the amount of cerium especially evident for K5.3. (4) Conclusions: These results enforce the use of P2O5-free cerium doped bioactive glasses as a new class of biomaterials.


Minerals ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 467
Author(s):  
Qing He ◽  
Yanfei An ◽  
Fangji Sun ◽  
Chunkit Lai

The occurrence of pyrite concretions in the Permian Longtan Formation sheds light on the paragenesis, formation conditions and regional paleoenvironment. We analyzed the mineral and geochemical characteristics of pyrite concretions using scanning electron microscopy-energy dispersive spectrometer (SEM-EDS), X-ray diffraction (XRD) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) from the Longtan Formation shales in Anhui, Eastern China. These pyrite concretions consist of two types, each with a distinct nucleus and outer layer: The former is mainly made up of quartz, bivalve fragments and minor gypsum, ankerite, siderite and pyrite, the latter consists of pyrite (FeS2) in the voids of quartz. Based on the correlation matrix and geochemical/mineralogical affinity, trace elements in the pyrite concretions fall into three groups, that is, I (Sr, Ba, Rb and K) in calcic minerals from bivalve-bearing nucleus, II (Nb, Ta, Zr and Hf) in certain heavy minerals and III (V, Cr, Co and Ni) in pyrites. Mineral assemblage and paragenetic analysis show that the formation of pyrite concretions can be divided into three stages: (1) deposition of bivalve-bearing nucleus, (2) lithification of diatoms and (3) diagenesis of pyrite. Mineral and geochemical indicators suggest that the formation environment of pyrite concretions has undergone a major shift from lagoon with intense evaporation, to strong reducing marsh.


Crystals ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 98 ◽  
Author(s):  
Sijia Wang ◽  
Zengzhe Xi ◽  
Pinyang Fang ◽  
Xiaojuan Li ◽  
Wei Long ◽  
...  

A single crystal with nominal composition Pb(Mg1/3Nb2/3)O3-32PbTiO3 (PMN-32PT) was grown by the Bridgman technique. Crystal orientation was determined using the rotating orientation X-ray diffraction (RO-XRD). Element distribution was measured along different directions using inductively coupled plasma-mass spectrometry (ICP-MS). The effect of the element segregation along axial and radial directions on the electrical properties of the PMN-32PT crystal was investigated. It is indicated that the electrical properties of the samples along the axial direction were strongly dependent on the PT (PbTiO3) content. With the increase of the PT content, the piezoelectric coefficient and remnant polarization were improved. Differently, the electrical properties of the samples along the radial direction were mainly determined by the ratio of the Nb and Mg. The reasons for the element segregation and electrical properties varied with the composition were discussed.


Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 766
Author(s):  
Uxue Sanchez-Garmendia ◽  
Javier G. Iñañez ◽  
Gorka Arana

Ancient ceramics recovered after a long burial period have probably undergone several alterations and contaminations, introducing a chemical variability, affecting the ceramic’s natural variability. That is, the chemical and the mineralogical compositions of the ceramic pastes after their deposition will not be the same as they originally were. Therefore, it is known that the alteration and contamination processes, and the discrimination of some elements, should be considered when studying the ceramics to avoid incorrect interpretations about their provenance, technology and the use of the artefact, as well as its proper preservation. In the present work, the authors performed an experimental approach in order to study the alterations and contaminations that occurred in 60 ceramic cylinders buried in two different underwater environments. Once the pieces were taken out from the water environments, they were characterized by a multi-analytical approach. For this purpose, inductively coupled plasma mass spectrometry (ICP-MS), X-ray diffraction (XRD), scanning electron microscopy–energy dispersive spectrometry (SEM–EDS) and Raman spectroscopy were used. Newly formed minerals of different forms have been identified, with different crystallization grades. Some examples are the needles, flakes, sponges and long and short prisms composed of several elements such as Ca, F, S and O.


Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1006 ◽  
Author(s):  
Krzysztof Kupczak ◽  
Rafał Warchulski ◽  
Mateusz Dulski ◽  
Dorota Środek

Slags from the historic metallurgy of Zn-Pb ores are known for unique chemical and phase compositions. The oxides, silicates, aluminosilicates, and amorphous phases present therein often contain in the structure elements that are rare in natural conditions, such as Zn, Pb, As. The study focuses on processes occurring on the contact of the melted batch and the refractory materials that build the furnace, which lead to the formation of these phases. To describe them, chemical (X-ray fluorescence (XRF), inductively coupled plasma mass spectrometry (ICP-MS)) and petrological ((X-ray diffraction (XRD), electron probe micro-analyses (EPMA), Raman spectroscopy) analyses were performed on refractory material, slag, and contact of both. Two main types of reactions have been distinguished: gas/fluid- refractories and liquid- refractories. The first of them enrich the refractories with elements that migrate with the gas (Pb, K, Na, As, Zn) and transport the components building it (Fe, Mg, Ca) inward. Reactions between melted batch and refractory materials through gravitational differentiation and the melting of refractories lead to the formation of an aluminosilicate liquid with a high content of heavy elements. Cooling of this melt causes crystallization of minerals characteristic for slag, but with a modified composition, such as Fe-rich pyroxenes, Pb-rich K-feldspar, or PbO-As2O3-SiO2 glass.


Clay Minerals ◽  
2013 ◽  
Vol 48 (2) ◽  
pp. 295-308 ◽  
Author(s):  
E. Myllykylä ◽  
M. Tanhua-Tyrkkö ◽  
A. Bouchet ◽  
M. Tiljander

AbstractThe effects of simulant groundwater composition, pH and temperature on the dissolution and alteration of Na- and Ca-montmorillonite have been studied. Prior to the experiments, Wyoming type Na-montmorillonite, Swy-2, was purified to decrease the amount of accessory minerals. For Ca-montmorillonite experiments, the interlayer cation Na+ of purified Swy-2 was exchanged with Ca2+. The batch experiments were conducted with the purified montmorillonites in simulated fresh and saline waters at 25°C and 60°C under anaerobic conditions in an Ar atmosphere. The concentrations of Si, Al, Fe and Mg were analysed from ultra-filtered solution samples with High Resolution Inductively Coupled Plasma Mass Spectrometry (HR-ICP-MS) as a function of dissolution time. The pH evolution was also measured. The solid smectite phases were analysed with X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). XRD analyses indicated that the nature of the smectite mineral did not change over 140 days. However, the experimental conditions, more or less, modified the structure (e.g. the layer stacking of montmorilllonite; the partial dissolution of the smectite), which cannot be detected by XRD but was evidenced by chemical data, and can be considered as a possible contributor to the stacking faults of the montmorillonite. The log rates (mol g–1 s–1), based on the dissolved amount of Si, varied between –10.64 and –12.13 depending on the experimental conditions.


2013 ◽  
Author(s):  
Ευθύμιος Καπέλλιος

Ως νανοσωματίδια ορίζονται υλικά των οποίων τουλάχιστον 2 διαστάσεις δεν ξεπερνούν τα 100 νανόμετρα (1-100 nm). Τα σωματίδια αυτά ταξινομούνται σε δύο κύριες κατηγορίες: τα φυσικά προϊόντα (πχ Μακρομόρια, Βιο-κολλοειδή) και τα τεχνητά κατασκευασμένα. Τις τελευταίες δεκαετίες έχει εκδηλωθεί τεράστιο ενδιαφέρον για τα νανοσωματίδια καθώς μπορούν να χρησιμοποιηθούν σε ποικίλες εφαρμογές λόγω των διαφορετικών φυσικών, χημικών και βιολογικών ιδιοτήτων τους. Τα νανοσωματίδια μπορούν να χαρακτηριστούν χρησιμοποιώντας διάφορες τεχνικές συμπεριλαμβανομένης της ηλεκτρονικής μικροσκοπίας, της χρωματογραφίας αποκλεισμού μεγέθους, της κρυσταλλογραφία ακτίνων Χ και της Φασματοσκοπίας πυρηνικού μαγνητικού συντονισμού. Αντίθετα με την μεγάλη ποικιλία των διαθέσιμων τεχνικών, η ανάγκη για γρήγορες, χωρίς σήμανση και στατιστικά ισχυρές αναλύσεις παραμένει. Μεγάλος αριθμός ερευνητικών εργαστηρίων και εταιριών ασχολείται με την ανάπτυξη νέων τεχνικών αλλά κυρίως με την βελτίωση και τον συνδυασμό των ήδη υπαρχόντων. Τα τελευταία χρόνια είναι διαθέσιμη μια καινούργια συνδυαστική τεχνική που περιλαμβάνει νανο-ηλεκτροψεκασμό (nanoelectrospray: nES) συζευγμένο με φασματομετρία διαφορικού αναλυτή κινητικότητας ιόντων (ion mobility spectrometry: IMS) και ανιχνευτή μέτρησης συμπυκνωμένων σωματιδίων (condensed particle counting: CPC). Η τεχνική αυτή, σε αρκετές δημοσιεύσεις αναφέρεται ως μοριακός αναλυτής ηλεκτροφορετικής κινητικότητας αέριας φάσης (Gas-phase Electrophoretic Mobility Molecular Analyzer: GEMMA) και μέχρι στιγμής έχει χρησιμοποιηθεί με επιτυχία για τον προσδιορισμό μεγέθους μακρομορίων βιολογικής προέλευσης καθώς και σε πληθώρα ανόργανων τεχνητά κατασκευασμένων νανοσωματιδίων.Ο σκοπός της παρούσας εργασίας είναι η αξιολόγηση και η ανάπτυξη του GEMMA για το προσδιορισμό του μεγέθους και της στοιχειακής σύνθεσης νανοσωματιδίων. Για την επίτευξη του, αναλύθηκε μεγάλος αριθμός πρωτεϊνών και πρωτεϊνικών συμπλόκων τα οποία απομονώθηκαν και καθαρίστηκαν χρησιμοποιώντας καθιερωμένα βιοχημικά πρωτόκολλα. Τα αποτελέσματα συγκρίθηκαν με εκείνα, δύο υδροδυναμικών τεχνικών (multi-angle laser light scattering: MALLS, quasi-elastic light scattering: QELS) καθώς και με μια καλά εδραιωμένη τεχνική φασματομετρίας Μάζας (LTQ-Orbitrap). Έμφαση δόθηκε στην αξιολόγηση διάφορων αναλυτικών παράμετρων όπως ευαισθησία, ακρίβεια, επαναληψιμότητα, χρόνος μέτρησης, χρόνος ανάλυσης των δεδομένων, δείγμα που χρειάζεται και καταναλώνεται ανά μέτρηση. Επιπλέον το GEMMA χρησιμοποιήθηκε για τον προσδιορισμό της ολιγομερικής κατάστασης πρωτεΐνης με διαφορετικές σημειακές μεταλλάξεις. Επίσης αναλύθηκαν δείγματα DNA. Το πιο απαιτητικό κομμάτι αυτής της μελέτης ήταν η ανάπτυξη θεωρητικού μοντέλου για τον προσδιορισμό της αλλάγης της δομικής διαμόρφωσης του πρωτεϊνικού ομοιοπολικού συμπλόκου GFP-GBP-YFP (Fluo) με προσθήκη υποστρώματος. Η Fluo λειτουργεί ως βιοαισθητήρας γλυκόζης.Η δυναμική της τεχνικής ελέγχτηκε περαιτέρω με ανάλυση διάφορων ανόργανων νανοσωματιδίων γνωστού μεγέθους, σχήματος και συσσωματωμάτων. Η μελέτη επεκτάθηκε σε εργαστηριακά συντιθέμενα νανοσωματίδια από άνθρακα και τα αποτελέσματα συγκρίθηκαν με μετρήσεις Ηλεκτρονικής Μικροσκοπίας Διέλευσης (Transmission Electron Microscopy: TEM).Το βασικό μειονέκτημα αυτής της τεχνικής προκύπτει από τις δυνατότητες του ανιχνευτή συμπυκνωμένων σωματιδίων (CPC). Αυτός ο εξαιρετικά ευαίσθητος ανιχνευτής δεν παρέχει πληροφορία σχετικά με την στοιχειακή σύσταση των νανοσωματιδίων που ανιχνεύει. Σε μια προσπάθεια να ξεπεραστεί αυτή η αδυναμία, έγινε off-line σύζευξη του nES-DMA με Φασματομετρία επαγωγικά συζευγμένου πλάσματος (Inductively Coupled Plasma Mass Spectrometry: ICP-MS) σε λειτουργία ανίχνευσης μεμονωμένων σωματιδίων (single particle mode,SPM). Με τον τρόπο αυτό επιτεύχθηκε ο προσδιορισμός τόσο του μεγέθους όσο και της στοιχειακής σύστασης νανοσωματιδίων σε μια μόνο μέτρηση. Οι προσπάθειες εστιάστηκαν, επίσης, στη βελτιστοποίηση της λειτουργίας της GEMMA. Έτσι προσαρμόστηκαν 4 διαφορετικοί τριχοειδείς σωλήνες στην μονάδα ηλεκτροψεκασμού και προσδιορίστηκαν οι αποδοτικότερες συνθήκες λειτουργίας (π.χ ροή, αγωγιμότητα κ.λ.π).Οι κύριοι άξονες της παρούσας μελέτης μπορούν να συνοψιστούν: 1) στην κατανόηση και έλεγχο της δυνατότητας προσδιορισμού των ιδιοτήτων βιομορίων (μέγεθος, σχήμα, ολιγομερισμός και σχετική μοριακή μάζα) που απομονώθηκαν και καθαρίστηκαν, χρησιμοποιώντας καθιερωμένα εργαστηριακά πρωτόκολλα, 2) στον έλεγχο των δυνατοτήτων της ως προς τον χαρακτηρισμό των ιδιοτήτων (μέγεθος, σχήμα ολιγομερισμός, σύσταση) ανόργανων νανοσωματιδίων, και 3) στην βελτίωση της τεχνικής (σύζευξη με άλλους ανιχνευτές, αλλαγές στην οργανολογία) για την εξάλειψη των μειονεκτημάτων της και την διεύρυνση των δυνατοτήτων της. Οι πειραματικές προσεγγίσεις για την επίτευξη του σκοπού της διδακτορικής διατριβής διαφαίνεται με μεγαλύτερη λεπτομέρεια στο σχήμα 1.των μειονεκτημάτων της και την διεύρυνση των δυνατοτήτων της.


2021 ◽  
Vol 947 (1) ◽  
pp. 012027
Author(s):  
Tuyet-Mai Tran-Thuy ◽  
Ngoc-Thuy Nguyen-Thi ◽  
Trong-Phu Tran ◽  
Ngoc-Hung Tran-Le ◽  
Minh-An Dang ◽  
...  

Abstract K-OMS-2 (non-modified sample) and Ce-modified OMS-2 with different Ce-loading amounts were prepared by the refluxed method. The cryptomelane structure and elemental composition of synthesized samples were characterized with X-ray diffraction (XRD) and inductively coupled plasma mass spectrometry (ICP-MS), respectively. ICP-MS analysis revealed ~0.06 – 0.11 of K/Mn molar ratio and the Ce-loading amounts increased from 0 to —11.27 wt.% under increasing Ce-precursor concentration. Antibacterial activity against Pseudomonas aeruginosa was evaluated by the agar well diffusion method. The antibacterial ability against Pseudomonas aeruginosa was not recorded over K-OMS-2 (Ce0; 4.5 wt.% of K; 0 wt.% of Ce) and Ce3 (0.89 wt.% of K; 11.27 wt.% of Ce) samples while Ce2 sample (1.89 wt.% of K; 8.7 wt.% of Ce) showed a comparable antibacterial activity against Pseudomonas aeruginosa with ~12 mm of inhibition-zone diameter. This suggested the potentiality of using metal-modified cryptomelane in acceleration of antimicrobial ability.


Author(s):  
Julien M. Allaz ◽  
Joseph R. Smyth ◽  
Rhiana E. Henry ◽  
Charles R. Stern ◽  
Philip Persson ◽  
...  

ABSTRACT Gadolinite, REE2FeBe2Si2O10, is a monoclinic orthosilicate member of the gadolinite supergroup of minerals and occurs in beryllium and rare earth element (REE) bearing granites, pegmatites, and some metamorphic rocks. Gadolinite from the White Cloud pegmatite, South Platte Pegmatite district, Colorado, USA, has been investigated and shows unusually variable REE compositions and distinct Be-Si disorder. Crystal structure and chemistry of two petrographically distinct gadolinite samples from this locality have been studied by electron microprobe chemical analysis, laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS), single-crystal X-ray diffraction (XRD), and micro-Raman spectroscopy. Within these samples, the gadolinite was found to range from gadolinite-(Y) to gadolinite-(Ce). Regions of nearly full occupancy of Fe at the M site, and partial substitution of Si for Be at the Q tetrahedral site, as well as substitution of Be for Si at the T site were observed, with up to 15% vacancy at the Fe site and up to 15% disorder between Be and Si at distinct tetrahedral sites elsewhere. The layered nature of the crystal structure allows for large variation of the radius of the cation at the A site which contains the REE. This study shows that Be may substitute for Si and that Be may be more abundant in geochemical systems than previously assumed.


Sign in / Sign up

Export Citation Format

Share Document