Synthesis and Characterization of Analcime (ANA) Zeolite using a Kaolinitic Rock

Experimental Conditions ◽

Economic Point ◽

Synthesis Conditions ◽

Cell Parameters ◽

Synthesis Protocol

Abstract Analcime is nowadays an important component in dental porcelain sysytems, in heterogeneous catalysis, in the nanoelectronic field, in selective adsorption and in stomatology. Analcime synthesis from a kaolinite rock coming from Romana (Sassari, Italy) is here presented. A synthesis protocol is proposed that aims to make an improvement of synthesis conditions compared to the past. The hydrothermal treatment is in fact here achieved without aging times and without the use of sodium silicate, as reported in the literature. Lower calcination temperature, synthesis temperatures and crystallization times are verified in this work. The kaolin is subjected to calcination at the temperature of 650°C and then mixed with NaOH. The experiment is performed at ambient pressure and 170 ± 0.1°C. The degree of purity of Analcime is calculated in 97,57 % at 10h. Analcime is characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, inductively coupled plasma optical emission spectrometry and thermal analysis. Density is also calculated. Cell parameters and the amount of amorphous phase in the synthesis powders is estimated with quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. The experimental conditions make the synthesis protocol particularly attractive from an economic point of view. Both chemical and physical characterization of Analcime is satisfactory making the experimental protocol very promising for an industrial transfer.

Synthesis and characterization of analcime (ANA) zeolite using a kaolinitic rock

Scientific Reports ◽

10.1038/s41598-021-92862-0 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Daniela Novembre ◽

Domingo Gimeno

Keyword(s):

Ambient Pressure ◽

Added Value ◽

Emission Spectrometry ◽

Crystallization Time ◽

Experimental Protocol ◽

Economic Point ◽

Cell Parameters ◽

Synthesis Protocol

AbstractAnalcime is nowadays an important component in dental porcelain systems, in heterogeneous catalysis, in the nanoelectronic field, in selective adsorption and in stomatology (dental filling and prosthesis). Analcime synthesis from an impure, silica-rich kaolinite rock coming from Romana (Sassari, Italy) is here presented. A synthesis protocol is proposed that aims to make an improvement of synthesis conditions compared to the past. The hydrothermal treatment is in fact here achieved without aging times and without the use of sodium silicate or other additional silica source reported in the literature. Lower calcination temperature, synthesis temperature and crystallization time are verified in this work. The kaolin is subjected to calcination at the temperature of 650 °C and then mixed with NaOH. The experiment is performed at ambient pressure and 170 ± 0.1 °C. The degree of purity of analcime is calculated in 97.57% at 10 h. Analcime is characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, inductively coupled plasma optical emission spectrometry and thermal analysis. Density is also calculated. Cell parameters and the amount of amorphous phase in the synthesis powders is estimated with quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. The experimental conditions make the synthesis protocol particularly attractive from an economic point of view. Also this work does not use a commercial kaolin but silica-rich impure kaolinitic rock from a disused quarry. This further reduces the costs of the experimental protocol. It also gives the protocol an added value, as the synthesis of a useful mineral is obtained through the valorization of an otherwise unused georesource. Both chemical and physical characterization of analcime is satisfactory making the experimental protocol very promising for an industrial transfer.

Synthesis and characterization of Na-P1 (GIS) zeolite using a kaolinitic rock

10.21203/rs.3.rs-111813/v1 ◽

2020 ◽

Author(s):

Daniela Novembre ◽

Domingo Gimeno ◽

Alessandro Del Vecchio

Keyword(s):

Rietveld Method ◽

Ambient Pressure ◽

Optical Emission ◽

Emission Spectrometry ◽

X Ray Diffraction ◽

X Ray ◽

Cell Parameters ◽

Inductively Coupled

Abstract This work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 ° and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods.The results make the experimental protocol very promising for an industrial transfer.

Synthesis and characterization of Na-P1 (GIS) zeolite using a kaolinitic rock

Scientific Reports ◽

10.1038/s41598-021-84383-7 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Daniela Novembre ◽

Domingo Gimeno ◽

Alessandro Del Vecchio

Keyword(s):

Rietveld Method ◽

Ambient Pressure ◽

Optical Emission ◽

Emission Spectrometry ◽

X Ray Diffraction ◽

X Ray ◽

Cell Parameters ◽

Inductively Coupled

AbstractThis work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. The results make the experimental protocol very promising for an industrial transfer.

Preparation and Characterization of New Molybdenum Nitride or Oxynitride Phases

MRS Proceedings ◽

10.1557/proc-368-15 ◽

1994 ◽

Vol 368 ◽

Cited By ~ 3

Author(s):

Roger J. Marchand ◽

X. Gouin ◽

F. Tessier ◽

Y. Laurent

Keyword(s):

Surface Area ◽

Structure Type ◽

Molybdenum Sulfide ◽

Fine Tuning ◽

Material Surface ◽

Molybdenum Nitride ◽

Initial Surface ◽

Experimental Conditions ◽

Synthesis Conditions

ABSTRACTSeveral methods of synthesizing molybdenum nitride or oxynitride fine powders are presented.We have prepared a γ-Mo2N type oxynitride phase by reacting ammonia with MoO3. The surface area and morphology of the oxynitride powders depend on the synthesis conditions. Characterization of the solids by elemental analysis, X-ray and neutron diffraction, and thermogravimetric analysis shows dramatic modification of the stoichiometry of conventional Mo2N nitride. Aging at room temperature under air results in decreasing the material surface area. The initial surface area can be recovered be fine tuning of experimental conditions. MoCl5 and Ca3N2 are reacted in a molten CaCl2 medium leading to a new Mo2N structure type.The reaction between molybdenum sulfide and NH3 produces two different phases depending on the reaction conditions. They are structurally related to δ-MoN.

Synthesis and characterization of wollastonite-2Mby using a diatomite precursor

10.1180/minmag.2017.081.025 ◽

2018 ◽

Vol 82 (1) ◽

pp. 95-110 ◽

Cited By ~ 5

Author(s):

Daniela Novembre ◽

Carla Pace ◽

Domingo Gimeno

Keyword(s):

Solid Phase ◽

Ambient Pressure ◽

Solid Phase Reaction ◽

Phase Reaction ◽

Chemical Treatments ◽

Natural Rock ◽

Reactive Silica ◽

Data Estimation

ABSTRACTSolid phase reaction synthesis of wollastonite-2Mby a natural rock precursor as the source of amorphous silica and CaCO3is reported. Chemical treatments were carried out on a diatomitic rock from Crotone (Calabria, Italy) in order to measure its reactive silica and CaCO3contents. Four series of synthesis were performed at 1000°C at ambient pressure by mixing, at different stoichiometry, the diatomitic rock with a natural limestone as a source of additive CaCO3, and sodium carbonate (Na2CO3) as triggering agent.Wollastonite-2Mwas characterized by chemo-physical, crystallographical and morphological-microtextural analyses. All these characterizations, together with infrared and nuclear magnetic resonance (29Si) responses provide values comparable to literature data. Estimation of the amorphous phase in the synthesis powders was performed through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods, resulting in a final product of 96.3% wollastonite-2M.

Syntheses and characterization of zeolites K-F and W type using a diatomite precursor

10.1180/minmag.2014.078.5.08 ◽

2014 ◽

Vol 78 (5) ◽

pp. 1209-1225 ◽

Cited By ~ 11

Author(s):

D. Novembre ◽

C. Pace ◽

D. Gimeno

Keyword(s):

Potassium Hydroxide ◽

Rietveld Method ◽

Morphological Characterization ◽

Raw Material ◽

Cell Parameters ◽

Chemical Treatments ◽

Natural Rock

AbstractZeolites K-F and W (EDI and MER types) were synthesized hydrothermally using a natural rock as raw material. Chemical treatments were carried out on a diatomitic rock (containing opaline silica) from Crotone (Calabria, Italy) in order to separate/obtain potassium silicate, a reagent necessary for synthesizing zeolites. Synthesis experiments were performed by mixing the obtained siliceous solution with potassium hydroxide and alumina in varying proportions at 150°C and room pressure. Four synthesis series were performed to form zeolite K-F (EDI) and zeolite W (MER).The chemical-physical and morphological characterization of the zeolite phases were carried out. Cell parameters were calculated using the Rietveld method. Infrared, thermal and nuclear magnetic resonance (29Si) experiments confirmed the high quality of the zeolite products. The amorphous phase in the synthesis powders was estimated with quantitative phase analysis using the combined Rietveld and reference intensity ratio methods.

Hydrothermal synthesis and characterization of kalsilite by using a kaolinitic rock from Sardinia, Italy, and its application in the production of biodiesel

10.1180/minmag.2017.081.080 ◽

2018 ◽

Vol 82 (4) ◽

pp. 961-973 ◽

Cited By ~ 2

Author(s):

Daniela Novembre ◽

Domingo Gimeno ◽

Nicola d'Alessandro ◽

Lucia Tonucci

Keyword(s):

Hydrothermal Synthesis ◽

Metastable Phase ◽

Synthesis Method ◽

Optical Emission ◽

Emission Spectrometry ◽

Cell Parameters ◽

Inductively Coupled ◽

Biodiesel Synthesis

ABSTRACTThe present work deals with the synthesis of kalsilite using material from a kaolinitic rock outcrop in Romana, Sassary Province, Sardinia, Italy.The hydrothermal synthesis method required the dissolution of kaolin and Al(OH)3 in a KOH solution at a temperature of 190°C and 1.013 bar. Crystallization of kalsilite was confirmed at 12 h in association with kaliophilite H2 as a metastable phase.The products of synthesis were fully characterized by powder X-ray diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry, infrared spectroscopy and 29Si nuclear magnetic resonance. The amorphous phase in the synthesis powders was estimated with quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. Cell parameters and density were also calculated for the kalsilite. A potential application of kalsilite was investigated as a heterogeneous catalyst for biodiesel synthesis from sunflower oil used for frying.

PREPARATION AND CHARACTERIZATION OF TlBa2Ca2Cu3Oy WITH A DIFFERENT MAXIMUM Tc

International Journal of Modern Physics B ◽

10.1142/s0217979207044263 ◽

2007 ◽

Vol 21 (18n19) ◽

pp. 3230-3232

Author(s):

S. MIKUSU ◽

S. TAKAMI ◽

K. TOKIWA ◽

K. TAKEUCHI ◽

A. IYO ◽

...

Keyword(s):

Crystal Structure ◽

Neutron Diffraction ◽

Thermoelectric Power ◽

Ambient Pressure ◽

X Ray Diffraction ◽

Key Factors ◽

X Ray ◽

Synthesis Conditions ◽

Drastic Increase

We have succeeded to prepare Tl -1223 samples with a maximum Tc above 130K at ambient pressure using a conventional sealed quartz tube method. We found that, by adequately controlling the starting composition, it is possible to control the maximum Tc from ~120K to 130K. In order to seek the key factors for a drastic increase in the Tc, we carried out the measurements of the thermoelectric power, powder X-ray diffraction and neutron diffraction for these samples. As a result, it is found that the characteristics in the Tl -1223 samples with high Tc show essentially similar to those in the Hg -1223 with the highest Tc and are different from those in the Tl -1223 samples with low Tc. The details of the synthesis conditions, the transport properties and the refinements of the crystal structure will be presented.

Characterization and identification of mixed-metal phosphates in soils: the application of Raman spectroscopy

10.1180/0026461036760166 ◽

2003 ◽

Vol 67 (6) ◽

pp. 1299-1316 ◽

Cited By ~ 25

Author(s):

A. M. Lanfranco ◽

P. F. Schofield ◽

P. J. Murphy ◽

M. E. Hodson ◽

J. F. W. Mosselmans ◽

...

Keyword(s):

Raman Spectroscopy ◽

Emission Spectrometry ◽

X Ray Diffraction ◽

Plasma Atomic Emission Spectrometry ◽

X Ray ◽

Mixed Metal ◽

Synthesis Conditions ◽

Metal Phosphates ◽

Cell Parameters

AbstractThe development of protocols for the identification of metal phosphates in phosphate-treated, metalcontaminated soils is a necessary yet problematical step in the validation of remediation schemes involving immobilization of metals as phosphate phases. The potential for Raman spectroscopy to be applied to the identification of these phosphates in soils has yet to be fully explored. With this in mind, a range of synthetic mixed-metal hydroxylapatites has been characterized and added to soils at known concentrations for analysis using both bulk X-ray powder diffraction (XRD) and Raman spectroscopy.Mixed-metal hydroxylapatites in the binary series Ca –Cd, Ca –Pb, Ca –Sr and Cd –Pb synthesized in the presence of acetate and carbonate ions, were characterized using a range of analytical techniques including XRD, analytical scanning electron microscopy (SEM), infrared spectroscopy (IR), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and Raman spectroscopy. Only the Ca –Cd series displays complete solid solution, although under the synthesis conditions of this study the Cd5(PO4)3OH end member could not be synthesized as a pure phase. Within the Ca –Cd series the cell parameters, IR active modes and Raman active bands vary linearly as a function of Cd content. X-ray diffraction and extended X-ray absorption fine structure spectroscopy (EXAFS) suggest that the Cd is distributed across both the Ca(1) and Ca(2) sites, even at low Cd concentrations.In order to explore the likely detection limits for mixed-metal phosphates in soils for XRD and Raman spectroscopy, soils doped with mixed-metal hydroxylapatites at concentrations of 5, 1 and 0.5 wt.% were then studied. X-ray diffraction could not confirm unambiguously the presence or identity of mixed-metal phosphates in soils at concentrations below 5 wt.%. Raman spectroscopy proved a far more sensitive method for the identification of mixed-metal hydroxylapatites in soils, which could positively identify the presence of such phases in soils at all the dopant concentrations used in this study. Moreover, Raman spectroscopy could also provide an accurate assessment of the degree of chemical substitution in the hydroxylapatites even when present in soils at concentrations as low as 0.1%.

Adsorption Studies on Magnetic Nanoparticles Functionalized with Silver to Remove Nitrates from Waters

Water ◽

10.3390/w13131757 ◽

2021 ◽

Vol 13 (13) ◽

pp. 1757

Author(s):

Yesica Vicente-Martínez ◽

Manuel Caravaca ◽

Antonio Soto-Meca ◽

Miguel Ángel Martín-Pereira ◽

María del Carmen García-Onsurbe

Keyword(s):

Magnetic Nanoparticles ◽

Nitrate Content ◽

Adsorption Efficiency ◽

Experimental Conditions ◽

Dependent Behavior ◽

Before And After ◽

Naoh Solution ◽

High Concentrations ◽

Interference Studies

This paper presents a novel procedure for the treatment of contaminated water with high concentrations of nitrates, which are considered as one of the main causes of the eutrophication phenomena. For this purpose, magnetic nanoparticles functionalized with silver (Fe3O4@AgNPs) were synthesized and used as an adsorbent of nitrates. Experimental conditions, including the pH, adsorbent and adsorbate dose, temperature and contact time, were analyzed to obtain the highest adsorption efficiency for different concentration of nitrates in water. A maximum removal efficiency of 100% was reached for 2, 5, 10 and 50 mg/L of nitrate at pH = 5, room temperature, and 50, 100, 250 and 500 µL of Fe3O4@AgNPs, respectively. The characterization of the adsorbent, before and after adsorption, was performed by energy dispersive X-ray spectroscopy, scanning electron microscopy, Brunauer-Emmett-Teller analysis and Fourier-transform infrared spectroscopy. Nitrates can be desorbed, and the adsorbent can be reused using 500 µL of NaOH solution 0.01 M, remaining unchanged for the first three cycles, and exhibiting 90% adsorption efficiency after three regenerations. A deep study on equilibrium isotherms reveals a pH-dependent behavior, characterized by Langmuir and Freundlich models at pH = 5 and pH = 1, respectively. Thermodynamic studies were consistent with physicochemical adsorption for all experiments but showed a change from endothermic to exothermic behavior as the temperature increases. Interference studies of other ions commonly present in water were carried out, enabling this procedure as very selective for nitrate ions. In addition, the method was applied to real samples of seawater, showing its ability to eliminate the total nitrate content in eutrophized waters.