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

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno

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.

2021 ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno

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.


2020 ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Alessandro Del Vecchio

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.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Alessandro Del Vecchio

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.


2018 ◽  
Vol 82 (1) ◽  
pp. 95-110 ◽  
Author(s):  
Daniela Novembre ◽  
Carla Pace ◽  
Domingo Gimeno

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.


2014 ◽  
Vol 78 (5) ◽  
pp. 1209-1225 ◽  
Author(s):  
D. Novembre ◽  
C. Pace ◽  
D. Gimeno

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.


2018 ◽  
Vol 82 (4) ◽  
pp. 961-973 ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Nicola d'Alessandro ◽  
Lucia Tonucci

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.


Author(s):  
Youssriah Yahia Sabri ◽  
Ikram Hamed Mahmoud ◽  
Lamis Tarek El-Gendy ◽  
Mohamed Raafat Abd El-Mageed ◽  
Sally Fouad Tadros

Abstract Background There are many causes of pleural disease including variable benign and malignant etiologies. DWI is a non-enhanced functional MRI technique that allows qualitative and quantitative characterization of tissues based on their water molecules diffusivity. The aim of this study was to evaluate the diagnostic value of DWI-MRI in detection and characterization of pleural diseases and its capability in differentiating benign from malignant pleural lesions. Results Conventional MRI was able to discriminate benign from malignant lesions by using morphological features (contour and thickness) with sensitivity 89.29%, specificity 76%, positive predictive value 89%, negative predictive value 76.92%, and accuracy 85.37%. ADC value as a quantitative parameter of DWI found that ADC values of malignant pleural diseases were significantly lower than that of benign lesions (P < 0.001). Hence, we discovered that using ADC mean value of 1.68 × 10-3 mm2/s as a cutoff value can differentiate malignant from benign pleural diseases with sensitivity 89.3%, specificity 100%, positive predictive value 100%, negative predictive value 81.2%, and accuracy 92.68% (P < 0.001). Conclusion Although DWI-MRI is unable to differentiate between malignant and benign pleural effusion, its combined morphological and functional information provide valid non-invasive method to accurately characterize pleural soft tissue diseases differentiating benign from malignant lesions with higher specificity and accuracy than conventional MRI.


2020 ◽  
Vol 35 (10) ◽  
pp. 2369-2377
Author(s):  
Helmar Wiltsche ◽  
Matthias Wolfgang

The MICAP is a microwave driven plasma source employing nitrogen as the plasma gas. In this work we compare LODs and LOQs obtained in axial viewing with those obtained by ICP-OES and evaluate the effect of air instead of nitrogen as the plasma gas.


2018 ◽  
Vol 82 (5) ◽  
pp. 1049-1055 ◽  
Author(s):  
Daniel Atencio ◽  
Marcelo B. Andrade ◽  
Luca Bindi ◽  
Paola Bonazzi ◽  
Matteo Zoppi ◽  
...  

ABSTRACTThis study presents a complete characterization of kenoplumbomicrolite, (Pb,□)2Ta2O6[□,(OH),O], occurring in an amazonite pegmatite from Ploskaya Mountain, Western Keivy Massif, Kola Peninsula, Murmanskaja Oblast, Northern Region, Russia.Kenoplumbomicrolite occurs in yellowish brown octahedral, cuboctahedral and massive crystals, up to 20 cm, has a white streak, a greasy lustre and is translucent. The Mohs hardness is ~6. Attempts to measure density (7.310–7.832 g/cm3) were affected by the ubiquitous presence of uraninite inclusions. Reflectance values were measured in air and immersed in oil. Kenoplumbocrolite is optically isotropic. The empirical formula is (Pb1.30□0.30Ca0.29Na0.08U0.03)Σ2.00(Ta0.82Nb0.62Si0.23Sn4+0.15Ti0.07Fe3+0.10Al0.01)Σ2.00O6[□0.52(OH)0.25O0.23]Σ1.00 (from the crystal used for the structural study) and (Pb1.33□0.66Mn0.01)Σ2.00(Ta0.87Nb0.72Sn4+0.18Fe3+0.11W0.08Ti0.04)Σ2.00O6[□0.80(OH)0.10O0.10]Σ1.00 (average including additional fragments). The mineral is cubic, space group Fd$\overline 3 $m. The unit-cell parameters refined from powder X-ray diffraction data are a = 10.575(2) Å and V = 1182.6(8) Å3, which are in accord with those obtained previously from a single crystal of a = 10.571(1) Å, V = 1181.3(2) Å3 and Z = 8. The mineral description and its name have been approved by the Commission on New Minerals, Nomenclature and Classification of the International Mineralogical Association (IMA2015-007a).


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