scholarly journals Luminescence reveals variations in local structural order of calcium carbonate polymorphs formed by different mechanisms

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Michael B. Toffolo ◽  
Giulia Ricci ◽  
Luisa Caneve ◽  
Ifat Kaplan-Ashiri
Keyword(s):  
Infrared Spectroscopy ◽  
Calcium Carbonate ◽  
Construction Materials ◽  
Reference Database ◽  
Formation Processes ◽  
X Ray Diffraction ◽  
Structural Order ◽  
Lime Plaster ◽  
Calcium Carbonate Polymorphs

Abstract In nature, calcium carbonate (CaCO3) in the form of calcite and aragonite nucleates through different pathways including geogenic and biogenic processes. It may also occur as pyrogenic lime plaster and laboratory-precipitated crystals. All of these formation processes are conducive to different degrees of local structural order in CaCO3 crystals, with the pyrogenic and precipitated forms being the least ordered. These variations affect the manner in which crystals interact with electromagnetic radiation, and thus formation processes may be tracked using methods such as X-ray diffraction and infrared spectroscopy. Here we show that defects in the crystal structure of CaCO3 may be detected by looking at the luminescence of crystals. Using cathodoluminescence by scanning electron microscopy (SEM-CL) and laser-induced fluorescence (LIF), it is possible to discern different polymorphs and their mechanism of formation. We were thus able to determine that pyrogenic calcite and aragonite exhibit blue luminescence due to the incorporation of distortions in the crystal lattice caused by heat and rapid precipitation, in agreement with infrared spectroscopy assessments of local structural order. These results provide the first detailed reference database of SEM-CL and LIF spectra of CaCO3 standards, and find application in the characterization of optical, archaeological and construction materials.

Synthesis and Characterization of Dumbbell Shaped Calcium Carbonate Induced by Lignin

2010 ◽  
Vol 658 ◽  
pp. 49-52 ◽  
Author(s):  
Wen Kun Zhu ◽  
Xue Gang Luo ◽  
An Kai Luo ◽  
Xuan Liang
Keyword(s):  
Infrared Spectroscopy ◽  
Calcium Carbonate ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis Mechanism ◽  
Ft Ir ◽  
Ir Analysis ◽  
Decomposition Behavior ◽  
Normal Calcium

Calcium carbonate with various structures and morphologies were prepared under double injection of the CaCl2 and Na2CO3 solutions with molar ratio of 1:1 at 30 °C, taking lignin as the induction agents. They were characterized by scanning electron microscopy, infrared spectroscopy thermal analysis and X-ray diffraction. The synthesis mechanism was also discussed. The results showed that calcium carbonate of different shape were obtained with the concentration of lignin at 10g/L, 20g/L and 30g/L, respectively, under 30°C while CaCl2 and Na2CO3 were kept at the same concentration of 0.5mol/L. The size of the particles was in a range between 3 and 5μm and the particles were calcites. Compared with the normal calcium carbonate, the compound has advanced thermal decomposition behavior. Fourier transform infrared spectroscopy (FT-IR) analysis revealed the presence of lignin and calcite. The electrostatic interaction of Ca2+ with lignin and the complementary of stereo-structure play important roles in the formation of Dumbbell Shaped Calcium Carbonate.

Characterization of the Snail’s Carapace Collected at Coast of Brazilian’s State of Paraíba

2008 ◽  
Vol 396-398 ◽  
pp. 141-144
Author(s):  
R.S.C. Lima ◽  
Marcus Vinícius Lia Fook ◽  
Thiago Bizerra Fideles ◽  
A.C.B.M. Fook ◽  
Sara Verusca de Oliveira ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Infrared Spectroscopy ◽  
Calcium Carbonate ◽  
Brazilian Coast ◽  
Economic Potential ◽  
X Ray Diffraction ◽  
X Ray ◽  
Marine Snails ◽  
Northern Brazil

Calcium carbonate (CaCO3) is a ceramic of strong economic potential, given the versatility of its application in industry in many different areas. Protective shells of marine snails of the Brazilian coast were analyzed in this study, to verify the content of calcium carbonate available in this type of material. The samples were collected at Bessa´s Beach located in the João Pessoa’ coast Capital of Paraíba state, northern Brazil. The collection occurred during the month of February 2008; the sample was processed into powder and it was examined by X-ray Fluorescence (XRF), X-ray diffraction (XRD) and Infrared Spectroscopy with Fourier Trasformating (FTIR). The material was also submitted to heat treatment at 110°C and characterized by same techniques. The results confirmed the presence of a high content of calcium carbonate in the samples (over 95%,) which has not changed with the heat treatment used. It was presents the morphologies calcite and aragonite with prevalence of the second, both showing high levels of crystallinity. From the results obtained, calcium carbonate of the coast Paraíba has a potential application like bioceramic.

Stability of sodalite relative to nepheline in NaCl–H2O brines at 750 °C: Implications for hydrothermal formation of sodalite

2020 ◽  
Vol 58 (1) ◽  
pp. 3-18 ◽  
Author(s):  
Jonathan B. Schneider ◽  
David M. Jenkins
Keyword(s):  
Infrared Spectroscopy ◽  
Constant Temperature ◽  
Molar Ratio ◽  
Standard State ◽  
X Ray Diffraction ◽  
Cage Structure ◽  
X Ray ◽  
Brine Concentration

ABSTRACT Formation of the feldspathoid sodalite (Na6Al6Si6O24·2NaCl) by reaction of nepheline (NaAlSiO4) with NaCl-bearing brines was investigated at 3 and 6 kbar and at a constant temperature of 750 °C to determine the brine concentration at which sodalite forms with variation in pressure. The reaction boundary was located by reaction-reversal experiments in the system NaAlSiO4–NaCl–H2O at a brine concentration of 0.16 ± 0.08 XNaCl [= molar ratio NaCl/(NaCl + H2O)] at 3 kbar and at a brine concentration of 0.35 ± 0.03 XNaCl at 6 kbar. Characterization of the sodalite using both X-ray diffraction and infrared spectroscopy after treatment in these brines indicated no obvious evidence of water or hydroxyl incorporation into the cage structure of sodalite. The data from this study were combined with earlier results by Wellman (1970) and Sharp et al. (1989) at lower (1–1.5 kbar) and higher (7–8 kbar) pressures, respectively, on sodalite formation from nepheline and NaCl which models as a concave-down curve in XNaCl – P space. In general, sodalite buffers the concentration of neutral aqueous NaCl° in the brine to relatively low values at P < 4 kbar, but NaCl° increases rapidly at higher pressures. Thermochemical modeling of these data was done to determine the activity of the aqueous NaCl° relative to a 1 molal (m) standard state, demonstrating very low activities (<0.2 m, or 1.2 wt.%) of NaCl° at 3 kbar and lower, but rising to relatively high activities (>20 m, or 54 wt.%) of NaCl° at 6 kbar or higher. The results from this study place constraints on the concentration of NaCl° in brines coexisting with nepheline and sodalite and, because of the relative insensitivity of this reaction to temperature, can provide a convenient geobarometer for those localities where the fluid compositions that formed nepheline and sodalite can be determined independently.

X-Ray Diffraction Analysis of the Calcium Carbonate Polymorphs

1970 ◽  
Vol 14 ◽  
pp. 29-37 ◽  
Author(s):  
S. T. Silk ◽  
S. Z. Lewin
Keyword(s):  
Calcium Carbonate ◽  
Size Distributions ◽  
X Ray Diffraction ◽  
Particle Size Distributions ◽  
Ray Method ◽  
X Ray ◽  
Packing Efficiency ◽  
Integrated Intensities ◽  
Packing Effect ◽  
Calcium Carbonate Polymorphs

AbstractIt is shown that the integrated intensities of diffraction lines from calcite and aragonite powders prepared by precipitation vary markedly, due to variations in sample packing efficiency arising from different degrees of polydispersity in the particle size distributions. Since prolonged grinding to equalize initially divergent distributions changes the polymorph composition, the packing effect imposes the principal limitation on the precision of the x-ray method for certain types of calcium carbonate preparations.

Characterization of a new Ca–Cd hydroxide hydrothermally synthesized and its implications for cement isolation of Cd

1998 ◽  
Vol 13 (1) ◽  
pp. 16-21 ◽  
Author(s):  
S. Gñni ◽  
A. Macías ◽  
J. Madrid ◽  
J. M. Díez
Keyword(s):  
Infrared Spectroscopy ◽  
Pore Solution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Predominant Species ◽  
Solubility Constant ◽  
Tg And Dtg ◽  
Low Solubility ◽  
Mechanism Of The Reaction

Mixtures of CaO–CdO (1 : 1) were hydrothermally treated in a pressure reactor at 200 °C and 200 psi of pressure during a period of 16 h. The evolution of the reaction was followed by x-ray diffraction (XRD), infrared spectroscopy (IR), and thermogravimetric (TG and DTG) analysis. Also, the composition of the filtered solutions was analyzed to determine the mechanism of the reaction as well as the thermodynamic solubility constant of the new compound formed. The results show that CaO and CdO react, giving rise to a new CaCd(OH)4 hydroxide whose thermodynamic solubility constant, 1.5 ± 0.4 × 10−11 M2, is six orders of magnitude lower than those of both Ca(OH) 2 and β–Cd(OH) 2. This low solubility constant justifies the Cd2+ concentration measured in the pore solution of cement matrices used to immobilize cadmium containing wastes. The mechanism of the reaction proposed is via dissolution of both Ca(OH) 2 and β–Cd(OH)2, Ca2+ and being the predominant species in solution.

Preparation and characterization of poly(tetramethyl-p-phenylenediamine)/clay hybrids via intercalative polymerization

2003 ◽  
Vol 18 (2) ◽  
pp. 482-486 ◽  
Author(s):  
Guangming Chen ◽  
Nobuo Iyi ◽  
Taketoshi Fujita
Keyword(s):  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Thermal Behavior ◽  
Fourier Transform Infrared Spectroscopy ◽  
Interlayer Space ◽  
X Ray Diffraction ◽  
X Ray ◽  
Noncovalent Bonding ◽  
Intercalative Polymerization

New noncovalent bonding polymer/clay hybrids were prepared, including the polymer poly(tetramethyl-p-phenylenediamine) (poly-TMPD). Polymerization occurred in the interlayer space of clay mineral successively after intercalation of monomers. Two types of clay minerals with different surface properties—a hydrophilic lithium fluorotaeniolite (TN) and four kinds of organophilic fluorotaeniolites (org-TNs)—were used as the hosts. Powder x-ray diffraction results showed an increase of 0.7–1.0 nm in the basal spacings, indicating the formation of poly–TMPD in the interlayer space of the hosts. Intercalative polymerization was also supported by Fourier transform infrared spectroscopy. The orientation of the poly-TMPD and thermal behavior were also discussed.

Characterization of Three 'Active' Rhodium(III) Hydroxides

1995 ◽  
Vol 48 (3) ◽  
pp. 557 ◽  
Author(s):  
SJ Crimp ◽  
L Spiccia
Keyword(s):  
Thermal Analysis ◽  
Thermal Decomposition ◽  
Infrared Spectroscopy ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
X Ray

Pure solutions of [ Rh (H2O)6]3+, dimer [Rh2(μ-OH)2(H2O)8]4+ and trimer [Rh3(μ-OH)4(H2O)10]5+ have been converted into their respective 'active' hydroxides by dropwise addition to an imidazole solution. These 'active' hydroxides have been analysed by a variety of techniques including rhodium determination, infrared spectroscopy, thermal analysis and powder X-ray diffraction. Purity determinations using ion-exchange chromatography showed that the three hydroxides consist primarily of the neutral forms of the starting aqua ion (>96%) with small amounts of species with higher nuclearity. Rhodium analysis and thermogravimetric measurements confirmed the composition of these hydroxides to be Rh (OH)3(H2O)3.H2O, Rh2(μ-OH)2(OH)4(H2O)4 and Rh3(μ-OH)4(OH)5(H2O)5.5H2O. A scheme for the thermal decomposition of each of the hydroxides has been proposed on the basis of the t.g . and d.t.a . data and the knowledge that the final product in each case is α-Rh2O3. Heating of the hydroxides in air resulted in oxidation of RhIII to RhIV (temperature 250-300°C) forming RhO2 which on further heating decomposed to α-Rh2O3 and dioxygen.

Characterization of Cellulose/Calcium Carbonate Biocomposite Film

2016 ◽  
Vol 675-676 ◽  
pp. 209-212 ◽  
Author(s):  
Wichian Siriprom ◽  
Nirun Witit-Anun ◽  
Auttapol Choeysuppaket ◽  
T. Ratana
Keyword(s):  
Calcium Carbonate ◽  
Composite Film ◽  
X Ray Diffraction ◽  
X Ray ◽  
Film Forming ◽  
Ft Ir ◽  
Good Biocompatibility ◽  
Biocomposite Film ◽  
Calcium Carbonate Particle

In this study were to explore the properties of interaction between cellulose and calcium carbonate particle (CaCO3) which derive from Papia Undulates Shell in procedure of biocomposite synthesis. The structural properties of cellulose powder Papia Undulates Shell and cellulose-calcium carbonate composite film were investigated by using X-ray Diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) and the compositions of cellulose/CaCO3 biocomposite film were studied by Energy Dispersive X-ray Fluorescence (EDXRF). The experimental results demonstrated the morphology of Papia Undulates Shell were crystalline aragonite phase and the cellulose have structural as amorphous-crystalline but after film forming the composite film between cellulose and Papia Undulates Shell also have amorphous structural. The result of FTIR used to confirmed the formation of bonding between molecular, it indicated that the cellulose/CacO3 biocomposite film had good biocompatibility due to the biocomposite film have both characteristic feature of CO3-2 group (~874 cm-1 and ~713 cm-1) and the glucose of cellulose at ~1635, ~1064 and ~946 cm-1. Another that, the result from EDXRF shown the chemical composition of organic compound of cellulose/CaCO3 biocomposite film was highest with 99.437 while the Papia Undulates Shell have 0.341 Wt% with corresponding with the ratio of filler material which mixture as 1%. So that, the cellulose/calcium carbonate bicomposite film could be candidate for biocomposite film application.

Synthesis and Structural Characterization of a Series of Group 11 2,2-Dialkyl-1,3-dicyclohexylguanidinate Complexes

2014 ◽  
Vol 67 (7) ◽  
pp. 1021 ◽  
Author(s):  
Sonya K. Adas ◽  
Jesus A. Ocana ◽  
Scott D. Bunge
Keyword(s):  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
7Li Nmr ◽  
Elemental Analyses ◽  
Lithium Diethylamide ◽  
Structural Aspects

The addition of either lithium dimethylamide or lithium diethylamide to a tetrahydrofuran (THF) solution of 1,3-dicyclohexylcarbodiimide yielded THF adducts of lithium 2,2-dimethyl-1,3-dicyclohexylguandidinate (1) and lithium 2,2-diethyl-1,3-dicyclohexylguandidinate (2), respectively. One equivalent of either 1 or 2 was subsequently reacted with one equivalent of Group 11 halide (CuCl, AgBr, and AuCl) to generate oligonuclear complexes with the general formula {M[CyNC(NR2)NCy]}n where M, R, and n are respectively Cu, CH3, 2 (3); Cu, CH2CH3, 2 (4); Ag, CH3, 3 (5); Ag, CH2CH3, 3 (6); Au, CH3, 2 (7); and Au, CH2CH3, 2 (8). Compounds 1–8 were characterized by single-crystal X-ray diffraction. The bulk powders for all complexes were found to be in agreement with the crystal structures based on elemental analyses, Fourier transform infrared spectroscopy, and 1H, 13C, and 7Li NMR studies. The unique structural aspects of this family of Group 11 complexes are highlighted.

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