Quantitative X-ray diffraction of free, not chemically bound water with the PONKCS method

2018 ◽  
Vol 51 (6) ◽  
pp. 1535-1543 ◽  
Author(s):  
Sebastian Scherb ◽  
Nancy Beuntner ◽  
Karl-Christian Thienel ◽  
Jürgen Neubauer

The free water in calcined phyllosilicate–water mixtures exhibits a distinctly different behaviour in its X-ray amorphous scattering contribution as opposed to fly ash– or limestone powder–water mixtures. While fly ash and limestone powder yield a continuous increase in the scattering contribution when water is added, the scattering contribution stagnates for calcined phyllosilicates over a wide range of water addition. There is a direct correlation between the consistency of the sample and the X-ray amorphous scattering contribution caused by the water. The same correlation can also be found in in situ X-ray diffraction measurements of hydrating systems. As long as the sample has a pasty consistency, the scattering contribution of the water decreases with progressive reaction. After the transition from fresh paste to final set, there is no further reduction of the X-ray amorphous scattering contribution caused by the free water, which means that the free water cannot be quantified correctly from this point in time.

2016 ◽  
Vol 2016 ◽  
pp. 1-9
Author(s):  
Meijuan Rao ◽  
Wan Tang ◽  
Wei Zhou ◽  
Yaning Kong ◽  
Shuhua Liu

Cement-based materials were investigated by comparing the strength and microstructure of pastes and mortar containing limestone powder or low quality fly ash. The compressive strength of the mortar at 28 and 90 d was examined whose microstructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis, and differential thermal analysis (TG-DTA). The results indicated that the strength of mortar decreased with increasing mineral admixtures. The limestone powder mainly acted as inert filler and hardly took part in the chemical reaction. Low quality fly ash may accelerate the formation of hydration products in samples with more chemically bonded water. This further resulted in a higher degree of cement hydration and denser microstructure, while the overall heat of hydration was reduced. At the early stage of hydration, low quality fly ash can be considered as an inert material whereas its reactivity at the later stage became high, especially for ground low quality fly ash.


Materials ◽  
2020 ◽  
Vol 13 (2) ◽  
pp. 343 ◽  
Author(s):  
Dumitru Doru Burduhos Nergis ◽  
Mohd Mustafa Al Bakri Abdullah ◽  
Andrei Victor Sandu ◽  
Petrică Vizureanu

In this paper, the effect on thermal behavior and compounds mineralogy of replacing different percentages of fly ash with compact particles was studied. A total of 30% of fly ash was replaced with mass powder glass (PG), 70% with mass natural aggregates (S), and 85% with mass PG and S. According to this study, the obtained fly ash based geopolymer exhibits a 20% mass loss in the 25–300 °C temperature range due to the free or physically bound water removal. However, the mass loss is closely related to the particle percentage. Multiple endothermic peaks exhibit the dihydroxylation of β-FeOOH (goethite) at close to 320 °C, the Ca(OH)2 (Portlandite) transformation to CaCO3 (calcite) occurs at close to 490 °C, and Al(OH)3 decomposition occurs at close to 570 °C. Moreover, above 600 °C, the curves show only very small peaks which may correspond to Ti or Mg hydroxides decomposition. Also, the X-ray diffraction (XRD) pattern confirms the presence of sodalite after fly ash alkaline activation, whose content highly depends on the compact particles percentage. These results highlight the thermal stability of geopolymers in the 25–1000 °C temperature range through the use of thermogravimetric analysis, differential thermal analysis, and XRD.


Materials ◽  
2021 ◽  
Vol 14 (5) ◽  
pp. 1267
Author(s):  
David Längauer ◽  
Vladimír Čablík ◽  
Slavomír Hredzák ◽  
Anton Zubrik ◽  
Marek Matik ◽  
...  

Large amounts of coal combustion products (as solid products of thermal power plants) with different chemical and physical properties cause serious environmental problems. Even though coal fly ash is a coal combustion product, it has a wide range of applications (e.g., in construction, metallurgy, chemical production, reclamation etc.). One of its potential uses is in zeolitization to obtain a higher added value of the product. The aim of this paper is to produce a material with sufficient textural properties used, for example, for environmental purposes (an adsorbent) and/or storage material. In practice, the coal fly ash (No. 1 and No. 2) from Czech power plants was firstly characterized in detail (X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX), particle size measurement, and textural analysis), and then it was hydrothermally treated to synthetize zeolites. Different concentrations of NaOH, LiCl, Al2O3, and aqueous glass; different temperature effects (90–120 °C); and different process lengths (6–48 h) were studied. Furthermore, most of the experiments were supplemented with a crystallization phase that was run for 16 h at 50 °C. After qualitative product analysis (SEM-EDX, XRD, and textural analytics), quantitative XRD evaluation with an internal standard was used for zeolitization process evaluation. Sodalite (SOD), phillipsite (PHI), chabazite (CHA), faujasite-Na (FAU-Na), and faujasite-Ca (FAU-Ca) were obtained as the zeolite phases. The content of these zeolite phases ranged from 2.09 to 43.79%. The best conditions for the zeolite phase formation were as follows: 4 M NaOH, 4 mL 10% LiCl, liquid/solid ratio of 30:1, silica/alumina ratio change from 2:1 to 1:1, temperature of 120 °C, process time of 24 h, and a crystallization phase for 16 h at 50 °C.


Materials ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1786
Author(s):  
Carla Queirós ◽  
Chen Sun ◽  
Ana M. G. Silva ◽  
Baltazar de Castro ◽  
Juan Cabanillas-Gonzalez ◽  
...  

The development of straightforward reproducible methods for the preparation of new photoluminescent coordination polymers (CPs) is an important goal in luminescence and chemical sensing fields. Isophthalic acid derivatives have been reported for a wide range of applications, and in addition to their relatively low cost, have encouraged its use in the preparation of novel lanthanide-based coordination polymers (LnCPs). Considering that the photoluminescent properties of these CPs are highly dependent on the existence of water molecules in the crystal structure, our research efforts are now focused on the preparation of CP with the lowest water content possible, while considering a green chemistry approach. One- and two-dimensional (1D and 2D) LnCPs were prepared from 5-aminoisophthalic acid and Sm3+/Tb3+ using hydrothermal and/or microwave-assisted synthesis. The unprecedented LnCPs were characterized by single-crystal X-ray diffraction (SCRXD), powder X-ray diffraction (PXRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM), and their photoluminescence (PL) properties were studied in the solid state, at room temperature, using the CPs as powders and encapsulated in poly(methyl methacrylate (PMMA) films, envisaging the potential preparation of devices for sensing. The materials revealed interesting PL properties that depend on the dimensionality, metal ion, co-ligand used and water content.


2017 ◽  
Vol 866 ◽  
pp. 199-203
Author(s):  
Chidchanok Chainej ◽  
Suparut Narksitipan ◽  
Nittaya Jaitanong

The aims of this research were study the microstructures and mechanical properties for partial replacement of cement with Fly ash (FA) and kaolin waste (KW). Ordinary Portland cement were partially replaced with FA and KW in the range of 25-35% and 10-25% by weight of cement powder. The kaolin waste was ground for 180 minutes before using. The specimen was packing into an iron mold which sample size of 5×5×5 cm3. Then, the specimens were kept at room temperature for 24 hours and were moist cured in the incubation lime water bath at age of 3 days. After that the specimens were dry cured with plastic wrap at age of 3, 7, 14 and 28 days. After that the compounds were examined by x-ray diffraction patterns (XRD) and the microstructures were examined by scanning electron microscopy (SEM). The compressive strength was then investigated.


1987 ◽  
Vol 113 ◽  
Author(s):  
Scott Schlorholtz ◽  
Ken Bergeson ◽  
Turgut Demirel

ABSTRACTThe physical and chemical properties of fly ash produced at Ottumwa Generating Station have been monitored since April, 1985. The fly ash is produced from burning a low sulfur, sub-bituminous coal obtained from the Powder River Basin near Gillette, Wyoming. One-hundred and sixty samples of fly ash were obtained during the two year period. All of the samples were subjected to physical testing as specified by ASTM C 311. About one-hundred of the samples were also subjected to a series of tests designed to monitor the self-cementing properties of the fly ash. Many of the fly ash samples were subjected to x-ray diffraction and fluorescence analysis to define the mineralogical and chemical composition of the bulk fly ash as a function of sampling date. Hydration products in selected hardened fly ash pastes, were studied by x-ray diffraction and scanning electron microscopy. The studies indicated that power plant operating conditions influenced the compressive strength of the fly ash paste specimens. Mineralogical and morphological studies of the fly ash pastes indicated that stratlingite formation occurred in the highstrength specimens, while ettringite was the major hydration product evident in the low-strength specimens.


2021 ◽  
pp. 096739112199822
Author(s):  
Ahmed I Abou-Kandil ◽  
Gerhard Goldbeck

Studying the crystalline structure of uniaxially and biaxially drawn polyesters is of great importance due to their wide range of applications. In this study, we shed some light on the behaviour of PET and PEN under uniaxial stress using experimental and molecular modelling techniques. Comparing experiment with modelling provides insights into polymer crystallisation with extended chains. Experimental x-ray diffraction patterns are reproduced by means of models of chains sliding along the c-axis leading to some loss of three-dimensional order, i.e. moving away from the condition of perfect register of the fully extended chains in triclinic crystals of both PET and PEN. This will help us understand the mechanism of polymer crystallisation under uniaxial stress and the appearance of mesophases in some cases as discussed herein.


2012 ◽  
Vol 9 (4) ◽  
pp. 1788-1795 ◽  
Author(s):  
Olushola S. Ayanda ◽  
Olalekan S. Fatoki ◽  
Folahan A. Adekola ◽  
Bhekumusa J. Ximba

In this study, fly ash was obtained from Matla power station and the physicochemical properties investigated. The fly ash was characterized by x-ray fluorescence, x-ray diffraction, scanning electron microscopy, and inductively coupled plasma mass spectrometry. Surface area, particle size, ash and carbon contents, pH, and point of zero charge were also measured. The results showed that the fly ash is alkaline and consists mainly of mullite (Al6Si2O13) and quartz (SiO2). Highly toxic metals As, Sb, Cd, Cr, and Pb as well as metals that are essential to health in trace amounts were also present. The storage and disposal of coal fly ash can thus lead to the release of leached metals into soils, surface and ground waters, find way into the ecological systems and then cause harmful effect to man and its environments.


2021 ◽  
Vol 325 ◽  
pp. 181-187
Author(s):  
Martin Nguyen ◽  
Radomír Sokolář

This article examines the influence of fly ash on corrosion resistance of refractory forsterite-spinel ceramics by molten iron as a corrosive medium. Fly ash in comparison with alumina were used as raw materials and sources of aluminium oxide for synthesis of forsterite-spinel refractory ceramics. Raw materials were milled, mixed in different ratios into two sets of mixtures and sintered at 1550°C for 2 hours. Samples were characterized by X-ray diffraction analysis and thermal dilatometric analysis. Crucibles were then made from the fired ceramic mixtures and fired together with iron at its melting point of 1535°C for 5 hours. The corrosion resistance was evaluated by scanning electron microscopy on the transition zones between iron and ceramics. Mixtures with increased amount of spinel had higher corrosion resistance and mixtures with fly ash were comparable to mixtures with alumina in terms of corrosion resistance and refractory properties.


2021 ◽  
Vol 11 (5) ◽  
pp. 724-731
Author(s):  
Hemin Liu ◽  
Qian Huang ◽  
Liang Zhao

This study investigates the deterioration of concrete containing limestone powder exposed to sulfate solution under ambient temperature (20~25 °C). Microstructure and mineral phases within the attacked concrete were measured by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD). It was found that the addition of limestone powder increased the initial porosity of concrete. Consequently, a larger amount of SO2–4 ions diffused into the concrete containing limestone powder, and their degree of deterioration caused by sulfate attack increased with the increase in limestone powder content. At ambient temperature, gypsum and ettringite were the major attack products, respectively within the surface and nearsurface portions of concrete containing limestone powder, which was consistent with the products of sulfate attack within concrete without limestone powder. Therefore, the type and distribution of the attack products in concrete had not been revised due to the addition of limestone powder. Nevertheless, the adverse influence of limestone powder on the sulfate resistance of concrete, even at ambient temperature, should be considered. Furthermore, effective measures should be implemented to improve the durability of concrete containing limestone powder in this environment.


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