Protocol for Analytical Techniques and Identification of Reusable Silica from Acid Oxidative Purification

Fluid catalytic cracking is one of the major secondary conversion process in petroleum refinery. Nowadays, the spent fluid catalytic cracking catalysts (FCCCs) are disposed of in landfill or stocked for a long period. Environmental risks and lack of space suggest that the management of FCCCs needs to be reviewed. The FCC catalysts contain about 3-3.5 %wt. of rare earth (RE) oxides; rare earth elements (REEs) are important for stabilization of the matrix of FCC catalysts. The main challenge is to develop an efficient process based on recovery of REEs and reuse of the solid leaching residue for some applications. In this paper a new process is proposed to recover cerium and lanthanum from FCCCs combined with reuse of the leaching solid residue for the production of synthetic zeolites. Three different zeolites were synthesized by using the solid residues from hydrochloric, nitric and sulfuric acid leaching. The chemical and physical properties of zeolites were characterized by different spectroscopic techniques including Scanning Electron Microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS) for evaluating the surface morphology. The X-Ray Diffraction (XRD), the Brunauer–Emmett–Teller (BET) and Infrared Spectroscopy (FT-IR) analyses were used to characterize the structure of such zeolites. In addition, the X-ray Fluorescence (XRF) was used to identify the chemical composition. Zeolite is a solid porous material widely used as adsorbent in different processes, particularly applied to wastewater treatments. In this paper, adsorption of heavy metals onto zeolites were investigated by Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES). The best results in terms of metal removal were achieved by the zeolite synthesized from the sulfuric acid leaching residue.

Molecular and Structural Changes in Induced-Brain Stroke Tissue Using FTIR Imaging Spectroscopy, Scanning Electron and Atomic Force Microscopy

Magnetic nanoparticle-supported molybdate sulfuric acid (MNPs-MSA) was synthesized and characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectroscopy (EDX), and scanning electron microscopy (SEM). The catalytic activity of MNPs-MSA was investigated as a recoverable catalyst for the one-pot synthesis of novel 2-substituted aryl (amino) and aryl (indolyl) kojic acid derivatives from the reaction of aldehydes with aniline or indole and kojic acid in high yield at room temperature under solvent-free conditions Abstract should briefly state the purpose of the research, the principal results, and the major conclusions of the study.

In the present study, nano zeolite A (LTA) was synthesized by the alkaline fusion method without adding an organic template. Effect of temperature and aging time were studied on the crystallinity and morphology of the final product. The synthesized LTA was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC) and N2 adsorption/desorption technique. The prepared nano LTA zeolite was applied to the water softening process. The main effects and interaction of factors such as pH, the amount of LTA, initial total hardness, temperature and contact time were investigated by response surface methodology (RSM). The obtained optimum values of factors were applied to hard water to remove Ca2+ and Mg2+ ions. Pseudo-first and second-order models were applied to kinetic and rate data. It was found that the adsorption rate follows the pseudo-second-order kinetic model.

Cow urine is known for possessing therapeutic potency which is found to vary depending upon its physical forms such as fresh sterile urine, distillate, lyophilized powder, etc. In the current work, we demonstrate the physicochemical characteristics and cytocompatibility of lyophilized powder of cow urine obtained from Sahiwal and the pure Indian breed. We have used several analytical techniques, including Thermogravimetric Analysis (TGA), Fourier Transform Infrared (FTIR) Spectroscopy, Differential Scanning Calorimetry (DSC), Nuclear Magnetic Resonance (NMR) spectroscopy and Scanning Electron Microscopy – Energy Dispersive X-ray Spectroscopy (SEM-EDX) to examine the physical and chemical nature of cow urine powder obtained through lyophilization. SEM-EDX analysis showed clusters like morphology and revealed 25-30% of metal ions present in both samples. TGA analysis showed three steps of degradation sequentially most likely due to initial desorption of adsorbed water, urea degradation, and loss of glycoside moiety present in flavonoid. DSC data revealed the presence of both irregular (amorphous) and ordered molecular structures (crystalline) in the lyophilized powder of cow urine. <sup>1</sup>H NMR spectra of all the prepared cow urine samples exhibited a similar trend and did not vary significantly and; confirming the presence of the same flavonoid/compounds in each sample. FTIR spectra of all the prepared cow urine samples exhibited a similar trend and did not vary significantly as observed through <sup>1</sup>H NMR spectra. In addition, a cytocompatibility study and MTT assay using NIH-3T3 fibroblast cells revealed that lyophilized cow urine powders possessed no deleterious effects on healthy fibroblast cells. Thus, the outcomes provide a benchmark for further understanding of the lyophilized form of cow urine that could be potentially useful for analyzing its therapeutic value.

Artificial biomineralisation and metallic soaps

Study on foam concrete incorporated with expanded vermiculite/capric acid PCM – A novel thermal storage high-performance building material

Continuous production of drug nanocrystals by porous hollow fiber-based anti-solvent crystallization

We report studies of recently precipitated terrestrial Mn oxides from Pinal Creek (Arizona, U.S.A.) and from Yuno-Taki Falls (Hokkaido, Japan). In addition to chemical analysis [by energy dispersive X-ray spectroscopy (EDS) and proton induced X-ray emission spectroscopy (PIXE)], the following methods were used: X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), contraction and expansion tests, thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), infrared spectroscopy (IR), and Mössbauer spectroscopy. Selected area electron diffraction (SAED) was applied in a few cases, but only on synthetic samples. The most useful methods for characterizing the 10 Å Mn minerals were XRD, contraction test, and DSC. Mössbauer spectroscopy was a very useful complementary method to XRD for differentiation of the poorly crystalline Fe compounds. IR spectroscopy was found not to be very useful in distinguishing buserite and birnessite, but a distinct pattern was observed for todorokite. For heterogeneous deposits composed of many minerals, IR was not useful without separation of phases. Three types of samples were identified from Yuno-Taki. One of them, representing a relatively fresh deposit exposed to water, was found to be a nearly ideal buserite with an XRD pattern similar to synthetic samples. An older, non-ideal buserite could be dehydrated but not expanded, suggesting that it had been slightly transformed. The third sample was from a deposit that was dry at the time of sampling. It is a 7 Å mineral (birnessite or takanelite/rancieite). The sample also contains amorphous Fe hydroxide, confirmed by Mössbauer spectroscopy. A test of the possibility of buserite transformation showed that autoclaving a sample of the synthetic 10 Å phyllomanganate, Mg-buserite, resulted in a compound with the XRD pattern and IR spectrum of todorokite. We suggest that this pure synthetic product be used as a model compound for the high-temperature hydrothermal 10 Å manganate with tunnel structure, todorokite. Experiments at other conditions demonstrated that synthetic buserite collapses to birnessite during dehydration. Pinal Creek crusts are composed of quartz, feldspar, Fe minerals (magnetite, maghemite, ilmenite, hematite), and Mn minerals. Resistance to dehydration and expansion tests, and the initial endotherm shown in DSC analysis, suggest that the 10 Å manganate is todorokite. A 7 Å mineral (birnessite or takanelite/rancieite) is also present. Based on comparison of XRD and electron microscopy data for the natural samples with tests done on the synthetic samples, we postulate that the birnessite or takanelite/rancieite and todorokite found in th Pinal Creek crusts may be a transformation products of a buserite precursor.

Синтезированы соли кобальта(II) насыщенных монокарбоновых кислот – муравьиной, масляной, валериановой, капроновой, энантовой, каприловой. Полученные соединения охарактеризованы с помощью элементного анализа, ИК-спектроскопии, термогравиметрии и дифференциально-сканирующей калориметрии. В результате термического разложения синтезированных карбоксилатов, а также ацетата кобальта получены кобальтсодержащие нанокомпозиты. Полученные нанокомпозиты исследованы методами элементного анализа, ИК-спектроскопии, сканирующей и просвечивающей электронной микроскопии, энергодисперсионной рентгеновской спектроскопии и рентгенофазового анализа. Проведены магнитные исследования полученных нанокомпозитов.

Nickel (II) and cobalt (II) salts were synthesized with saturated monocarboxylic acids: butyric, valeric, nylon,enanthic, and caprylic. The obtained compounds were characterized by elemental analysis, IR spectroscopy,and differential scanning calorimetry. As a result of thermolysis of the synthesized carboxylates, nanocomposites were obtained, which were studied by scanning and transmission electron microscopy, elemental analysis, IR spectroscopy, energy dispersive X-ray spectroscopy, and X-ray phase analysis. The magnetic properties of the obtained nanocomposites have been studied.

Cobalt(II) salts are synthesized from saturated monocarboxylic acids: formic, butyric, valerianic, caproic, enanthic, and caprylic acids. The resulting compounds are characterized by elemental analysis, IR spectroscopy, thermogravimetry, and differential scanning calorimetry. As a result of the thermal decomposition of the synthesized carboxylates and cobalt acetate, cobalt-containing nanocomposites are obtained. The obtained nanocomposites are studied by elemental analysis, IR spectroscopy, scanning and transmission electron microscopy, energy dispersive X-ray spectroscopy, and X-ray phase analysis. Magnetic studies of the obtained nanocomposites are carried out.

The structure and composition of aluminum wear debris generated by unlubricated sliding in different environments

Performance assessment of capric acid-ethyl alcohol/expanded vermiculite phase change material incorporated cement mortar for thermal insulation in buildings

Activated carbon (AC) is an effective material for various environmental and industrial applications. The characteristics and performance of AC is a result of interaction between source and method of preparation. In the current work, AC has been prepared from date seed waste using microwave heating under nitrogen using basic medium such as potassium hydroxide and acidic medium such as sulfuric acid as chemical activating agents. The AC was characterised using X-ray diffraction (XRD), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA) with differential scanning calorimetry (DSC). XRD patterns of the AC in both cases exhibited three peaks corresponding to the crystalline graphite form of carbon. Scanning electron microscopy (SEM) images of the freshly prepared carbons showed that the samples contained particles of various sizes including both nanoparticles as well as millimetre-range particles. DSC analysis showed that the samples exhibited endothermic reaction in low temperature ranges until 300°C and exothermic reaction above this temperature. SEM analysis of the AC, separated into three different size ranges, showed significant etching of the surface of the carbon to yield porous structures. The AC produced using sulfuric acid showed better adsorption capacity (9.2 g g−1) when compared to that produced using potassium hydroxide (7.7 g g–1). We conclude that the AC prepared from date seeds can find potential application in water purification and oil spill clean-up.