scholarly journals High Throughput Screening and Characterization Methods of Jordanian Oil Shale as a Case Study

Energies ◽  
2019 ◽  
Vol 12 (16) ◽  
pp. 3148 ◽  
Author(s):  
Ziad Abu El-Rub ◽  
Joanna Kujawa ◽  
Esra’a Albarahmieh ◽  
Nafisah Al-Rifai ◽  
Fathieh Qaimari ◽  
...  
Keyword(s):  
High Throughput Screening ◽  
Oil Shale ◽  
Analytical Techniques ◽  
Economic Feasibility ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Characterization Methods ◽  
X Ray ◽  
Hydrogen Mass

Oil shale is an important possible solution to the problem of energy in Jordan. To explore the technical and the economic feasibility of oil shale deposits, numerous samples are analyzed using the standard Fischer Assay (FA) method. However, it would be useful to develop faster, cheaper, and reliable methods for determining the oil content of oil shale. Therefore, the aim of this work was to propose and investigate rapid analytical techniques for the screening of oil shale deposits and to correlate them with the FA method. The Omari deposit located east of Jordan was selected as a case study for analysis using thermogravimetric analysis (TGA) coupled with Fourier-transform infrared (FTIR), differential scanning calorimetry (DSC), elemental analysis, X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray (EDX) analysis. Results obtained from the TGA method were linearly correlated with FA with high regression factor (R2 = 0.99); a quadratic correlation (R2 = 0.98) was maintained between the FA and the elemental hydrogen mass content, and a quadratic correlation (R2 = 0.97) was found between the FA and the aliphatic hydrocarbons (FTIR peak at 2927 cm−1) produced in the pyrolysis zone. Although other techniques were less correlated, further investigation might lead to better results. Subsequently, these correlated techniques can be a practical alternative to the conventional FA method when, in particular, specific correlation is made for each deposit.

scholarly journals Toward an Understanding of the Formation and Desolvation of Methanol Solvate, and Structure of Methanolysis Product: A Case Study of Nicosulfuron

Crystals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 157
Author(s):  
Huaxiang Zhu ◽  
Bei Zhang ◽  
Di Wu ◽  
Xiaowei Cheng ◽  
Guiping Li ◽  
...  
Keyword(s):  
Solid Phase ◽  
Great Influence ◽  
Acid Methyl Ester ◽  
Analytical Techniques ◽  
Systematic Investigation ◽  
Herbicidal Activity ◽  
Carbamic Acid ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray

Nicosulfuron (NS) is a widely used sulfonylurea herbicide because of its high selectivity, broad spectrum of herbicide activity, and excellent performance. In this work, nicosulfuron methanol solvate (NS-MeOH) and [[3-[(Dimethylamino)carbonyl]-2-pyridinyl]sulfonyl]carbamic acid methyl ester (PCM) as a product of methanolysis of NS were obtained. Both of their structures were determined by a single crystal X-ray diffraction. A broad range of analytical techniques was applied to characterize the NS-MeOH, such as Powder X-ray diffraction (PXRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and hot stage microscopy (HSM). Combined with the analysis of the Independent gradient model (IGM), Atom-in-molecules (AIM), and Hirshfeld surface (HS), direct insights into the role of solvent played in the formation of NS-MeOH and the mechanism of solid-to-solid phase transformation of NS-MeOH could be obtained. In addition, the aqueous solubility of NS was improved through the formation of NS-MeOH. A systematic investigation of herbicidal activity of NS and PCM was carried out. It was found that NS and NS-MeOH had similar herbicidal activities at the experimental concentrations while PCM exhibited significantly lower activity. It was suggested that methanolysis of the sulfonylurea bridge in the NS molecule exerted a great influence on the herbicidal activity.

Mechanochemical Synthesis of Nanocrystalline CeO2: The Effect of Annealing Temperatures on the Particle Size

2006 ◽  
Vol 517 ◽  
pp. 252-256 ◽  
Author(s):  
Abdul Hadi ◽  
Iskandar Idris Yaacob ◽  
Lee Seok Ling
Keyword(s):  
Annealing Temperature ◽  
Gas Adsorption ◽  
Weight Ratio ◽  
X Ray Diffraction ◽  
Treatment Results ◽  
Scanning Calorimetry ◽  
Characterization Methods ◽  
X Ray ◽  
Annealing Temperatures ◽  
Adsorption Desorption

Cerium dioxide (CeO2) nanoparticles were synthesized by a novel mechanochemical process. The precursors of Ce2(CO3)3.xH2O and NaOH were mixed at a weight ratio of 4 to 1. The mixtures were milled using a planetary ball mill with ball to powder ratio of 10:1. The products were then characterized using a battery of characterization methods, including X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and gas adsorption-desorption measurement. The as-prepared particles were largely amorphous with an average specific surface area of about 119.94 m2/g. Nanocrystalline CeO2 with crystallite size of 4.5 nm was obtained when the sample was annealed in air at 350 oC. The heat treatment results showed that the crystallinity of nanocrystalline CeO2 increased with increasing annealing temperature.

scholarly journals Improvement of the optical and photocatalytic properties of ZnAl2O4: 1% La3+, x% Pb2+ nanoparticles synthesized by citrate sol-gel route

2021 ◽  
Author(s):  
Hichem Filali ◽  
Nahman Boukheit ◽  
Rafika Bouhroum ◽  
Wassila Chekirou ◽  
Ahcène Karaali
Keyword(s):  
Raman Spectroscopy ◽  
Single Phase ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Constant Amount ◽  
Pure Zinc ◽  
Characterization Methods ◽  
X Ray ◽  
Gel Technique

Abstract Samples of pure zinc aluminate (ZnAl2O4) and doped both with lead (Pb2+) at different ratios (0, 0.5, 1, 1.5, 2 and 2.5% mol) and a constant amount of lanthanum (La: 1% mol), were prepared by the citrate sol-gel technique, and then annealed at 900°C for 2h. In order to study the structural, optical and thermal properties; different characterization methods were used, such as: powder X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), differential scanning calorimetry (DSC), TGA, Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. The Analyzes by XRD revealed the presence of the cubic single phase ZnAl2O4 for all samples, with a crystallites size between 19 and 25 nm. These results were confirmed using FTIR, Raman spectroscopy and SEM. Also, photocatalytic study for different samples of ZnAl2O4 shows that they can be used like as photocatalyst and good adsorbents for degradation of Hexamethyl crystallized violet dye in aqueous solution.

scholarly journals Stabilising peroxyacids in niche microenvironments

2014 ◽  
Vol 70 (a1) ◽  
pp. C644-C644
Author(s):  
Dyanne Cruickshank ◽  
Chick Wilson
Keyword(s):  
Chemical Reactivity ◽  
Analytical Techniques ◽  
Direct Consequence ◽  
High Reactivity ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Wide Range ◽  
Chemically Reactive Species ◽  
Household Cleaning Products

There has been dramatic evolution in the formulation of household cleaning products over the last decade, this is mainly due to the influence of social change, regulatory pressure and the need for new less toxic, safer formulations with increased performance. Due to their high chemical reactivity, peroxides are found in a wide range of bleaching agents, they are known for their instability which is a direct consequence of their high reactivity (in turn essential for function). Stabilising such materials for implementation in a range of product types is a significant target within the domestic products industry. Supramolecular approaches are already being explored to try stabilise other chemically reactive species such as explosives [1,2] thus illustrating the feasibility of this research. The work to be presented will deal with peroxyacids that include small model compounds such as m-chloroperbenzoic acid as well as a commericially relevant bleaching agent and their inclusion in both crystalline and amorphous hosting systems. Single crystal X-ray diffraction methods are used to elucidate the ordered crystalline structures and to confirm whether or not the peroxo group is still intact within the crystalline host environments. Simple reactivity tests are used to demonstrate whether or not the amorphous host-guest complexes contain the active peroxy acid within their host cavity. Other complementary analytical techniques such as powder X-ray diffraction, differential scanning calorimetry and thermogravimetry have also been used to characterise the newly-hosted peroxyacid materials. By hosting these molecules in microenvironments it is possible to prepare formulations that are less pH sensitive, thus making their storage safer while allowing their reactivity to be controlled and tuned.

Evaluation of properties of sulfur-based polymers obtained by inverse vulcanization: Techniques and challenges

2020 ◽  
pp. 096739112095407 ◽  
Author(s):  
Ali Shaan Manzoor Ghumman ◽  
Mohamed Mahmoud Nasef ◽  
M Rashid Shamsuddin ◽  
Amin Abbasi
Keyword(s):  
Elemental Sulfur ◽  
Complex Structure ◽  
X Ray Diffraction ◽  
Renewable Materials ◽  
Scanning Calorimetry ◽  
Characterization Methods ◽  
X Ray ◽  
Characterization Techniques ◽  
Thermal Gravimetric Analyzer ◽  
Treatment Conditions

Sulfur-based polymers are unique renewable materials that are receiving a growing attention. The utilization of elemental sulfur with a variety of monomers in their preparation in the absence of solvents using the inverse vulcanization are granting them green nature and unique properties. Several characterization techniques have been used to evaluate the properties of sulfur-based polymers. However, the complex structure and lack of solubility undermine the applicability of some standard characterization techniques in the usual manners. This article reviews the characterization methods used for the evaluation of various properties of sulfur-based polymers such as chemical, morphological, structural, thermal, rheological and mechanical properties, all of which vary depending on the type of comonomer involved in the reaction and heat treatment conditions. The successful applications of different characterization techniques including Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, nuclear magnetic resonance (NMR), scanning electron microscopy/X-ray energy dispersion (SEM-EDX), X-ray diffraction (XRD), mechanical tester, rheometer, thermal gravimetric analyzer (TGA) and differential scanning calorimetry (DSC) are discussed. The challenges to the evaluation of the properties of sulfur-based polymers and the innovative applications of the conventional techniques to overcome them are also deliberated.

scholarly journals Tuning the Crystal Habits of Organic Explosives by Antisolvent Crystallization: The Case Study of 2,6-dimaino-3,5-dinitropyrazine-1-oxid (LLM-105)

Crystals ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 392 ◽  
Author(s):  
Xiaoqing Zhou ◽  
Junhui Shan ◽  
Dong Chen ◽  
Hongzhen Li
Keyword(s):  
Methylene Chloride ◽  
Crystal Habit ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Crystallization Experiments ◽  
Antisolvent Crystallization ◽  
Ft Ir ◽  
Habit Modification

Crystallization is one of the most important methods in the crystal habit control of explosive products. For this study, the antisolvent crystallization experiments were carried out to tune the crystal habits of 2,6-dimaino-3,5-dinitropyrazine-1-oxid (LLM-105). Dimethyl sulphoxide (DMSO) was used as an organic solvent. Water, methanol, acetic acid, nitromethane, acetone, ethanol, methylene chloride, o-dichlorobenzene, and toluene were selected as antisolvents. The X-shaped, spherical cluster-like, rod-like, needle-like, and dendritic crystals were successfully produced by varying the kind of the antisolvent. These results manifested that the polarity and functional groups of antisolvent molecules played important roles in the crystal habits of LLM-105 explosive. The powder X-ray diffraction (PXRD) and Fourier transform infrared (FT-IR) measurements indicated that these antisolvents just tuned the crystal habit of LLM-105 but did not change the crystal structure. The differential scanning calorimetry (DSC) and thermogravimetry (TG) results of the obtained crystals showed that the crystal habits significantly affected the thermal properties. This study can contribute to the investigation of the mechanism of antisolvent-induced crystal habit modification and screen out the efficient antisolvents.

scholarly journals Structural studies of crystalline forms of triamterene with carboxylic acid, GRAS and API molecules

IUCrJ ◽  
2018 ◽  
Vol 5 (3) ◽  
pp. 309-324 ◽  
Author(s):  
Abida Rehman ◽  
Amit Delori ◽  
David S. Hughes ◽  
William Jones
Keyword(s):  
Analytical Techniques ◽  
Gravimetric Analysis ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Evaporative Crystallization ◽  
Structural Database ◽  
Crystalline Forms ◽  
Good Agreement

Pharmaceutical salt solvates (dimethyl sulfoxide, DMSO) of the drug triamterene with the coformers acetic, succinic, adipic, pimelic, azelaic and nicotinic acid and ibuprofen are prepared by liquid-assisted grinding and solvent-evaporative crystallization. The modified ΔpK a rule as proposed by Cruz-Cabeza [(2012). CrystEngComm, 14, 6362–6365] is in close agreement with the results of this study. All adducts were characterized by X-ray diffraction and thermal analytical techniques, including single-crystal X-ray diffraction, powder X-ray diffraction, differential scanning calorimetry and thermal gravimetric analysis. Hydrogen-bonded motifs combined to form a variety of extended tapes and sheets. Analysis of the crystal structures showed that all adducts existed as salt solvates and contained the aminopyridinium–carboxylate heterodimer, except for the solvate containing triamterene, ibuprofen and DMSO, as a result of the presence of a strong and stable hemitriamterenium duplex. A search of the Cambridge Structural Database (CSD 5.36, Version 1.18) to determine the frequency of occurrence of the putative supramolecular synthons found in this study showed good agreement with previous work.

scholarly journals Synthesis of Polytetrahydrofuran Using Protonated Kaolin as A Solid Acid Catalyst

2019 ◽  
Vol 14 (2) ◽  
pp. 294
Author(s):  
Abdelhak Moumen ◽  
Zhour Hattab ◽  
Youghourta Belhocine ◽  
Kamel Guerfi ◽  
Nacer Rebbani
Keyword(s):  
Solid Acid ◽  
Solid Acid Catalyst ◽  
Analytical Techniques ◽  
Acid Catalyst ◽  
Crystalline Substance ◽  
High Catalytic Activity ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir

In this work, a non-toxic protonated kaolin clay exchanged with protons, was successfully applied as a solid acid catalyst for the polymerization of tetrahydrofuran (poly(THF)) at room temperature in the presence of acetic anhydride. Prior to using the kaolin as a catalyst, it was treated with HCl (0.1 M) and characterized using various analytical techniques. The amounts of catalyst and reaction time on the conversion of THF were investigated. Characterizations of nuclear magnetic Resonance of proton (1H-NMR), Fourier Transform Infrared spectroscopy (FT-IR), X-ray Diffraction (XRD), Optical Microscopy (OM), and Differential Scanning Calorimetry (DSC) techniques were used to examine the resulting polymer. X-ray characterization and DSC data indicated that the obtained poly(THF) is a highly crystalline substance. The results showed that protonated kaolin (kaolin–H+) has a high catalytic activity for the polymerization of THF with a conversion rate of 50.02% after 20 hours. Copyright © 2019 BCREC Group. All rights reserved. 

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

Studies on the Preparation, Characterization and Solubility of -Cyclodextrin-Roxythromycin Inclusion Complexes

2009 ◽  
Vol 2 (2) ◽  
pp. 523-530
Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  
Keyword(s):  
Dissolution Rate ◽  
Inclusion Complexes ◽  
Phase Solubility ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ir Studies ◽  
Poorly Soluble ◽  
Poorly Soluble Drug

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.

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