X-Ray Diffraction and Melting Point-Composition Studies on the 9,10-Epoxy- and Dihydroxystearic Acids and 9,10-Epoxyoctadecanols2

1950 ◽  
Vol 72 (8) ◽  
pp. 3364-3368 ◽  
Author(s):  
Lee P. Witnauer ◽  
Daniel Swern
Keyword(s):  
Melting Point ◽  
Composition Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Point Composition

Structural and thermodynamic properties of nanocrystalline fcc metals prepared by mechanical attrition

1992 ◽  
Vol 7 (7) ◽  
pp. 1751-1761 ◽  
Author(s):  
J. Eckert ◽  
J.C. Holzer ◽  
C.E. Krill ◽  
W.L. Johnson
Keyword(s):  
Thermal Analysis ◽  
Grain Size ◽  
Melting Point ◽  
Grain Boundary ◽  
Bulk Modulus ◽  
Atomic Level ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fcc Metals ◽  
Mechanical Attrition

Nanocrystalline fcc metals have been synthesized by mechanical attrition. The crystal refinement and the development of the microstructure have been investigated in detail by x-ray diffraction, differential scanning calorimetry, and transmission electron microscopy. The deformation process causes a decrease of the grain size of the fcc metals to 6–22 nm for the different elements. The final grain size scales with the melting point and the bulk modulus of the respective metal: the higher the melting point and the bulk modulus, the smaller the final grain size of the powder. Thus, the ultimate grain size achievable by this technique is determined by the competition between the heavy mechanical deformation introduced during milling and the recovery behavior of the metal. X-ray diffraction and thermal analysis of the nanocrystalline powders reveal that the crystal size refinement is accompanied by an increase in atomic-level strain and in the mechanically stored enthalpy in comparison to the undeformed state. The excess stored enthalpies of 10–40% of the heat of fusion exceed by far the values known for conventional deformation processes. The contributions of the atomic-level strain and the excess enthalpy of the grain boundaries to the stored enthalpies are critically assessed. The kinetics of grain growth in the nanocrystalline fcc metals are investigated by thermal analysis. The activation energy for grain boundary migration is derived from a modified Kissinger analysis, and estimates of the grain boundary enthalpy are given.

Crystal Structure and Colorimetric Behavior of Low Melting Point Ternary Alloy

2020 ◽  
Vol 1002 ◽  
pp. 12-20
Author(s):  
Tarik T. Issa ◽  
Sadeer M. Majeed ◽  
Duha S. Ahmed
Keyword(s):  
Crystal Structure ◽  
Melting Point ◽  
Mechanical Alloying ◽  
Ternary Alloy ◽  
High Purity ◽  
Milling Time ◽  
X Ray Diffraction ◽  
X Ray ◽  
Before And After

Elements of high purity (99.999) ,were used to prepare the alloy , Bi ,Sn,Zn and Cu .Two types alloy Bi – Sn – Zn and Bi – Sn – Cu were prepared by mechanical alloying technique (MA) .Annealing at 100 °Cfor 8 hours was applied for the resulting alloys . X-ray diffraction and differential scanning colorimetriy were tested for the two types of alloy before and after annealing. The best results was noticed in the ternary alloythat prepared at 4 hours milling time ,and annelid at 100 °C, for 8 hours ,under static air.

The Influence of Emulsifiers on the Crystal Properties of Tristearin and Trilaurin

1988 ◽  
Vol 3 (1) ◽  
pp. 19-22 ◽  
Author(s):  
J. Schlichter ◽  
I. Mayer ◽  
S. Sarig ◽  
N. Garti
Keyword(s):  
Crystal Structure ◽  
Melting Point ◽  
Diffraction Method ◽  
The Other ◽  
Sorbitan Monostearate ◽  
X Ray Diffraction ◽  
Sorbitan Monolaurate ◽  
X Ray ◽  
Crystal Properties ◽  
Long Chain

AbstractThe effect of solid emulsifiers, added at the level of 10%, on the lattice parameters of tristearin and trilaurin, has been studied by powder X-ray diffraction method. The presence of sorbitan monostearate and glycerol-l-stearate affects slightly the lattice constant a in tristearin; on the other hand, although sorbitan monostearate causes an increase in a of trilaurin, glycerol-l-stearate does not. The presence of sorbitan monolaurate and glycerol-l-laurate affect a of trilaurin similarly to the long chain emulsifiers.A correlation between the effect on a and the increase in melting point has been found.The presence of the emulsifier does not alter drastically the lattice dimensions of the fat. The slight dissimilarity in crystal structure between tristearin and trilaurin is confirmed by the diverse effects of the emulsifiers on the internal structure of the fat.

Determination of average carbon number of petroleum waxes by X-ray diffraction

2008 ◽  
Vol 41 (5) ◽  
pp. 950-951 ◽  
Author(s):  
Sanat Kumar ◽  
S. P. Srivastava ◽  
H. U. Khan
Keyword(s):  
Melting Point ◽  
Long Range ◽  
Carbon Number ◽  
High Melting ◽  
X Ray Diffraction ◽  
High Melting Point ◽  
X Ray ◽  
Long Range Ordering ◽  
Standard Gas

Eight petroleum waxes, both paraffin as well as microcrystalline, have been analysed by X-ray diffraction. The average carbon number has been estimated by the long-range ordering observed in the diffractograms of these waxes. The average carbon number has also been determined following the standard gas chromatographic (GC) method. The results obtained by X-ray diffractometry compare well with those obtained by the GC method. The former method also permits determination of the average carbon number of high melting point waxes, which is otherwise difficult using GC.

scholarly journals The Usefulness of X-ray Diffraction and Thermal Analysis to Study Dietary Supplements Containing Iron

Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 197
Author(s):  
Izabela Jendrzejewska ◽  
Robert Musioł ◽  
Tomasz Goryczka ◽  
Ewa Pietrasik ◽  
Joanna Klimontko ◽  
...  
Keyword(s):  
Thermal Analysis ◽  
Melting Point ◽  
Dietary Supplements ◽  
Polymorphic Form ◽  
Food Supplements ◽  
X Ray Diffraction ◽  
Iron Compounds ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Amorphous Compounds

X-ray powder diffraction (XRPD) and thermal analysis (differential scanning calorimetry/derivative of thermogravimetry (DSC/DTG)) are solid-state techniques that can be successfully used to identify and quantify various chemical compounds in polycrystalline mixtures, such as dietary supplements or drugs. In this work, 31 dietary supplements available on the Polish market that contain iron compounds, namely iron gluconate, fumarate, bisglycinate, citrate and pyrophosphate, were evaluated. The aim of the work was to identify iron compounds declared by the manufacturer as food supplements and to try to verify compliance with the manufacturer’s claims. Studies performed by X-ray and thermal analysis confirmed that crystalline iron compounds (iron (II) gluconate, iron (II) fumarate), declared by the manufacturers, were present in the investigated dietary supplements. Iron (II) bisglycinate proved to be semi-crystalline. However, depending on the composition of the formulation, it was possible to identify this compound in the tested supplements. For amorphous iron compounds (iron (III) citrate and iron (III) pyrophosphate), the diffraction pattern does not have characteristic diffraction lines. Food supplements containing crystalline iron compounds have a melting point close to the melting point of pure iron compounds. The presence of excipients was found to affect the shapes and positions of the endothermic peaks significantly. Widening of endothermic peaks and changes in their position were observed, as well as exothermic peaks indicating crystallization of amorphous compounds. Weight loss was determined for all dietary supplements tested. Analysis of the DTG curves showed that the thermal decomposition of most food supplements takes place in several steps. The results obtained by a combination of both simple, relatively fast and reliable XRPD and DSC/DTG methods are helpful in determining phase composition, pharmaceutical abnormalities or by detecting the presence of the correct polymorphic form.

scholarly journals ISOLATION AND STRUCTURAL ELUCIDATION OF A NEW DEPSIDE OF LICHEN Everniopsis trulla

2021 ◽  
Vol 87 (2) ◽  
pp. 97-106
Author(s):  
Olivio Nino Castro ◽  
Jesús López Rodilla ◽  
Sofia Pombal ◽  
Francisca Sanz González ◽  
Julio Santiago Contreras
Keyword(s):  
Mass Spectrometry ◽  
Melting Point ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Spectroscopic Data ◽  
Intermolecular Forces ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Uv Visible

In this research, a new depside of the lichen Everniopsis trulla has been isolated. The extraction was carried out to 400 g of dry sample and ground with ethanol for 3 repetitions, then, it was fractionated by applying column chromatography with the CHCl3-MeOH system and purified by recrystallization with MeOH-Acetone (1: 1); Finally, white crystals in the form of needles (solid C) with a melting point of 198 ° C were obtained, whose structure was elucidated based on spectroscopic data (UV-Visible, IR, NMR-H1, NMR-C13, mass spectrometry and single crystal X-ray diffraction). According to the Science Finder databases, it is a new depside, called trullarin, and it is observed that molecular packing is influenced by both intramolecular and intermolecular forces. Intermolecular hydrogen bonds of O - H -O type binds neighboring molecules forming dimers.

scholarly journals Synthesis Candidates Herbicide Through Optimization Quinclorac Containing 3-Methyl-1H-pyrazol-5-yl

2021 ◽  
Vol 9 ◽  
Author(s):  
Dingfeng Luo ◽  
Haodong Bai ◽  
Xiaomao Zhou ◽  
Lamei Wu ◽  
Chengjia Zhang ◽  
...  
Keyword(s):  
Melting Point ◽  
Detrimental Effect ◽  
Herbicidal Activity ◽  
X Ray Diffraction ◽  
Fresh Weight ◽  
Neutral Group ◽  
Barnyard Grass ◽  
X Ray ◽  
Inhibition Effect ◽  
Stage 1

To enhance quinclorac potency, twenty-five derivatives were synthesized containing 3-methyl-1H-pyrazol-5-yl by intermediate derivatization methods (IDMs). These compounds were confirmed by melting point (mp), 1HNMR, 13CNMR, and HRMS. The compound 1,3-dimethyl-1H-pyrazol-5-yl 3,7-dichloroquinoline-8-carboxylate (10a) was determined by X-ray diffraction. The activity of these compounds substituent on the phenyl was: electron-drawing group > neutral group > donor-drawing group, the results was like that of substituted benzyl group on pyrazole. The herbicidal activity assays showed that compounds 1-(2-fluorophenyl)-3-methyl-1H-pyrazol-5-yl 3,7-dichloroquinoline-8-carboxylate (8l, EC50 = 10.53 g/ha) and 10a (EC50 = 10.37 g/ha) had an excellent inhibition effect on barnyard grass in greenhouse experiment. Greenhouse safety experiment of rice exhibited almost no difference in plant height and fresh weight treated 10a at stage 1∼2-leaf of rice after 14 days but 8l had a detrimental effect. Two season field assays showed 10a herbicidal activity on barnyard grass at 150 g/ha as equal as 300 g/ha quinclorac in fields in 2019 and 2020. The study demonstrated that 10a could be further researched as a potential herbicide to control barnyard grass in fields.

scholarly journals Evaluation of Thermal-Induced Polymorphic Transformation on Desloratadine and Desloratadine-Benzoic Acid Salt

2020 ◽  
Vol 26 (4) ◽  
pp. 399-405
Author(s):  
Ahmad Ainurofiq ◽  
Rachmat Mauludin ◽  
Diky Mudhakir ◽  
Sundani Nurono Soewandhi
Keyword(s):  
Melting Point ◽  
Benzoic Acid ◽  
Polymorphic Transformation ◽  
Heating Process ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Physicochemical Changes ◽  
Transformation Methods

Background: Active pharmaceutical ingredients face a challenge in manufacturing due to adverse physicomechanical properties. Desloratadine (DES) form I exhibits poor mechanical behavior through the formation of capping during the tableting process. Salt formation from DES and benzoic acid (BA) has been observed to resolve poor mechanical properties. However, the ability to withstand heat from the manufacturing process should be implemented in DES and DES-BA salt. The aim of this study was to determine the differences between thermal treatment results on DES and DES-BA salt and whether it causes them to undergo polymorphic transformation. Methods: Salt was crystallized between DES and BA using the solvent evaporation method. DES and DES-BA salt were heated at 110°C, 159°C (melting point of DES), 181°C (melting point of DES-BA), and 190°C. Following this, characterization was performed using differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and solubility testing. Results: Polymorphic transformation caused by heat occurred in DES, but not in DES-BA salt. The transformation of DES was induced by the effect of heating, which changed polymorph I to a mixture of polymorph I and III at 110°C, to polymorph II at 159°C, and to a mixture of polymorph I, II, and III at 190°C. Under 190oC, DES-BA is still stable and did not undergo a polymorphic transformation. However, at 190oC, decomposition started to occur, which implied decreased solubility, which did not occur in DES. Conclusion: The heating process did not cause DES-BA salt to undergo a polymorphic transformation. However, it caused decomposition at 190oC. DES underwent a polymorphic transformation when exposed to the same condition without decomposition. This provided information to always pay attention to temperature during manufacturing processes that include DES or DES-BA salt to avoid physicochemical changes.

High-temperature powder x-ray diffraction of yttria to melting point

1999 ◽  
Vol 14 (2) ◽  
pp. 456-459 ◽  
Author(s):  
V. Swamy ◽  
N. A. Dubrovinskaya ◽  
L. S. Dubrovinsky
Keyword(s):  
High Temperature ◽  
Solid State ◽  
Melting Point ◽  
Unit Cell Parameter ◽  
Cell Parameter ◽  
Unit Cell ◽  
Diffraction Spectrum ◽  
X Ray Diffraction ◽  
Thermal Expansion Data ◽  
X Ray

Powder x-ray diffraction data of yttria (Y2O3) were obtained from room temperature to melting point with the thin wire resistance heating technique. A solid-state phase transition was observed at 2512 ± 25 K and melting of the high-uemperature phase at 2705 ± 25 K. Thermal expansion data for α–Y2O3 (C-type) are given for the range 298–2540 K. The unit cell parameter increases nonlinearly, especially just before the solid-state transition. The x-ray diffraction spectrum of the high-temperature phase is consistent with the fluorite-type structure (space group Fm3) with a refined unit cell parameter a = 5.3903(6) Å at 2530 K. The sample recrystallized rapidly above 2540 K, and above 2730 K, all the diffraction lines and spots disappeared from the x-ray diffraction spectrum that suggests complete melting.

Effect of Strain on Thermodynamic Melting Temperature of Polymers

1967 ◽  
Vol 40 (3) ◽  
pp. 788-800
Author(s):  
W. R. Krigbaum ◽  
J. V. Dawkins ◽  
G. H. Via ◽  
Y. I. Balta
Keyword(s):  
Free Energy ◽  
Melting Point ◽  
Natural Rubber ◽  
Sonic Velocity ◽  
X Ray Diffraction ◽  
Elongation Ratio ◽  
Flory Theory ◽  
X Ray ◽  
Theoretical Predictions ◽  
Crystallization Conditions

Abstract X-ray diffraction, sonic velocity, and birefringence measurements were used to study the variation of the apparent melting point of strained natural rubber and polychloroprene vulcanizates with elongation ratio and crystallization temperature. The procedure of Hoffman and Weeks was employed to obtain the thermodynamic melting point, tm, for each elongation ratio α. The parameter β relating to the distribution of fold lengths is unusually large for low elongation ratios and decreases into the usual range only at higher elongations. Observed variations of tm with α for these two polymers are compared with the theoretical predictions of Flory and Roe and Krigbaum. Although the predictions of the Flory theory depend somewhat upon the value assigned for the number of repeating units per statistical link, and this parameter is not well known for polychloroprene, we nevertheless conclude that his treatment offers a better representation of the melting point elevation for high elongations. Due to the approximations introduced, the treatment of Flory is not valid for lower elongations. Any attempt to improve this treatment must begin by specifying the free energy of the semicrystalline system, which implies a knowledge of the distribution of crystallite orientations and how this distribution varies with strain and with the crystallization conditions.

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