scholarly journals Humic acids characterization by EDXS and 13C NMR spectroscopy

2010 ◽  
Vol 58 (1) ◽  
pp. 139-146
Author(s):  
Ľubica Pospíšilová ◽  
Naděžda Fasurová ◽  
Tibor Liptaj ◽  
Lubomír Jurica
Keyword(s):  
Humic Acids ◽  
Quality Evaluation ◽  
Spectral Characteristics ◽  
13C Nmr Spectroscopy ◽  
Aromatic Carbon ◽  
X Ray ◽  
Aliphatic Carbon ◽  
C Nmr

Determination of humic acids spectral characteristics performed fast and convenient method for their quality evaluation. Humic acids (HA) were isolated from five different soil types (Luvi-haplic Chernozem, Haplic Luvisol, Haplic Cambisol, Leptic Cambisol and Eutric Cambisol) and from compost. Basic soil characteristics were determined by commonly used methods. Fractional compositon of humus showed that humic acids content was decreasing in order: compost > Luvi-haplic Chernozem > Haplic Luvisol > Eutric Cambisol > Haplic Cambisol > Leptic Cambisol. Isolated humic acids preparations were characterized comparatively by chemical and spectroscopic methods. Elemental analysis showed the highest carbon content in Luvi-haplic Chernozem HA. The lowest carbon amount was in Eutric Cambisol. Energy–dispersive X-ray spectroscopy detected elementsin situin HA molecule. All samples contained Fe, Cu, Zn, Ti, Ca, K, S, P, Si and Br. Practically no differences in elements content between soil humic substances and compost were detected. The amount of aromatic carbon was higher in Luvi-haplic Chernozem to compare with other samples. Humic acids isolated from Cambisols, on the basis13C NMR spectroscopic data, showed that all samples contained less aromatic carbon and significantly more aliphatic carbon.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

Determination of the crystal structure of magnesium perchlorate hydrates by X-ray powder diffraction and the charge-flipping method

2010 ◽  
Vol 66 (6) ◽  
pp. 579-584 ◽  
Author(s):  
Kevin Robertson ◽  
David Bish
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Fundamental Parameter ◽  
Magnesium Perchlorate ◽  
Space Group ◽  
X Ray ◽  
Partial Pressures ◽  
Dehydration Reactions

X-ray powder diffraction (XRD) data were used to solve the crystal structures of phases in the magnesium perchlorate hydrate system, Mg(ClO4)2·nH2O (n = 4, 2). A heating stage and humidity generator interfaced to an environmental cell enabled in-situ XRD analyses of dehydration reactions under controlled temperatures and partial pressures of H2O (P_{{\rm H}_2{\rm O}}). The crystal structures were determined using an ab initio charge-flipping method and were refined using fundamental-parameter Rietveld methods. Dehydration of magnesium perchlorate hexahydrate to tetrahydrate (348 K) results in a decrease in symmetry (space group = C2), where isolated Mg2+ cations are equatorially coordinated by four H2O molecules with two [ClO4]− tetrahedra at the apices. Further dehydration to the dihydrate (423 K) leads to bridging of the isolated packets to form double corner-sharing chains of octahedra and polyhedra (space group = C2/m).

Residual Stresses and Differential Deformation of Electroplated Structures

1989 ◽  
Vol 33 ◽  
pp. 161-169
Author(s):  
G. Sheikh ◽  
I. C. Noyan
Keyword(s):  
Residual Stresses ◽  
Lattice Parameter ◽  
Stress Profile ◽  
X Ray ◽  
Residual Stress Profile ◽  
Cyclic Loading And Unloading ◽  
Nickel Substrates ◽  
Loading And Unloading

AbstractWe report the results of a recent study where nickel substrates electroplated with chromium were loaded in-situ on an x-ray diffractometer. This technique allows determination of lattice spacings in the vicinity of the interface for both the film and the substrate as a function of the applied load. We used such lattice parameter data, SEM observations of the surface and x-ray peak breadth data to study the partitioning of deformation between the film and the substrate. The data indicates progressive loss of adhesion between the film and the substrate with increasing deformation. We observe significant effect of electroplating residual stresses on the mechanical behavior of the system. The loss of adhesion between the film and the substrate coupled with the initial residual stress profile causes an apparent 'negative Poisson's ratio' for the film during initial stages of the loading. This effect disappears with cyclic loading and unloading.

Structure determination of fatty acid ester biofuels via in situ cryocrystallisation and single crystal X-ray diffraction

CrystEngComm ◽  
2019 ◽  
Vol 21 (1) ◽  
pp. 41-52 ◽  
Author(s):  
Siriyara Jagannatha Prathapa ◽  
Cara Slabbert ◽  
Manuel A. Fernandes ◽  
Andreas Lemmerer
Keyword(s):  
Crystal Structure ◽  
Fatty Acid ◽  
Fatty Acid Ester ◽  
Structure Determination ◽  
Homologous Series ◽  
Methyl Esters ◽  
X Ray Diffraction ◽  
X Ray

In situ cryocrystallisation enabled the crystal structure determination of a homologous series of low-melting n-alkyl methyl esters Cn−1H2n+1CO2CH3.

scholarly journals Reactions of 3-(p-substituted-phenyl)-5-chloromethyl-1,2,4-oxadiazoles with KCN leading to acetonitriles and alkanes via a non-reductive decyanation pathway

2018 ◽  
Vol 14 ◽  
pp. 3011-3017
Author(s):  
Akın Sağırlı ◽  
Yaşar Dürüst
Keyword(s):  
Nmr Spectra ◽  
2D Nmr ◽  
Synthetic Route ◽  
X Ray ◽  
H Nmr ◽  
2D Nmr Spectra ◽  
Tof Ms ◽  
C Nmr

The present work describes an unfamiliar reaction of 5-(chloromethyl)-3-substituted-phenyl-1,2,4-oxadiazoles with KCN affording trisubstituted 1,2,4-oxadiazol-5-ylacetonitriles and their parent alkanes, namely, 1,2,3-trisubstituted-1,2,4-oxadiazol-5-ylpropanes. To the best of our knowledge, the current synthetic route leading to decyanated products will be the first in terms of a decyanation process which allows the transformation of trisubstituted acetonitriles into alkanes by the incorporation of KCN with the association of in situ-formed HCN and most likely through the extrusion of cyanogen which could not be detected or isolated. In addition, the plausible mechanisms were proposed for both transformations. The structures of the title compounds were identified by means of IR, 1H NMR, 13C NMR, 2D NMR spectra, TOF–MS and X-ray measurements.

scholarly journals In Situ Structural Determination of a Homogeneous Ruthenium Racemization Catalyst and Its Activated Intermediates Using X‐Ray Absorption Spectroscopy

2020 ◽  
Vol 26 (15) ◽  
pp. 3411-3419 ◽  
Author(s):  
Karl P. J. Gustafson ◽  
Arnar Guðmundsson ◽  
Éva G. Bajnóczi ◽  
Ning Yuan ◽  
Xiaodong Zou ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Absorption
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