Minimizing the effects of RF inhomogeneity and phase transients allows resolution of two peaks in the 1H CRAMPS NMR spectrum of adamantane

2015 ◽  
Vol 71 ◽  
pp. 30-40 ◽  
Author(s):  
Darren H. Brouwer ◽  
Matthew Horvath
Keyword(s):  
Nmr Spectrum ◽  
Rf Inhomogeneity ◽  
Two Peaks

scholarly journals ЯМР-исследование магнитной структуры и сверхтонких взаимодействий в бинарном гелимагнетике FeP

2019 ◽  
Vol 61 (5) ◽  
pp. 836
Author(s):  
A.A. Гиппиус ◽  
С.В. Журенко ◽  
N. Buttgen ◽  
M. Schadler ◽  
И.В. Морозов ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Nmr Spectra ◽  
Helical Structure ◽  
Spin Reorientation ◽  
Zero Field ◽  
Nmr Spectrum ◽  
Iron Phosphide ◽  
Powder Samples ◽  
Two Peaks ◽  
Weak Fields

AbstractAn NMR analysis of ^31P nuclei in metallic iron phosphide FeP has been performed both in a zero field and by sweeping the external magnetic field at several fixed frequencies with the aim of revealing and investigating the transformation of the magnetic helical structure of FeP. The NMR lineshape gradually changes with an increase in the field strength from trapezoidal (in weak fields) to pronounced asymmetric with two peaks (in strong fields). The former shape is typical of NMR spectra of powder samples under an applied magnetic field, while the latter is characteristic of NMR spectra of nonmagnetic atoms in single-crystalline helimagnetics. The observed transformation of the FeP NMR spectrum evidences in favor of the spin-reorientation transition of a spin-flop type in FeP at strong external fields.

Textural and spectroscopic studies on hydrothermal dumortierite from an Al-rich clay deposit, southeastern Korea

2003 ◽  
Vol 67 (4) ◽  
pp. 799-806
Author(s):  
C. O. Choo ◽  
Y. Kim
Keyword(s):  
Chemical Shifts ◽  
Volcanic Rocks ◽  
Structural Formula ◽  
Spectroscopic Studies ◽  
Mas Nmr ◽  
Thin Layers ◽  
Axially Symmetric ◽  
Nmr Spectrum ◽  
Clay Deposit ◽  
Two Peaks

AbstractDumortierite occurs as small nodules or thin layers along horizontal fractures in the altered volcanic rocks of the Milyang clay deposit, southeastern Korea. Textural evidence shows that dumortierite is associated with pyrophyllite, suggesting that the silica activity increased with decreasing B and Al activities during the hydrothermal alteration. Dumortierite chemistry shows a slight excess of Al, possibly due to common occurrence of Al-rich minerals in the clay deposit. The structural formula of dumortierite is recalculated as Al6.93(Fe0.03Mg0.07)B(Si2.99Al0.01)O18. An absorption peak at 1387 cm–1 in the IR spectrum indicates that B is present in three-fold coordinated sites. The 29Si MAS NMR spectrum has two peaks at –90.9 and –95.5 ppm, showing that Si in dumortierite is located in two different crystallographic sites and is linked to four octahedral Al atoms. The 27Al MAS NMR spectrum shows only one asymmetrical peak near 0 ppm, suggesting that there is no substitution of Al for Si. The 11B MAS NMR spectrum at 17.5 ppm shows a typical second order quadrupole pattern represented by the three-fold coordinated B. The 11B chemical shifts indicate that all of the B occupies such sites, indicating that the B sites are axially symmetric or nearly so in a very well defined site.

Synthesis, spectroscopic and configurational study, and ab initio calculations of new diazaphospholanes

2011 ◽  
Vol 65 (5) ◽  
Author(s):  
Khodayar Gholivand ◽  
Fatemeh Ghaziani
Keyword(s):  
Ab Initio Calculations ◽  
Ab Initio ◽  
1H Nmr ◽  
Nmr Spectra ◽  
31P Nmr ◽  
1H Nmr Spectra ◽  
Equatorial Position ◽  
Nmr Spectrum ◽  
Stable Forms ◽  
Two Peaks

AbstractNew 2-substituted diazaphospholane-2-oxides (I-III, V-VIII) and diazaphosphorinane-2-oxide (IV) were synthesised and characterised by 1H, 13C, and 31P NMR, IR spectroscopy, and elemental analysis. The presence of chiral diamino groups in compounds II and V–VIII gives rise to various diastereomers so that the 31P{1H} NMR spectra demonstrated three and two peaks with different ratios, respectively. Also, the 1H and 13C{1H} NMR spectra of compounds II and V–VIII revealed three and two sets of signals for the related conformers (diastereomers). Interestingly, the 31P NMR spectrum of V in D2O indicated a great upfield shift (Δδ = 19.0) for 31P relative to the value obtained in DMSO-d6 (solvent effect). The two signals in V split further to three signals in the presence of β-cyclodextrin. Moreover, conformational analysis of diazaphospholane V was studied by ab initio calculations at the HF and B3LYP levels of theory using the Gaussian 98 program. Results indicated that among four suggested diastereomers (C1–C4) of V, C1 and C3 containing methyl group in the equatorial position are the most stable forms.

Preparation and Characterization of NH2-Terminal Fibrinogen Bβ Fragments from N-DSK of Human Fibrinogen

1984 ◽  
Vol 51 (01) ◽  
pp. 016-021 ◽  
Author(s):  
S Birken ◽  
G Agosto ◽  
B Lahiri ◽  
R Canfield
Keyword(s):  
High Performance ◽  
Gel Filtration ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Reverse Phase ◽  
Human Fibrinogen ◽  
Human Volunteers ◽  
Cnbr Cleavage ◽  
Two Peaks

SummaryIn order to investigate the early release of NH2-terminal plasmic fragments from the Bβ chain of fibrinogen, substantial quantities of Bβ 1-42 and Bβ 1-21 are required as immunogens, as radioimmunoassay standards and for infusion into human volunteers to determine the half-lives of these peptides. Towards this end methods that employ selective proteolytic cleavage of these fragments from fibrinogen have been developed. Both the N-DSK fragment, produced by CNBr cleavage of fibrinogen, and Bβ 1-118 were employed as substrates for plasmin with the finding of higher yields from N-DSK. Bβ 1-42 and Bβ 1-21 were purified by gel filtration and ion-exchange chromatography on SP-Sephadex using volatile buffers. When the purified preparation of Bβ 1-42 was chromatographed on reverse-phase high performance liquid chromatography, two peaks of identical amino acid composition were separated, presumably due either to pyroglutamate or to amide differences.

Characterization of Microcrystalline Transition from Amorphous Silicon as a Function of Hydrogen Dilution and Substrate Temperature of Hot-wire CVD

2002 ◽  
Vol 715 ◽  
Author(s):  
Keda Wang ◽  
Haoyue Zhang ◽  
Jian Zhang ◽  
Jessica M. Owens ◽  
Jennifer Weinberg-Wolf ◽  
...  
Keyword(s):  
Substrate Temperature ◽  
Sudden Change ◽  
Chemical Vapor ◽  
Threshold Value ◽  
Ir Absorption ◽  
Sudden Increase ◽  
Hot Wire ◽  
Hydrogen Dilution ◽  
Integral Absorption ◽  
Two Peaks

Abstracta-Si:H films were prepared by hot wire chemical vapor deposition. One group was deposited at a substrate temperature of Ts=250°C with varied hydrogen-dilution ratio, 0<R<10; the other group was deposited with fixed R=3 but a varied Ts from 150 to 550°C. IR, Raman and PL spectra were studied. The Raman results indicate that there is a threshold value for the microstructure transition from a- to μc-Si. The threshold is found to be R ≈ 2 at Ts = 250°C and Ts ≈ 200°C at R=3. The IR absorption of Si-H at 640 cm-1 was used to calculate the hydrogen content, CH. CH decreased monotonically when either R or Ts increased. The Si-H stretching mode contains two peaks at 2000 and 2090 cm-1. The ratio of the integral absorption peaks I2090/(I2090+I2090) showed a sudden increase at the threshold of microcrystallinity. At the same threshold, the PL features also indicate a sudden change from a- to μc-Si., i.e. the low energy PL band becomes dominant and the PL total intensity decreases. We attribute the above IR and PL changes to the contribution of microcrystallinity, especially the c-Si gain-boundaries.

21,22-Disubstituted 18α,19βH-Ursane Derivatives with Oxabicyclooctane System in Ring E

1993 ◽  
Vol 58 (1) ◽  
pp. 173-190 ◽  
Author(s):  
Eva Klinotová ◽  
Jiří Klinot ◽  
Václav Křeček ◽  
Miloš Buděšínský ◽  
Bohumil Máca
Keyword(s):  
Spectral Data ◽  
Spin Systems ◽  
Coupling Constants ◽  
Complete Analysis ◽  
Nmr Spectrum ◽  
Proton Proton ◽  
H Nmr ◽  
Proton Coupling ◽  
C Nmr

Reaction of 3β-acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) and 20β,28-epoxy-21,22-dioxo-19α,19βH-ursan-3β-yl acetate (IIIb) with diazomethane afforded derivatives XII-XIV with spiroepoxide group in position 21 or 22, which were further converted into hydroxy derivatives XV and XVII. Ethylene ketals VIII-X were also prepared. In connection with the determination of position and configuration of the functional groups at C(21) and C(22), the 1H and 13C NMR spectral data of the prepared compounds are discussed. Complete analysis of two four-spin systems in the 1H NMR spectrum of bisethylenedioxy derivative Xb led to the proton-proton coupling constants from which the structure with two 1,4-dioxane rings condensed with ring E, and their conformation, was derived.

scholarly journals Biotin-Containing Third Generation Glucoheptoamidated Polyamidoamine Dendrimer for 5-Aminolevulinic Acid Delivery System

2021 ◽  
Vol 22 (4) ◽  
pp. 1982 ◽  
Author(s):  
Aleksandra Kaczorowska ◽  
Małgorzata Malinga-Drozd ◽  
Wojciech Kałas ◽  
Marta Kopaczyńska ◽  
Stanisław Wołowiec ◽  
...  
Keyword(s):  
Reactive Oxygen Species ◽  
Aminolevulinic Acid ◽  
Reactive Oxygen ◽  
Pamam Dendrimer ◽  
Variable Number ◽  
Amide Bond ◽  
Oxygen Species ◽  
Nmr Spectrum ◽  
Guest Molecules ◽  
Amine Groups

Polyamidoamine PAMAM dendrimer generation 3 (G3) was modified by attachment of biotin via amide bond and glucoheptoamidated by addition of α-D-glucoheptono-1,4-lacton to obtain a series of conjugates with a variable number of biotin residues. The composition of conjugates was determined by detailed 1-D and 2-D NMR spectroscopy to reveal the number of biotin residues, which were 1, 2, 4, 6, or 8, while the number of glucoheptoamide residues substituted most of the remaining primary amine groups of PAMAM G3. The conjugates were then used as host molecules to encapsulate the 5-aminolevulinic acid. The solubility of 5-aminolevulinic acid increased twice in the presence of the 5-mM guest in water. The interaction between host and guest was accompanied by deprotonation of the carboxylic group of 5-aminolevulinic acid and proton transfer into internal ternary nitrogen atoms of the guest as evidenced by a characteristic chemical shift of resonances in the 1H NMR spectrum of associates. The guest molecules were most likely encapsulated inside inner shell voids of the host. The number of guest molecules depended on the number of biotin residues of the host, which was 15 for non-biotin-containing glucoheptoamidated G3 down to 6 for glucoheptoamidated G3 with 8 biotin residues on the host surface. The encapsulates were not cytotoxic against Caco-2 cells up to 200-µM concentration in the dark. All encapsulates were able to deliver 5-aminolevulinic acid to cells but aqueous encapsulates were more active in this regard. Simultaneously, the reactive oxygen species were detected by staining with H2DCFDA in Caco-2 cells incubated with encapsulates. The amount of PpIX was sufficient for induction of reactive oxygen species upon 30-s illumination with a 655-nm laser beam.

scholarly journals Protein–Ligand Binding Volume Determined from a Single 2D NMR Spectrum with Increasing Pressure

2021 ◽  
Author(s):  
Gediminas Skvarnavičius ◽  
Zigmantas Toleikis ◽  
Vilma Michailovienė ◽  
Christian Roumestand ◽  
Daumantas Matulis ◽  
...  
Keyword(s):  
Ligand Binding ◽  
2D Nmr ◽  
Nmr Spectrum
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