Abstract: Nuclear Magnetic Resonance (NMR) spectroscopy is an indispensable technique used in structure determination of small and macromolecules to study their physical properties, elucidation of characteristic interactions, dynamics and thermodynamic processes. Quantum mechanics defines the theoretical description of NMR spectroscopy and treatment of the dynamics of nuclear spin systems. The phenomenon of residual dipolar coupling (RDCs) has become a routine tool for accurate structure determination by providing global orientation information of magnetic dipole-dipole interaction vectors within a common reference frame. This offers accessibility of distance-independent angular information and insights to local relaxation. The measurement of RDCs requires an anisotropic orientation medium for the molecules to partially align along the magnetic field. This can be achieved by introduction of liquid crystals or attaching a paramagnetic center. Although anisotropic paramagnetic tags continue to mark achievements in the biomolecular NMR of large proteins, its application in small organic molecules remains unspread. Here, we propose a strategy for the synthesis of a lanthanide tag and the measurement of RDCs in organic molecules using paramagnetic lanthanide complexes.
Abstract: The objective of this study was to synthesize and
characterize the poly(alkenoic acid)s with different molecular
structures, use these polymers to formulate a dental cement
restorative, and study the effect of molecular structures on reaction
kinetics, viscosity, and mechanical strengths of the formed polymers
and cement restoratives. In this study, poly(alkenoic acid)s with
different molecular structures were synthesized. The purified
polymers were formulated with commercial Fuji II LC glass fillers to
form the experimental cement restoratives. The reaction kinetics was
studied via 1HNMR spectroscopy. The formed restoratives were
evaluated using compressive strength, diametral tensile strength,
flexural strength, hardness and wear-resistance tests. Specimens were
conditioned in distilled water at 37oC for 24 h prior to testing. Fuji II
LC restorative was used as control. The results show that the higher
the arm number and initiator concentration, the faster the reaction
was. It was also found that the higher the arm number and branching
that the polymer had, the lower the viscosity of the polymer in water
and the lower the mechanical strengths of the formed restorative. The
experimental restoratives were 31-53% in compressive strength, 37-
55% in compressive modulus, 80-126% in diametral tensile strength,
76-94% in flexural strength, 4-21% in fracture toughness and 53-96%
in hardness higher than Fuji II LC. For wear test, the experimental
restoratives were only 5.4-13% of abrasive and 6.4-12% of attritional
wear depths of Fuji II LC in each wear cycle. The aging study also
showed that all the experimental restoratives increased their strength
continuously during 30 days, unlike Fuji II LC. It is concluded that
polymer molecular structures have significant and positive impact on
mechanical properties of dental cement restoratives.
Abstract: High Resolution NMR Spectroscopy offers unique screening capabilities for food quality and safety by combining non-targeted and targeted screening in one analysis.
The objective is to demonstrate, that due to its extreme reproducibility NMR can detect smallest changes in concentrations of many components in a mixture, which is best monitored by statistical evaluation however also delivers reliable quantification results.
The methodology typically uses a 400 MHz high resolution instrument under full automation after minimized sample preparation.
For example one fruit juice analysis in a push button operation takes at maximum 15 minutes and delivers a multitude of results, which are automatically summarized in a PDF report.
The method has been proven on fruit juices, where so far unknown frauds could be detected. In addition conventional targeted parameters are obtained in the same analysis. This technology has the advantage that NMR is completely quantitative and concentration calibration only has to be done once for all compounds. Since NMR is so reproducible, it is also transferable between different instruments (with same field strength) and laboratories. Based on strict SOP`s, statistical models developed once can be used on multiple instruments and strategies for compound identification and quantification are applicable as well across labs.
Abstract: Pure phase gallosilicate nitrite sodalite has been synthesized in a single step by low temperature (373 oK) hydrothermal technique. The product obtained was characterized using a combination of techniques including X-ray powder diffraction, IR, Raman spectroscopy, SEM, MAS NMR spectroscopy as well as thermogravimetry. Sodalite with an ideal composition was obtained after synthesis at 3730K and seven days duration using alkaline medium. The structural features of the Na8[GaSiO4]6(NO2)2 sodalite were investigated by IR, MAS NMR spectroscopy of 29Si and 23Na nuclei and by Reitveld refinement of X-ray powder diffraction data. The crystal structure of this sodalite has been refined in the space group P 4 3n; with a cell parameter 8.98386Å, V= 726.9 Å, (Rwp= 0.077 and Rp=0.0537) and Si-O-Ga angle is found to be 132.920 . MAS NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. The surface area of single entity with stoichiometry Na8[GaSiO4]6(NO2)2 was found to be 8.083 x10-15 cm2/g.
Abstract: The field of polymeric biomaterials is very important
from the socio-economical viewpoint. Synthetic carbohydrate
polymers are being increasingly investigated as biodegradable,
biocompatible and biorenewable materials. The aim of this study was
to synthesize and characterize some derivatives based on D-mannose.
D-mannose was chemically modified to obtain 1-O-allyl-2,3:5,6-di-
O-isopropylidene-D-mannofuranose and 1-O-(2-,3--epoxy-propyl)-
2,3:5,6-di-O-isopropylidene-D-mannofuranose.
The chemical structure of the resulting compounds was
characterized by FT-IR and NMR spectroscopy, and by HPLC-MS.
Abstract: Hydrate phase equilibria for the binary CO2+water and
CH4+water mixtures in silica gel pore of nominal diameters 6, 30, and
100 nm were measured and compared with the calculated results based
on van der Waals and Platteeuw model. At a specific temperature,
three-phase hydrate-water-vapor (HLV) equilibrium curves for pore
hydrates were shifted to the higher-pressure condition depending on
pore sizes when compared with those of bulk hydrates. Notably,
hydrate phase equilibria for the case of 100 nominal nm pore size were
nearly identical with those of bulk hydrates. The activities of water in
porous silica gels were modified to account for capillary effect, and
the calculation results were generally in good agreement with the
experimental data. The structural characteristics of gas hydrates in
silica gel pores were investigated through NMR spectroscopy.
Abstract: Five lignin samples were fractionated with
Acetone/Water mixtures and the obtained fractions were subjected to
extensive structural characterization, including Fourier Transform
Infrared (FT-IR), Gel permeation Chromatography (GPC) and
Phosphorus-31 NMR spectroscopy (31P-NMR). The results showed
that for all studied lignins the solubility increases with the increment
of the acetone concentration. Wheat straw lignin has the highest
solubility in 90/10 (v/v) Acetone/Water mixture, 400 mg lignin being
dissolved in 1 mL mixture. The weight average molecular weight of
the obtained fractions increased with the increment of acetone
concentration and thus with solubility. 31P-NMR analysis based on
lignin modification by reactive phospholane into phosphitylated
compounds was used to differentiate and quantify the different types
of OH groups (aromatic, aliphatic, and carboxylic) found in the
fractions obtained with 70/30 (v/v) Acetone/Water mixture.