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EN
A new series of chloride transition metal complexes containing a diethyl (pyridyn-2-ylmethyl) phosphate (2-pmOpe) ligand, of the general formula [M(2-pmOpe)2Cl2] (M = Cu, Ni, Mn) and [M(2-pmOpe)Cl2] (M = Co, Zn), were synthesized and studied. The stoichiometry and stereochemistry of the compounds were confirmed by elemental analysis, spectroscopic and magnetic studies. The ligand containing two donor atoms, heterocyclic pyridyl nitrogen and phosphoryl oxygen atoms, binds in a didentate chelate manner in all complexes. The octahedral (Cu, Ni, Mn) and tetrahedral (Co, Zn) coordination sphere complete chloride ions included in coordination. The magnetic behaviour (for paramagnetic centres) and spectroscopic analyses of the complexes indicate a mononuclear structure and suggest existence of a very weak exchange coupling between the metal centres in the crystal lattice.
EN
he present technical status and physical properties of the gas-liner pinch device in Bochum are presented and discussed. This comprises spectroscopic as well as diagnostic achievements. A short review on the measurements performed at this light source will also be given.
EN
A helium plasma produced in a 82 kJ theta pinch discharge has been seeded with carbon ions by a carbon solid rod positioned on the axis. The first shock front of the discharge ablates carbon atoms from the solid surface which are ionized and interact with the plasma. Some shock front properties (namely thickness, compression velocity and its shape) were analyzed with an ICCD-camera system taking 2-dimensional photos of the plasma continuum emitted along the axis with a time duration of 100 ns. While the influence on the shape was not found, the temporal behaviour was drastically changed when the rod was added. The shock front occurs earlier and compresses faster. An explanation remains to be given. Furthermore, the influence of the carbon impurities on the plasma parameters has been investigated by measuring the electron temperature and density by means of plasma spectroscopy comparing these results with those obtained from discharges in helium without rod. We found a decrease in the electron density about 500 ns after the shocked plasma has started to interact with the rod surface. Simultaneously increasing continuum emission and decreasing intensity of the HeII Pa line indicates a regime of recombination. No influence was found on the electron temperature.
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Content available remote Piezoelectric material characterization by acoustic methods
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EN
Two characterization methods of piezoelectric materials based on acoustic measurements are presented. Their main objective is to identify the entire set of electromechanical properties of piezoelectric materials from a single sample. In order to characterize new materials like single-crystals with small dimensions, the first section of the paper presents an identiffication protocol based on the study of the resonance spectra of parallelepipeds. The second characterization method is performed by means of the measurement of the transmission coefficients of plane waves propagating through an immersed plate. It is is suitable for the determination of the properties of bulk piezoelectric ceramics.
EN
Biological studies rely on measurements performed on large populations, which allow the statistic evaluation of gathered data. On the other hand, the need to precisely localize observed processes and the facts occurring in the microscale results in the need of high resolution qualitative imaging. These two approaches are complementary and without anyone of them no valuable experimental data can be gathered from studies of fluorescent dyes. Both approaches are based on common origin of laser-induced fluorescence, but due to the method of analysis they split into the quantitative (laser scanning cytometry) and qualitative (confocal microscopy) fields of research.
EN
Segregation process in binary alloys (CuPd, CoPd, AuNi) is investigated by X-ray photoelectron spectroscopy (XPS), auger electron spectroscopy (AES) and elastic peak electron spectroscopy (EPES) using the line shape analysis and the fyzzy k-nearest neighbour (fkNN) rule. Qualitative and quantitative results of the fkNN line shape analysis remain in agreement, indicating Pd and Au surface segregstion. The method investigates the values of mean escape depth (MED) and mean penetration depth (MPD) depending on selected electron kinetics energies (KE) in the range between few to several Angstroms. New application of the fkNN rule for EPES was shown.
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Content available remote Spektroskopia osłabionego całkowitego odbicia w podczerwieni
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Content available remote High pressure spectroscopy of Pr3+ doped KLa(MoO4)2 crystal
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EN
Optical properties and electronic structure of Pr3+ ion in KLa0.75Pr0.25(MoO4)2 have been investigated. The standard spectroscopy (excitation and photoluminescence spectra) and the high pressure spectroscopy methods have been used. Hydrostatic pressure up to 100 kbar has been applied in diamond anvil cell. The luminescence related to the transitions from the 3P0 and 1D2 states have been measured at ambient temperature for different pressures. We have found that the pressure shifts of the observed emission lines are negative and equal to 2–3 cm–1/kbar. It is due to the changes in Slater and α, β, γ parameters and diminishing of the spin-orbit coupling constant ζ.
EN
Continuous scientific research and the increasing saturation of the medical market in Poland implements the possibilities of using advanced MR techniques including MRS in everyday practice. This method, which has so far been used primarily for research purposes, can bring measurable benefits to patients not only in terms of clarifying diagnosis and narrowing differential diagnosis, but also monitoring the course of various diseases and their treatment. Here we present the basic principles of performing and interpreting spectroscopic spectra and possible clinical applications and development prospects of MRS. The literature reviewed both Polish and foreign articles both historically and in the past 10 years. The paper presents methodological issues related to the proper performance of magnetic resonance spectroscopy (MRS) and spectral composition and the role of major metabolites, as well as current clinical applications and directions of MRS development.
EN
In the article, light absorption properties of the fuel oil are considered with a view to create basis for establish optical indicator of the type and quality of this kind of crude oil derivative, in this case the Diesel fuel. The organic solvent – n-hexane – was chosen as a solvent to prepare samples of dilutions of Diesel fuel in several oil concentration. Spectrophotometer Aqualog Horiba were applied to record the absorbance spectra in the ultraviolet and visual range of the light (from 240 to 600 nm) for each previously prepared samples. Obtained results allow concluding that the changes of absorbance occur primarily in the wavelength range from 240 nm to 355 nm. Moreover, the absorbance spectra are characterized by the characteristic sharp peak located at 270 nm for excitation wavelength. Spectra of absorbance were converted to spectra of absorption coefficient based on Lambert-Beer law. Due to the independence the absorption coefficient from the fuel concentration, this parameter could be used as a potential indicator to access composition and quality Diesel fuel used in the diesel engine system. Therefore, preliminary tests allow concluding that absorption coefficient for selected wavelength located at 270 nm could be a sensitive indicator for quick access to fuel quality.
EN
In the present study, laser-induced breakdown spectroscopy (LIBS) has been applied for the determination of chromium and cadmium contents in wastewater of different canneries surrounding by leather factories. The plasma was generated with a Q-switched Nd:YAG laser having a fundamental wavelength of 1064 nm and delivers maximum pulse energy of 180 mJ. Experimental conditions were optimized to improve the sensitivity and to get a reasonable signal from the generated plasma. The results show that the concentration of chromium and cadmium are varying in different samples depending on the incoming flow of the wastewater from factories. The results from LIBS and standard analytical technique called flame atomic absorption spectroscopy (FAAS) were compared and found in good agreement within the experimental uncertainties.
EN
Biomaterials basing on natural polysaccharides, i.e. hiauronic acid, alginate, chitosane are an alternative for already applied bioresorbable synthetic materials basing on synthetic polyhydroxy acids. Their main advantages are good accessibility, low cost, easy forming and high biocompatibility. Additionally , they are a perfect matrix for bioactive nanoparticles i.e. hydroxy apatite (HAp), tricalcium phosphate (TCP) and silica (SiO2). The work presents results of research on nanocomposite consisting of chitosane matrix (CS) modified with a nanofiller, which was natural montmorillonite (MMT). Nanocomposite foils were produced by the casting method. In order to induce better biocompatibility, the surface of the CS/MMT composite was neutralized (bath in NaOH solution). The nanocomposite foils were subjected to a bioactivity test by incubation in SBF at 37oC for 7 days. It was observed that the CS/ MMT material surface showed a local supersaturation, which was a result of apatite nucleation. The CS/ MMT nanocomposites were investigated using FT-IR ( Fourier Transform Infrared Spectroscopy) and Fourier Raman Spectroscopy. FTIR measurements o f the samples were carried out on the transmission and reflection modes. The FTIR microscopy spectra were collected using BioRad Excalibur with ATR attachment as well as microscope UMA500 equipped with MCT detector. Spectra were measure at 4 cm -1 resolution in the region from 4 000 cm -1 to 600 cm -1 . FT-Raman spectra were obtained using a FTS 6000 Bio-Rad spectrometer with Ge detector. The samples were excited with a Nd-YAG laser (1064nm). Additional all materials in all steps experiments were observed under Scanning Electron Microscopy (Nova Nano SEM). Vibrational spectroscopy methods (FT Raman and FTIR) can be used for investigation of nanocomposite foils basing on biopolymers. High sensitivity the applied spectroscopy techniques show that in the result of the neutralization of CS/ MMT foil (via incubation in NaOH solution the biopolymer chain breaks. This phenomena is visible by intensity ratio between COC/COH bands. Increase of reactivity of chitosane chain lead to entrapment of PO4+3-, which is the origin of the apatite forms nucleation process. Chemical treatment of the nanocomposite foils, i.e. NaOH washes in fluences their chemical structure and microstructure. Neutralisation of the foils is the first processing stage which precedes the potential use o fCS/ MMT foils in biomedical applications. The materials show a tendency to apatite crystallisation which may support regeneration of damaged bone tissue. The applied spectroscopic methods allowed to observe changes in the whole volume of the sample. Individual ATR measurements taken at various spectral ranges and penetration depths allow to observe subtle changes in the polymer matrix caused by chemical treatment (NaOH and SBF incubation). Results of the investigations indicate that in the CS/ MMT systems new chemical bonds and related to them vibrations appear. Quantity and quality of the interact ions is related to characteristics of the nanoparticle and the presence of forming apatite structures.
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Content available remote Study of structures and properties of ZnO-Sb2O3-P2O5-Na2O glasses
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EN
The influence of ZnO substitution by 0 – 12 wt.% Na2O on the properties of ZnO–Sb2O3–P2O5–Na2O glasses has been investigated. The structure and properties of the glasses with the composition of (13.86–x)ZnO–57.93Sb2O3–28.21P2O5-xNa2O (x = 0 – 12 wt.%) were characterized by infrared spectra (IR), X-ray diffraction and differential thermal analysis (DTA). The results of IR indicated an increase in the intensity of symmetric vibrations of P–O–P bond, which was confirmed by the improvement of water durability with the increasing amount of Na2O in the range of 0 – 10 wt.%. Substitution of 10 wt.% Na2O led to the weight loss of the glass to 5.93 mg/cm-2 after immersion in deionized water at 50 °C for 24 h. The results of XRD showed that the ability of crystallization decreased, indicating the good thermal stability of the glass. The glass containing 8 wt.% Na2O had the best properties in every respect and might be an alternative to lead based glasses for the applications, providing further composition improvement.
EN
A new series of nitrate transition metal complexes containing diethyl(pyridin-3-ylmethyl)phosphonate (3-pmpe) as a ligand, having a general formula [M(3-pmpe)2(H2O)2](NO3)2 (M = Cu, Co and Ni) and [Zn(3-pmpe)2](NO3)2 were prepared. The complexes were identified and characterized by the elemental analysis, spectroscopic and magnetic studies. Ligands containing two donor atoms, heterocyclic nitrogen and phosphoryl oxygen atoms bind in a bidentate bridging manner via the pyridine nitrogen and the phosphoryl oxygen atoms. The magnetic behaviour in the temperature range 1.8-300 K) of the Cu(II), Ni(II), Co(II) complexes as well as their spectroscopic properties suggest polymeric structure of all complexes and the existence of a weak antiferromagnetic exchange coupling between paramagnetic centres inside the dibridged linear chains [M(3-pmpe)2M]n.
EN
Aluminized melt cast formulations based on 2,4,6-trinitrotoluene (TNT) deliver an enhanced blast effect because the secondary combustion process of aluminum (Al) occurs beyond the detonation zone. A new method is introduced to assess the detonation performance and characteristics of aluminized TNT explosives on the basis of the laser-induced breakdown spectroscopy (LIBS) technique, in both air and argon (Ar) atmospheres. The plasma emissions of the prepared samples were recorded, where the atomic lines of Al, C, O and H as well as the molecular bands of AlO, CN and C2 were identified. A good discrimination and separation between the samples was possible using LIBS and principle component analysis (PCA), although they had similar atomic compositions. The quantitative calibration curve obtained using the relative intensity of Al/O was used to determine the detonation velocity/pressure and aluminum content of the TNT/Al samples. Comparisons between experimental and theoretical spectra were made using a Nelder–Mead temperature program for CN bands, which provided good agreement with the fitted spectra. Finally, CN vibrational temperatures were calculated from these spectral fittings. These temperatures have higher values in an Ar atmosphere than in an air atmosphere. Thus, increasing the oxygen concentration can decrease these temperatures in TNT/Al standard samples.
EN
Nanometer-sized powder of TiO2 is prepared by chemical methods of gel to crystalline conversion. The crystallite sizes obtained are in the range of 160? to 180 ?,as estimated by Scanning Electron Microscopic (SEM) and X-ray diffraction studies. The photocatalytic activity of this powder in the mineralization of Indanthrene Red LGG is evaluated. The maximum photocatalytic activity is observed in the system, in which the photocatalyst is used in the presence of an oxidizing agent. The effect of inorganic oxidizing species to act as an electron scavenger, thus, influencing the rate of photocatalytic degradation, is studied. Extent of degradation is followed by UV-visible and IR spectroscopy. Based on the results, a kinetic model for the degradation is proposed.
EN
The compounds of general formula [ML2](ClO4)2 [M = Cu(II), Ni(II), Co(II)]; L = diethyl 3-pyridylmethyl[N-(butyl)amino]phosphonate (3-pmape) or diethyl 4-pyridylmethyl[N-(butyl)amino]phosphonate (4-pmape) were prepared. The new complexes were identified and characterized by elemental analysis, infrared, electronic spectral studies and magnetic measurements. The complexes are sixcoordinate. Metal ions are octahedrally surrounded by two pyridine and two amine nitrogens, and two oxygens of the phosphoryl groups. The results of the magnetic studies suggest polymeric chain structure of the above complexes and indicate weak antiferromagnetic interaction between the magnetic centers. The magnetic behavior of Co(II) complexes is characteristic for cobalt(II) system with an important orbital contribution via spin-orbit coupling.
EN
A new series of the chloride and nitrate transition metal complexes containing the ligand diethyl 2-quinolylmethylphosphonate (2-qmpe) of general formula M(2-qmpe)(NO3)2 (M = Cu, Co), [Zn(2-qmpe)(H2O)2NO3]NO3ź H2O, [Ni(2-qmpe)(H2O)2NO3]NO3, M(2-qmpe)2Cl2 (M = Cu, Ni, Co, Pd) and M(2-qmpe)Cl2 (M = Co, Zn) were prepared. The complexes were identified and characterized by elemental analysis, spectroscopic and magnetic studies. Ligand containing two donor atoms, heterocyclic nitrogen and phosphoryl oxygen atoms exhibits different coordination properties. It was shown that the ligand binds in a bidentate chelate manner via the quinoline nitrogen and the phosphoryl oxygen atoms (complexes with 1:1 metal to ligand molar ratio) and it can also acts as a monodentate ligand coordinated through the nitrogen in the Pd(II) or oxygen atom in the Cu(II) and Co(II) complexes (complexes with 1:2 metal to ligand molar ratio). The magnetic behaviour of the Cu(II), Ni(II) and Co(II) and spectroscopic investigation of Zn(II) complexes suggests mononuclear structure of all the complexes and the existence of a weak intermolecular exchange coupling between magnetic centres inside crystal lattice.
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