Biomedical subjects

Zbigniew Olejniczak

Publications and source records attributed to Zbigniew Olejniczak.

3 recordsLinked to original sources

PubMed2005

Missing first points and phase artifact mutually entangled in FT NMR data--noniterative solution.

Even moderate distortion at the beginning of the NMR signal contributes significantly to the baseline in the reciprocal domain, when the FID-type experiment is considered. If constant phase artifact is also involved, the net problem cannot be resolved accurately, according to its constituents considered in separation. This issue is particularly severe for powder patterns in solids, featuring complex broadband spectra, which substantially mask the baseline behavior. The complete correction procedure should intrinsically deal with both artifacts, due to the mutual dependency. The aim of this work is to indicate the possibility for the exact treatment of baseline and constant phase artifacts together, providing precise measure whether the correction is successful. We have found the analytical, noniterative solution for this coupled problem in the closed form. In this paper, we introduce the correction efficiency concept in order to have the measure for the correction reliability of the resulting spectrum. Relevant efficiency parameter eta is the subject for quantitative analysis resulting in certain constraints for the measurement. We have determined exemplar trends for this parameter as a function of experimental variables such as signal-to-noise ratio and missing points number. The method is model-free and drawn from the origin of the baseline artifact; therefore has potential to work for a broad range of applications.

Journal Article↗

PubMed2004

Preparation and surface properties of low-density gels synthesized using prepolymerized silica precursors.

Properties of silica xerogels and aerogels synthesized using a number of prepolymerized silica precursors were probed by 29Si magic-angle spinning (MAS) NMR spectroscopy, the small-angle X-ray scattering (SAXS) method, the nitrogen adsorption method, and transmission electron microscopy (TEM) to show that xerogels with attractive textural properties can easily be prepared using this type of precursors and the conventional one-step, base procedure. Pore sizes and overall pore volumes in these materials can be notably larger than those in the corresponding materials synthesized using tetraethoxysilane. This positive effect stems from the stronger structure of the polymeric network due to a higher degree of silica condensation on one side and a larger thickness of polymeric chains on the other. The thorough investigations of the fine silica structure demonstrate, however, that the relationship between the microstructure of the silica precursor and the micro- and macrostructures of dry gels is complex and the use of more condensed precursors favors, but does not necessarily ensure, more porous dry materials, under the same reaction conditions. Ethyl silicate 40 may be recommended as a low-cost precursor suitable for applications in this situation.

Magnetic Resonance Spectroscopy↗

PubMed2002

Location of the H atoms in ammonium persulphate by deuteron NMR. Verification by X-ray diffraction.

It is demonstrated that H atoms can be located by the spectroscopic method of deuteron NMR. The requirement is that the 'heavy-atom' positions are known from diffraction studies. The technique allows an accuracy of the order of 0.01 A. The compound studied is ammonium persulphate (APS), (NH(4))(2)S(2)O(8). APS crystallizes in space group P2(1)/n with lattice parameters a = 6.1340 (2), b = 7.9324 (3), c = 7.7541 (3) A and beta = 94.966 (1) degrees at T = 118 K. In perdeuterated crystals of APS, only one of the deuterons of every ND(4)(+) ion becomes localized at low temperatures. Therefore, most of this work uses samples with 9% deuteration. In such crystals, most of the ammonium ions containing deuterons come in the form of NDH(3)(+) ions. At T < 25 K, the single deuteron of these ions becomes localized in one of four equilibrium sites. The deuteron site occupancies differ from each other and are measured at 17 K. The deuterons are located in three steps. (i) The deuteron quadrupole-coupling (QC) tensors are measured at 17 K. Their unique principal directions are identified, as is well justified, with the N-D bond directions. (ii) The fine structure of a deuteron NMR line is analyzed in terms of the magnetic dipole-dipole interactions between all nuclei in an NDH(3)(+) ion to obtain the N-D and D-H internuclear distances. (iii) An empirical relation between deuteron QC constants and D.O distances in N-D.O hydrogen bonds is exploited to assign the N-D bond vectors to the appropriate N atom of which there are four in the unit cell. The results are highly relevant for an understanding of the complex tunnelling and stochastic reorientation dynamics of the ammonium ions in APS. They are verified by a complementary X-ray diffraction study.

Journal Article↗