Sample preparation techniques for the determination of natural 15N/14N variations in amino acids by gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS)

In order to identify natural nitrogen isotope variations of biologically important amino acids four derivatization reactions (t-butylmethylsilylation, esterification with subsequent trifluoroacetylation, acetylation and pivaloylation) were tested with standard mixtures of 17 proteinogenic amino acids and plant (moss) samples using GC-C-IRMS. The possible fractionation of the nitrogen isotopes, caused for instance by the formation of multiple reaction products, was investigated. For biological samples, the esterification of the amino acids with subsequent trifluoroacetylation is recommended for nitrogen isotope ratio analysis. A sample preparation technique is described for the isotope ratio mass spectrometric analysis of amino acids from the non-protein (NPN) fraction of terrestrial moss. ¹⁴N/¹⁵N ratios from moss (Scleropodium spec.) samples from different anthropogenically polluted areas were studied with respect to ecotoxicologal bioindication.     

ZnO–SnO2 branch–stem nanowires based on a two-step process: Synthesis and sensing capability

ZnO–SnO₂ branch–stem nanostructures were realized on a basis of a two-step process. In step 1, SnO₂-stem nanowires were synthesized. In step 2, ZnO-branch nanowires were successfully grown on the SnO₂-stem nanowires through a simple evaporation technique. We have pre-deposited thin Au layers on the surface of SnO₂ nanowire stems and subsequently evaporated Zn powders on the nanowires. The ZnO branches, which sprouted from the SnO₂ stems, had diameters in a range of 30–35 nm. As-synthesized branches were of single crystalline hexagonal ZnO structures. Since the branch tips were comprised of Au-containing nanoparticles, the Au-catalyzed vapor–liquid–solid growth mechanism was more likely to control the growth process of the ZnO branches. To test a potential use of ZnO–SnO₂ branch–stem nanostructures in chemical gas sensors, their sensing performances with respect to NO₂ gas were investigated, showing the promising potential in chemical gas sensors.     

Electron-ion Coulomb Bremsstrahlung in nonideal plasmas

The classical electron-ion Coulomb Bremsstrahlung process is investigated in nonideal plasmas. An effective pseudopotential model taking into account the plasma screening and collective effects is applied to describe the electron-ion interaction potential in a classical nonideal plasma. The classical straight-line trajectory method is applied to the motion of the projectile electron in order to visualize the variation of the differential Bremsstrahlung radiation cross-section (DBRCS) as a function of the scaled impact parameter, nonideal plasma parameter, projectile energy, photon energy, and Debye length. The results show that the DBRCS in ideal plasmas described by the Debye-Hückel potential is always greater than that in nonideal plasmas, i.e., the collective effects reduce the DBRCS for both the soft and hard photon cases. For large impact parameters, the DBRCS for the soft photon case is found to be always greater than that for the hard photon case. Received 1st December 1999     

Pion–Rho Meson Lagrangian in Nuclear Matter

We present an in-medium modified pion and rho meson Lagrangian which describes the pion, rho meson and the corresponding soliton properties in nuclear matter. Within the present approach pion properties in nuclear matter is closely related to the low-energy pion-nucleus scattering phenomenology. We discuss the possible modifications of rho meson properties in nuclear matter.     

First-order transitions and thermodynamic properties in the 2D Blume-Capel model: the transfer-matrix method revisited

We investigate the first-order transition in the spin-1 two-dimensional Blume-Capel model in square lattices by revisiting the transfer-matrix method. With large strip widths increased up to the size of 18 sites, we construct the detailed phase coexistence curve which shows excellent quantitative agreement with the recent advanced Monte Carlo results. In the deep first-order area, we observe the exponential system-size scaling of the spectral gap of the transfer matrix from which linearly increasing interfacial tension is deduced with decreasing temperature. We find that the first-order signature at low temperatures is strongly pronounced with much suppressed finite-size influence in the examined thermodynamic properties of entropy, non-zero spin population, and specific heat. It turns out that the jump at the transition becomes increasingly sharp as it goes deep into the first-order area, which is in contrast to the Wang–Landau results where finite-size smoothing gets more severe at lower temperatures.     

Surface redox induced bipolar switching of transition metal oxide films examined by scanning probe microscopy

The bipolar resistive switching mechanisms of a p-type NiO film and n-type TiO₂ film were examined using local probe-based measurements. Scanning probe-based current–voltage (I–V) sweeps and surface potential/current maps obtained after the application of dc bias suggested that resistive switching is caused mainly by the surface redox reactions involving oxygen ions at the tip/oxide interface. This explanation can be applied generally to both p-type and n-type conducting resistive switching films. The contribution of oxygen migration to resistive switching was also observed indirectly, but only in the cases where the tip was in (quasi-) Ohmic contact with the oxide.     

Synthesis and characterization of TiO2/Ag/polymer ternary nanoparticles via surface-initiated atom transfer radical polymerization

We report on the novel ternary hybrid materials consisting of semiconductor (TiO₂), metal (Ag) and polymer (poly(oxyethylene methacrylate) (POEM)). First, a hydrophilic polymer, i.e. POEM, was grafted from TiO₂ nanoparticles via the surface-initiated atom transfer radical polymerization (ATRP) technique. These TiO₂-POEM brush nanoparticles were used to template the formation of Ag nanoparticles by introduction of a AgCF₃SO₃ precursor and a NaBH₄ aqueous solution for reduction process. Successful grafting of polymeric chains from the surface of TiO₂ nanoparticles and the in situ formation of Ag nanoparticles within the polymeric chains were confirmed using transmission electron microscopy (TEM), UV-vis spectroscopy, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). FT-IR spectroscopy also revealed the specific interaction of Ag nanoparticles with the CO groups of POEM brushes. This study presents a simple route for the in situ synthesis of both metal and polymer confined within the semiconductor, producing ternary hybrid inorganic-organic nanomaterials.     

Proton relaxation times in human red bone marrow by volume selective magnetic resonance spectroscopy

In hematological diseases the composition of red bone marrow shows alterations. The relaxation timesT ₁ andT ₂ of water and lipids in human hemopoietic bone marrow of 14 normal volunteers and 10 patients with acute leukemia and bone marrow carcinosis are determined using a double spin echo spectroscopy sequencein vivo. The volumes of interest (VOI) of (13 mm)³ in the center of vertebral bodies are examined using different measurement parameters. ForT ₁ measurements an inversion-recovery method is used.T ₂ is evaluated from spectra with differentTE. T ₁ (water) is found in a range between 1000 and 1700 ms,T ₁ (lipids) in a range between 260 and 320 ms in healthy volunteers.T ₂ (water) is determined between 32 and 65 ms. In some cases phase distortions of the water signals occur in the spectra. Water flow within the VOI may be a possible reason.T ₂ (lipids) is evaluated between 73 and 91 ms. The patients with acute leukemia exhibit clearly reduced lipid signals in their spectra. Lipid relaxation times could not be determined in these cases.T ₂ (water) is prolonged in acute leukemia to 51–98 ms.T ₁ (water) was not significantly different from values of healthy volunteers in our measurements. Results are discussed in comparison to relaxometric data from imaging and STEAM spectroscopic methods of other authors.     

15N/14N Analysis of Amino Acids with GC-C-IRMS - Methodical Investigations and Ecotoxicological Applications

Abstract

In order to perform the ¹⁵N/¹⁴N analysis of amino acids using a gas chromatograph and isotope ratio mass spectrometer linked up via a combustion interface (GC-C-IRMS), the amino acids must be derivatized. Tert-butyldimethylsilylation is examined using various techniques (direct conversion to nitrogen gas, ConFlo-IRMS [1], GC-C-IRMS [2]) and subsequently applied to isotopic characterization of amino acids from wheat protein hydrolyzate obtained from plants exposed to ozone. The method provides a reliable tool for studying ecotoxicological effects on plants at a molecular level in addition to the investigation of the natural variations of different N fractions.