Bestimmung kleiner Mengen von Beimengungen in Wasserstoff und die Bereitung von reinem Wasserstoff mit der Durchflu?-Sorptionsmethode

Zusammenfassung Es wurde über die analytische Bestimmung von Spurenbeimengungen in elektrolytischem Wasserstoff mittels der Methode der Wärmedesorption, sowie über die Bereitung von reinem Gas mit der Durchfluß-Sorptionsmethode berichtet. Für diese Zwecke wurde eine Apparatur für Durchfluß-Sorptionsmessungen entwickelt, ihre Funktion erprobt und es wurden geeignete Bedingungen für die analytische und die präparative Arbeit festgestellt.Die vorliegende Arbeit wurde auf der Konferenz über Gaschromatographie am 2. Juni 1960 in Ostrava (Tschechoslowakei) vorgetragen.     

Electrochemical determination of lead and glutathione in a plant cell culture

In this work we established differential pulse anodic stripping voltammetry (DPASV) as the tool for analysis of lead in the plant cell culture. For the cultivation procedure, lead in Pb(II)-ethylenediaminetetraacetic acid (Pb-EDTA) chelate has been used. The detection limit of lead was found at 500 pM in phosphate buffer (pH 5.5), and 100 nM in prepared cells intracellular extract (20 pg Pb(II)/mg cells). For determination of cysteine-rich peptides, voltammetry in differential mode (DPV) in cobalt(III)-containing ammonia buffer (Brdicka reaction) was used. In this short communication, we present suitable voltammetric techniques for the physiological study of lead and thiols in plant cell culture.     

Regioselective syntheses, structural characterization, and electron ionization mass spectrometric behavior of regioisomeric 2,3-disubstituted 2-imino-1,3-thiazolidin-4-ones

The regioselective syntheses of 3-alkyl(aryl)-2-(anthracen-9'-ylimino)-1,3-thiazolidin-4-ones (2) and 2-alkyl(aryl)imino-3-(anthracen-9'-yl)-1,3-thiazolidin-4-ones (3) from N-(anthracen-9-yl)-N'-alkyl(aryl)thioureas were accomplished effectively using methyl bromoacetate and bromoacetyl bromide, respectively. Detailed structural characteristics were confirmed mainly by NMR techniques. The mass spectrometric behavior of the resulting sets of compounds of known structures was shown to be characteristic for each set. Some interesting fragmentation pathways involving the transfer and rearrangements of various moieties were also revealed, as well as regioisomerization for particular substituent-specific fragmentations.     

Simultaneous femtomole determination of cysteine, reduced and oxidized glutathione, and phytochelatin in maize (Zea mays L.) kernels using high-performance liquid chromatography with electrochemical detection

Thiol compounds such as cysteine (Cys), reduced (GSH) and oxidized (GSSG) gluathione, and phytochelatins (PCs) play an important role in heavy metal detoxification in plants. These thiols are biological active compounds whose function is elimination of oxidative stress in plant cells. The aim of our work was to optimise sensitive and rapid method of high-performance liquid chromatography coupled with electrochemical detector (HPLC-ED) for determination of the abovementioned thiol compounds in maize (Zea mays L.) kernels. New approach for evaluation of HPLC-ED parameters is described. The most suitable isocratic mobile phase for the separation and detection of Cys, GSH, GSSG and PC2 consisted of methanol (MeOH) and trifluoroacetic acid (TFA). In addition, the influence of concentrations of TFA and ratio of MeOH:TFA on chromatographic separation and detection of the thiol compounds were studied. The mobile phase consisting from methanol and 0.05% (v/v) TFA in ratio 97:3 (%; v/v) was found the most suitable for the thiol compounds determination. Optimal flow rate of the mobile phase was 0.18 ml min(-1) and the column and detector temperature 35 degrees C. Hydrodynamic voltammograms of all studied compounds was obtained due to the selection of the most effective working electrodes potentials. Two most effective detection potentials were selected: 780 mV for the GSSG and PC2 and 680 mV for determination of Cys and GSH. The optimised HPLC-ED method was capable to determine femtomole levels of studied compounds. The detection limits (3 S/N) of the studied thiol compounds were for cysteine 112.8 fmol, GSH 63.5 fmol, GSSG 112.2 fmol and PC2 2.53 pmol per injection (5 microl). The optimised HPLC-ED method was applied to study of the influence of different cadmium concentrations (0, 10 and 100 microM Cd) on content of Cys, GSH, GSSG and PC2 in maize kernels. According to the increasing time of Cd treatment, content of GSH, GSSG and PC2 in maize kernels increased but content of Cys decreased. Decreasing Cys concentration probably relates with the increasing GSH and phytochelatins synthesis.     

Phase-pure nanocrystalline Li<Subscript>4</Subscript>Ti<Subscript>5</Subscript>O<Subscript>12</Subscript> for a lithium-ion battery

Phase-pure nanocrystalline Li₄Ti₅O₁₂ with BET surface areas between 183 and 196 m²/g was prepared via an improved synthetic protocol from lithium ethoxide and titanium(IV) butoxide. The phase purity was proved by X-ray powder diffraction, Raman spectroscopy and cyclic voltammetry. Thin-film electrodes were prepared from two nanocrystalline samples of Li₄Ti₅O₁₂ and one microcrystalline commercial sample. Li-insertion behavior of these electrodes was related to the particle size.Presented at the 3rd International Meeting on Advanced Batteries and Accumulators, 16–20 June 2002, Brno, Czech Republic     

Separation of the homologous series of methylcyclopolysiloxanes, methylhydrocyclopolysiloxanes, methylethylhydrocyclopolysiloxanes and linear methylpolysiloxanes by means of gas-liquid chromatography

Summary A column loaded with 23% of linear polydimethylsiloxane (molecular weight 800 000) on Chromosorb W is suitable for the simultaneous gas-chromatographic separation of the homologous series of methylcyclopolysiloxanes, methylcyclopolysiloxanes having one methylhydrosiloxane or one ethylhydrosiloxane unit in the ring and of linear methylsiloxanes. The chromatographic behaviour of methylethylhydrocyclosiloxane compounds with one or two ethylhydride groups in the ring is described for the first time.

---

Zusammenfassung Zur gas-chromatographischen Trennung homologer Reihen von Methylcyclopolysiloxanen und ihrer Äthylhydro- und Methylhydroderivate wird eine Säule benutzt, die 23% eines linearen Polydimethylsiloxan-Polymeren (M.G. 800000) auf Chromosorb W enthält. Das chromatographische Verhalten von Methyläthylhydrosiloxan-Verbindungen, die eine oder zwei Äthylhydridgruppen im Ring enthalten, wird beschrieben.

     

Maximally non-hamiltonian graphs of girth 7

We describe a sufficient condition for graphs used in a construction of Thomassen (which yields hypohamiltonian graphs) to produce maximally non-hamiltonian (MNH) graphs as well. Then we show that the Coxeter graph fulfils this sufficient condition, and thus applying the Thomassen's construction to multiple copies of the Coxeter graph yields infinitely many MNH graphs with girth 7. So far, the Coxeter graph was the only known example of a MNH graph of girth 7; also no MNH graph of girth greater than 7 has been found yet. Finally, the Isaacs' flower snarksJ _k for oddk 5 are shown to fulfil (for certain vertices) this sufficient condition as well.The research of author was partially supported by Grant No. 2/1138/94 Computational models, algorithms and complexity of Slovak Academy of Sciences and by EC Cooperative Action IC1000 Algorithms for Future Technologies (Project ALTEC)     

A note on some relations among special sums of reciprocals modulo <Emphasis Type="Italic">p</Emphasis>

In this note the sums s(k, N) of reciprocals are investigated, where p is an odd prime, N, k are integers, p does not divide N, N ≥ 1 and 0 ≤ k ≤ N − 1. Some linear relations for these sums are derived using “logarithmic property” and Lerch’s Theorem on the Fermat quotient. Particularly in case N = 10 another linear relation is shown by means of Williams’ congruences for the Fibonacci numbers. Published results were acquired using the subsidization of the Ministry of Education, Youth and Sports of the Czech Republic, research plan MSM 0021630518 “Simulation modeling of mechatronic systems”.     

Spectroelectrochemistry of carbon nanostructures.

This review is focused on charge-transfer reactions at carbon nanotubes and fullerenes. The spectroelectrochemistry of fullerenes deals with the spin states of fullerenes, the role of mono-anions and the reactivity of higher charged states in C60. The optical (Vis-NIR) spectroelectrochemistry of single-walled carbon nanotubes (SWNTs) follows changes in the allowed optical transitions among the Van Hove singularities. The Raman spectroelectrochemistry of SWNT benefits from strong resonance enhancement of the Raman scattering. Here, both semiconducting and metallic SWNTs are analyzed using the radial breathing mode (RBM) and G-modes as well as the second order (D, G') and intermediate frequency modes. Raman spectroelectrochemistry of SWNT allows the addressing of index-identified tubes and even single isolated nanotubes. Optical and Raman spectroelectrochemistry of fullerene peapods, C60@SWNT and C70@SWNT indicates effective shielding of the intratubular fullerene (peas). The most striking effect in the spectroelectrochemistry of peapods is the so-called "anodic Raman enhancement" of intratubular C60. Double-walled carbon nanotubes (DWNTs) give a specific spectroscopic response in Vis-NIR spectroelectrochemistry for the inner and the outer tube. They are better distinguishable by Raman spectroelectrochemistry which allows a precise tracing of the specific doping response of outer/inner tubes.