A modified apparatus for determination of carbon in metals by the low pressure method

The low pressure method of determination of carbon in metals and alloys was modified to include certain new techniques. An isopentane slush bath dispensed with the use of liquid oxygen and the usual McLeod gauge was replaced by a differential oil manometer, which increased the sensitivity. As little as 5 μg of carbon in CaCO₃-quartz standards could be determined with a coefficient of variation of 16.0% which improved to 3.3% at the 100-μg level. The apparatus was used for the determination of carbon in metals such as uranium, zirconium and iron and in steels and cupronickel alloy.     

Thermal decompositions of sulphosalicylates of MG(II), CA(II) and ZN(II)

The thermal decompositions of the sulphosalicylates of Mg(II), Ca(II) and Zn(II) have been investigated by means of TG and DTA. The preparation and analysis of these compounds are included. The possible decomposition reactions in the various stages and the final decomposition products are discussed.     

Measurement of thermal constants of calcium chromite by Laser Flash method

Calcium chromite, CaCr₂O₄, was prepared and its purity and stoichiometry were ascertained by chemical analysis and X-ray diffraction methods. The thermal diffusivity, specific heat capacity and thermal conductivity of calcium chromite were measured by Laser Flash method using an Ulvac-Sinku Riko TC-3000 series instrument in the temperature range of 298 to 1100 K. The heat capacity data were utilised to calculate the thermodynamic parametersenthalpy increments, entropy increments and free energy increments—in the above temperature range.

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Zusammenfassung Kalziumchromit, CaCr₂O₄, wurde hergestellt und seine Reinheit und stöchiometrische Zusammensetzung mit Hilfe chemischer Analyse und Röntgendiffraktionsmethoden ermittelt. Anhand eines Ulyac-Sinku Riko TC-3000 Gerätes wurde mit Laser Flash Verfahren die Temperaturleitfähigkeit, die spezifische Wärmekapazität und die Wärmeleitfähigkeit von Kalziumchromit im Temperaturbereich 298–1100 K bestimmt. Die Wärmekapazitätsdaten wurden zur Berechnung der thermodynamischen Größen (Enthalpie-, Entropie-, Freie Energieänderung) in obigem Temperaturbereich benutzt.

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CaCr₂O₄, . , - TC-3000, 298–1100K , . , , .

     

Acid–base chemistry at the single ion limit

We present the results of acid–base experiments performed at the single ion (H⁺ or OH⁻) limit in ∼6 aL volume nanopores incorporating electrochemical zero-mode waveguides (E-ZMWs). At pH 3 each E-ZMW nanopore contains ca. 3600H⁺ ions, and application of a negative electrochemical potential to the gold working electrode/optical cladding layer reduces H⁺ to H₂, thereby depleting H⁺ and increasing the local pH within the nanopore. The change in pH was quantified by tracking the intensity of fluorescein, a pH-responsive fluorophore whose intensity increases with pH. This behavior was translated to the single ion limit by changing the initial pH of the electrolyte solution to pH 6, at which the average pore occupancy 〈n〉_pore ∼3.6H⁺/nanopore. Application of an electrochemical potential sufficiently negative to change the local pH to pH 7 reduces the proton nanopore occupancy to 〈n〉_pore ∼0.36H⁺/nanopore, demonstrating that the approach is sensitive to single H⁺ manipulations, as evidenced by clear potential-dependent changes in fluorescein emission intensity. In addition, at high overpotential, the observed fluorescence intensity exceeded the value predicted from the fluorescence intensity-pH calibration, an observation attributed to the nucleation of H₂ nanobubbles as confirmed both by calculations and the behavior of non-pH responsive Alexa 488 fluorophore. Apart from enhancing fundamental understanding, the approach described here opens the door to applications requiring ultrasensitive ion sensing, based on the optical detection of H⁺ population at the single ion limit.

Visualizing dynamic change in the number of protons during electroreduction of protons in attoliter volume zero-mode waveguides.     

Structural and magnetic studies on spark plasma sintered SmCo5/Fe bulk nanocomposite magnets

SmCo₅+x wt% Fe (x=0$x=0$, 5 and 10) nanocomposite powders were synthesized by mechanical milling and were consolidated into bulk shape by spark plasma sintering (SPS) technique. The evolution of structure and magnetic properties were systematically investigated in milled powders as well as in SPS samples. A maximum coercivity of 8.9 kOe was achieved in spark plasma sintered SmCo₅+5 wt% Fe sample. The exchange spring interaction between the hard and soft magnetic phases was evaluated using δM–H measurements and the analysis revealed that the SPS sample containing 5 wt% Fe had a stronger exchange coupling between the magnetic phases than that of the sample with10 wt% Fe.     

Enhanced Thermal Oxidation Stability of Reduced Graphene Oxide by Nitrogen Doping

Nitrogen‐doped reduced graphene oxide (N‐doped RGO) samples with a high level of doping, up to 13 wt. %, have been prepared by annealing graphene oxide under a flow of pure ammonia. The presence of nitrogen within the structure of RGO induces a remarkable increase in the thermal stability against oxidation by air. The thermal stability is closely related with the temperature of synthesis and the nitrogen content. The combustion reaction of nitrogen in different coordination environments (pyridinic, pyrrolic, and graphitic) is analyzed against a graphene fragment (undoped) from a thermodynamic point of view. In agreement with the experimental observations, the combustion of undoped graphene turns out to be more spontaneous than when nitrogen atoms are present.