The study of hydronium NASICON conductivity with deuterium

The ionic conductivity of the bulk phase of bonded hydronium NASICON (Hyceram^TM) was measured at equilibrium with an H₂O/N₂ and then a D₂O/N₂ atmosphere, each at 100% relative humidity and 75% relative humidity over the temperature range 25°C to 50°C. At 100% relative humidity and 25°C, the protonic system had a bulk conductivity of 5.0×10⁻⁴ S/cm and an activation energy of 17.3kJ/mole; the same sample, when deuterated, had a bulk conductivity of 2.2×10⁻⁴ S/cm and an activation energy of 19.3kJ/mole. At 75% relative humidity and 25°C, the conductivity of the protonated system decreased to 1.4×10⁻⁴S/cm with an activation energy of 24.1 kJ/mole. The deuterated sample at 75% relative humidity had a bulk conductivity of 5.4×10⁻⁵ S/cm with an activation energy of 26.0 kJ/mole. The isotope effect suggested a proton hopping (Grotthus) mechanism as the means by which the protons pass through the lattice.     

Ultrasound induced aqueous polycyclic aromatic hydrocarbon reactivity

An investigation to determine the ability of ultrasonic radiation to chemically alter polycyclic aromatic hydrocarbons (PAHs) in aqueous solution has been conducted. The data indicate that chemical alteration of PAHs can be induced under intense ultrasonic treatment. The extent and outcome of reaction is a function of irridation time and aqueous solution parameters. Reaction products were analysed by gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS). Reaction products from ultrasonic treatment of aqueous solutions of biphenyl include ortho, meta, and para-1,1 biphenols. The principal product from ultrasonic treatment of aqueous phenanthrene solutions appears to be a phenanthrene-diol. The number and composition of reaction products for both PAHs tested suggest that a free radical mechanism is likely during aqueous high intensity ultrasonic treatment. The use of ultrasound to treat PAH contaminated aqueous solutions in tandem with other methodologies appears promising. However, the toxicity of reaction products produced by treatment remains to be determined.     

The determination of the plate count for large molecules under reversed-phase gradient conditions

The true performance of HPLC columns in the gradient separation of macromolecules can be assessed by measuring the true plate count, if we know the retention factor of the analyte at the point of elution. We are demonstrating in this short communication how this can accomplished in a straightforward fashion. The procedure used here is a significant simplification over previous approaches, and enables the chromatographer to do so without complex algebra or additional experiments.     

Synthetic nanomotors in microchannel networks: directional microchip motion and controlled manipulation of cargo

We illustrate the use of catalytic nanowire motors for directional motion and microscale transport of cargo within microfluidic channel networks. The CNT-based synthetic nanomotor can propel a large cargo load at high speeds through predetermined paths and junctions of the microchannel network. The magnetic properties of the nickel-containing nanomotors offer controlled cargo manipulations, including en-route load, drag, and release. Such use of synthetic nanomachines can lead to chemically powered versatile laboratory-on-a-chip devices performing a series of tasks simultaneously or sequentially.     

Submicron scale patterning in sintered silica colloidal crystal films using a focused ion beam

Focused ion beam milling is used to fabricate micron and submicron scale patterns in sintered silica colloidal crystal films. Rectangular cavities with both solid and porous boundaries, fluidic channels, and isolation of a small number of packed spheres are patterned. The ion beam can pattern sintered films of individual submicron size spheres and create patterns that cover up to 40 mum in less than 15 min. The experiments in this work indicate that the amount of redeposited material on the surface of a milled cavity determines whether the surface will be porous or solid. FIB direct patterning has applications in colloidal crystal based lithography, integrated photonic devices, optofluidic devices, and micrototal-analytical systems.     

The application of small porous particles, high temperatures, and high pressures to generate very high resolution LC and LC/MS separations

The effect of combining sub-2 microm porous particles with elevated operating temperatures on chromatographic performance has been investigated in terms of chromatographic efficiency, productivity, peak elution order, and observed operating pressure. The use of elevated temperature in LC does not increase the obtainable performance but allows the same performance to be obtained in less time. Increasing the column temperature did allow the use of longer columns, generating column efficiencies in excess of 100,000 plates and gradient peak capacities approaching 1000. Raising the temperature increased the optimal mobile phase linear velocity, negating somewhat the pressure benefits observed by reducing the solvent viscosity. When operating at higher temperature the analyte retention is not only reduced, but the order of elution will also often change. High temperature separations allowed exotic organic modifiers such as isopropanol to be exploited for alternative selectivity and faster analysis. Finally, care must be taken when using high temperature separations to ensure that the narrow peak widths produced do not compromise the quality of data obtained from detectors such as high resolution mass spectrometers.     

Differences in preparative loadability between the charged and uncharged forms of ionizable compounds

Ionizable compounds experience a drastic difference in preparative loadability as a function of pH. It can be shown that the preparative loadability of a compound in the ionic form is by a factor of 20 or more inferior to the loadability of the same compound in the unionized form. In this paper, we demonstrate the reason for this behavior, and show practical applications of the principle.