Optimization of the design and operation of FAIMS analyzers

Field asymmetric waveform ion mobility spectrometry (FAIMS) holds significant promise for post-ionization separations in conjunction with mass-spectrometric analyses. However, a limited understanding of fundamentals of FAIMS analyzers has made their design and operation largely an empirical exercise. Recently, we developed an a priori simulation of FAIMS that accounts for both ion diffusion (including anisotropic components) and Coulomb repulsion, and validated it by extensive comparisons with FAIMS/MS data. Here it is corroborated further by FAIMS-only measurements, and applied to explore how key instrumental parameters (analytical gap width and length, waveform frequency and profile, the identity and flow speed of buffer gas) affect FAIMS response. We find that the trade-off between resolution and sensitivity can be managed by varying gap width, RF frequency, and (in certain cases) buffer gas, with equivalent outcome. In particular, the resolving power can be approximately doubled compared to "typical" conditions. Throughput may be increased by either accelerating the gas flow (preferable) or shortening the device, but below certain minimum residence times performance deteriorates. Bisinusoidal and clipped-sinusoidal waveforms have comparable merit, but switching to rectangular waveforms would improve resolution and/or sensitivity. For any waveform profile, the ratio of two between voltages in high and low portions of the cycle produces the best performance.     

Characterization and electrochemical investigation of boron-doped mesocarbon microbead anode materials for lithium ion batteries

The structure and anodic performance of boron-doped and undoped mesocarbon microbeads (MCMBs) have been comparatively studied and the results obtained by XPS, XRD, SEM, Raman spectroscopy and electrochemical measurements are discussed. It is found that boron doping introduces a depressed d ₀₀₂ spacing and the larger amount of "unorganized carbon", which induces vacancy formation in the graphite planes and leads to a quite different morphology from that of the undoped material. Electrochemical charge/discharge cycle tests indicated that after boron doping the lithium intercalation was carried through at a somewhat higher potential, being attended by greater irreversible capacity loss. Electronic Publication     

Infrared-optical properties of vapour-deposited metal films

Spectroscopic infrared ellipsometry was applied to determine the optical constants of thin metal layers deposited on dielectric substrates such as glass or CaF(2). The layers were produced by evaporating gold or silver in a vacuum, and the coverage, that is the deposited mass per area, was chosen in the range 80-1200 mg m(-2) for gold, which refers to thicknesses in the lower nanometer range; in the case of the specifically lighter silver, about half the coverage was applied. At low coverage a metal island structure is obtained, which gives rise to surface-enhanced infrared absorption (SEIRA). Depending on the coverage, the deposited films exhibit either dielectric or metallic optical properties. Atomic force microscopy and conductivity measurements complement the spectroscopic observation.     

Enzymatic surface modification of Kevlar fibers

Horseradish peroxidase catalyzed grafting of acrylamide (AM) onto Kevlar fibers has been studied. The modified fiber has been characterized with scanning electron microscopy (SEM), elemental analysis and the grafting yield. From the SEM micrographs, the surface of the grafted Kevlar fiber is rougher than that of the untreated fiber, and the elemental analysis indicated that the nitrogen content of the treated fibers is higher than that of the untreated fiber. All the results suggested that AM must have been grafted onto the Kevlar surface through HRP-mediated radical initiated grafting reaction. The probably mechanism of HRP catalyzed grafting of AM onto Kevlar surface is proposed.     

Electrospun cellulose acetate fibers: effect of solvent system on morphology and fiber diameter

This paper reports an investigation of the effects of solvent system, solution concentration, and applied electrostatic field strength (EFS) on the morphological appearance and/or size of as-spun cellulose acetate (CA) products. The single-solvent systems were acetone, chloroform, N,N -dimethylformamide (DMF), dichloromethane (DCM), methanol (MeOH), formic acid, and pyridine. The mixed-solvent systems were acetone–DMAc, chloroform–MeOH, and DCM–MeOH. Chloroform, DMF, DCM, MeOH, formic acid, and pyridine were able to dissolve CA, forming clear solutions (at 5% w/v), but electrospinning of these solutions produced mainly discrete beads. In contrast, electrospinning of the solution of CA in acetone produced short and beaded fibers. At the same solution concentration of 5% (w/v) electrospinning of the CA solutions was improved by addition of MeOH to either chloroform or DCM. For all the solvent systems investigated smooth fibers were obtained from 16% (w/v) CA solutions in 1:1, 2:1, and 3:1 (v/v) acetone–DMAc, 14–20% (w/v) CA solutions in 2:1 (v/v) acetone–DMAc, and 8–12% (w/v) CA solutions in 4:1 (v/v) DCM–MeOH. For the as-spun fibers from CA solutions in acetone–DMAc the average diameter ranged between 0.14 and 0.37 μm whereas for the fibers from solutions in DCM–MeOH it ranged between 0.48 and 1.58 μm. After submersion in distilled water for 24 h the as-spun CA fibers swelled appreciably (i.e. from 620 to 1110%) but the physical integrity of the fibrous structure remained intact.     

Studies on metal — protein interactions: Inter-comparison among various approaches

Binding ability of mercury, thallium, lead and bismuth with Erythrina variegata seed protein have been investigated using tracer packet technique. Due to the lack of standard methods, inter-comparisons have been made among three different approaches, like trichloroacetic acid (TCA) precipitation, isoelectric precipitation and dialysis of protein after incubation with the metals. Good agreement was observed for all the cases except that of lead.     

Shear and NMR experiments of materials with flow behaviour depending on the deformation history

Oxide ceramic masses react to simple shearing with hardening (peptisation: increase in the shear stress with the shear deformation). In the present study the correlation between the increase in the shear stress and the porosity, agglomeration processes and the type of flow are analysed. For this purpose oxide ceramic masses are tested in a shear device especially developed for pastes and analysed by rheometric experiments, NMR methods and particle size analysis. The results support the hypothesis that structural changes (hardening, increase in the mean porosity) of the material during the peptisation mainly depend on the magnitude and not on the kind of the energy input and thus of the type of flow. The fraction of bound (more generally, the immobilised) water increases with the shear displacement. Also crushing of primary particles could be observed. Both the crushing of solid particles causing an increased solid surface and the formation of a three-dimensional gel structure are microscopic effects capable of resulting in the binding or retaining water. On a macroscopic scale these phenomena cause hardening. Magnetic resonance imaging visualises flow-induced agglomerates, which form owing to the shear flow and increase the porosity averaged over the whole sample. After the shear experiment rolls of paste can be seen which indicate that the general assumption of a plane shear flow in the shear device is not warrantable. Received: 19 July 2001 Accepted: 25 October 2001     

Resolution method for overlapping peaks based on the fractional-order differential

Equations between the differential order and the maximum of the fractional-order differential for the specified peak signals are developed based on the variation of the maximum of the specified peak signals at different orders. Also, equations between the differential order and the zero-crossing of the fractional-order differential of the specified peak signals are proposed according to the variation of the zero-crossing of the specified peak signals at different orders. Characteristic paramters of the Gaus- sian peak, Lorentzian peak, and Tsallis peak can be estimated using estimator I and estimator II which are obtained by the equations above. As a result, a new method is presented to resolve the overlapped peaks signal. Firstly, a fractional-order differential of the specified peak signals is obtained with the fractional-order differentiation filter. Then, characteristic paramters of the specified peak signals can be extracted using estimator I and estimator II. Finally, the Tsallis peak is used as a model to assign the overlapping peak signals correctly. Experimental results show that the proposed method is efficient and effective for the simulated overlapping peaks and detected overlapping voltammetric peak signals.     

Growth of ramification-like ZnO rods in the presence of polyaniline

To obtain new materials with synergetic or complementary behaviors, polyaniline composite filled with ZnO rods in ramification-like structure was prepared by a hydrothermal approach. Comparative experiments of ZnO preparation in the presence of some metal ions were also carried out. The results indicated that the morphology of ZnO was strongly affected by the preparation condition. The method to grow ZnO rods in the presence of polyaniline offers a simple approach to obtain polyaniline composite filled with linear ZnO structure. The results of X-ray photoelectron spectroscopy show that the strong interaction between ZnO and polyaniline possibly exists to cause the charge transfer.     

Synthesis of 5-Substituted 1,3-Dimethylpyrazolo[4,3-<Emphasis Type="Italic">e</Emphasis>][1,2,4]triazines

Summary.  A novel method for the synthesis of a new series of 5-substituted 1,3-dimethyl pyrazolo[4,3-e][1,2,4]triazines is described. The new synthetic strategy is based on the classical Bischler 1,2,4-benzotriazine synthesis. This approach involves the preparation of 5-hydrazinopyrazole from 5-chloro-1,3-dimethyl-4-nitropyrazole followed by acylation and nitro group reduction to form the corresponding 4-amino-3-(acylhydrazino)pyrazoles. Intramolecular oxidative cyclization of the latter derivatives, using polyphosphoric acid, produced the respective target pyrazolotriazines.