Flow-through microdispenser for interfacing micro-HPLC to Raman and mid-IR spectroscopic detection

A flow-through microdispenser has been coupled to a micro HPLC separation system and used as a solvent elimination interface for Fourier transform infrared (FTIR) and Raman spectroscopic detection of the separated compounds. Using the microdispenser picoliter sized droplets can be generated and deposited on an appropriate target placed on a computerized x, y-stage. Evaporation of volatile solvent and buffer is rapid and allows analysis of the obtained dry deposits by various techniques. Due to the destruction free character of Raman and FTIR spectroscopy they can be applied sequentially to interrogate the same deposit. In the reported application five phenolic acids typically present in wine have been separated on a C-18 column technique using a mixture of water, methanol and acetic acid as mobile phase. For spectrum acquisition infrared and Raman microscopes have been used. The spectra recorded from the dried deposits of the separated compounds agreed well with the reference spectra of corresponding components.     

Electron radiation effects on the structure of ultradisperse polytetrafluoroethylene

Electron radiation effects (40 mrad, 70 mrad, and 100 mrad) on the molecular and supramolecular structure and morphology of ultradisperse polytetrafluoroethylene obtained by the thermogas dynamic (TGD) method were studied by IR and EPR spectroscopy, X-ray phase analysis, and atomic force microscopy. Irradiation of ultradisperse powder in air leads to oxidized polymer forms due to the terminal carbonyl groups and stable peroxide radicals that appear in the structure. Fast electron radiation in doses of up to 100 mrad did not change the polymer crystallinity and particle entity, while thin films on the surface of ultradisperse polytetrafluoroethylene powder decomposed.     

PHOTOEMISSION WITHIN AND BEYOND THE ONE-STEP MODEL

Photoemission in the vacuum ultraviolet photon regime has proved to be an effective tool for the investigation of valence band surface electronic structure. The interpretation cannot be exclusively confined to the valence bands but has to consider cross sections with realistic final states consistently designed within the one-step model. Therefore especially in the surface sensitive photoemission, several effects hide the final goal of deducing the energetic and wavefunction structure together with microscopic potential parameters through a convincing agreement of calculated with measured spectra. The final states band structure is much less well understood than the valence band structure under consideration. The optical potential, which controls the surface sensitivity through the underlying damping mechanisms, widely relies on empirical assumptions. Furthermore, the photon field is not only strongly influenced but in the vicinity of the plasma frequency also deteriorated by the electronic response. In view of high resolution spectroscopy the accuracy of the data interpretation is affected, and in fact, band-mapping methods are no longer valid. Examples of recent calculations to account for these effects are reviewed.     

规整链球型含C_(60)聚(丙烯酸β-羟乙酯)的合成及其在水中的自组装

Ｃ60 由于其独特的物理化学性质 ,在生命科学中引起了人们的广泛兴趣 .例如 :水溶性Ｃ60 的羧酸衍生物 ,羟基取代Ｃ60 ,Ｃ60 的氨基酸水溶性衍生的合成已有报道[1～ 3] ,并被用来研究Ｃ60 的生物化学及医学活性 .Ｔｏｋｕｙａｍａ[4 ] 等合成了酶功能化Ｃ60及与核酸连接的Ｃ60 ,研究并证明了它的细胞毒性及Ｇ 选择ＤＮＡ切割能力等生化活性 .Ｆｒｉｅｄｍａｎ[5]等合成了水溶性Ｃ60 的羧酸衍生物 ,研究了它对ＨＩＶ 1艾滋病毒的抑制作用 ,此外 ,关于不同Ｃ60含量的Ｃ60 蛋白质衍生物的合成及性质的研究也有报道[6] .Ｃ60 是一个直径为 0 71…     

Atom-probe field ion microscopy

The atom probe field ion microscope (AP-FIM) is a combination of a field ion microscope and a time-of-flight mass spectrometer with a single ion detection sensivity. With the field ion microscope topology of a surface, surface reactions and surface modifications can be studied in atomic detail. By time-of-flight measurements surface layers and interface layers can be chemically analyzed atom by atom and atomic layer by atomic layer. Compositional variations according to surface or interface segregation, precipitations, or surface changes in corrosion or in electrochemical layer formation etc. can be studied quantitatively on a subnanometer scale. Some of our studies on related problems will be decribed briefly.     

Metallurgical factors determining the coercivity of ND-FE-B magnets

In Nd-Fe-B based permanent magnets a high magnetocrystalline anisotropy of the hardmagnetic phase is necessary for a high intrinsic coercivity. In fact, metallurgical parameters (distribution of phases, chemical composition and crystal structures of phases) and processing parameters (alloy preparation, size and shape of particles, sintering and annealing treatments) determine the value of the coercive force of each sintered Nd-Fe-B magnet. Our analytical electron microscope study shows that melt-spun and sintered Nd-Fe-B based magnets contain more or less a distribution of nucleation centres for reversed domains, such as iron-rich phases and-iron precipitates within the hardrnagnetic 2141-grains. A continuous non-magnetic layer phase between the hardrnagnetic 2141-grains increases the expansion field of reversed domains and increase the coercivity. In melt-spun magnets the contribution of the pinning of magnetic domain walls becomes effective during the magnetization reversal process.     

Structure and dynamics of self-assembled poly(ethylene glycol) based coiled-coil nano-objects.

Herein we describe the structure and dynamics of self-assembled nano-objects generated from poly(ethylene glycol) based (PEG-ylated) coiled-coil hybrid block copolymers. Electron paramagnetic resonance (EPR) experiments on spin-labeled samples provided a strong indication for a parallel alignment of the peptide helices in at least the dimeric coiled-coil nano-object and indicated that the PEG chains are folded rather closely around the peptide core of the nano-objects. The EPR results were supported by AFM studies, which revealed the presence of discrete nanosized objects in thin, spin cast films of the block copolymers on mica substrates. Since their size and structure may be engineered via directed mutations in the amino acid sequence, these nano-objects may be interesting building blocks for the development of supramolecular materials with various potential applications.     

Controlling the self-assembly of a deoxiguaninosine on mica

We report a tapping mode scanning force microscopy investigation on the growth from solutions of a lipophilic deoxiguanosine derivative on the basal plane of a muscovite mica surface. By varying the chemical composition of the substrate surface it is possible to drive the self-assembly towards either layered thin films, which are very likely to consist of guanosine quartets, or nanoribbons, comprising hydrogen bonded networks. Both these two architectures, which are peculiar to the guanine base itself, are of notable importance for the fabrication of molecular nanowires. Moreover, the first arrangement provides evidence that the guanosine is able to behave as ionophore, thus, suggesting its utilization in the development of solid-state ion selective sensors.     

On the Rigidity of Polynorbornenes with Dipolar Pendant Groups

A range of polynorbornenes (PNBs) with fused dipolar pendant groups at C‐5,6 positions was synthesized by ring‐opening metathesis polymerization catalyzed by a ruthenium carbene complex (Grubbs I). Photophysical studies, EFISH measurements, and atomic force microscopy images have been used to investigate the structures and morphology of these polymers. These results suggest that the polymers may adopt rigid rod‐like structures. The presence of the double bonds in PNBs appeared to be indispensable for the rigidity of the polymers. Interaction between unsaturated pendant groups may result in coherent alignment leading to a rod‐like structure.