Reaction of indolylmagnesium bromide and chloromethylpyridines. Synthesis of skatylpyridines and piperidines

The reaction of indolylmagnesium bromide with the 2-, 3-, and 4-chloromethyl-pyridines is reported. Methods are described for the preparation of 2-, 3- and 4-skatylpyridine and 2-, 3- and 4-skatylpiperidine.     

Structure-specific DNA cleavage on surfaces

The structure-specific invasive cleavage reaction is a useful means for sensitive and specific detection of single nucleotide polymorphisms, or SNPs, directly from genomic DNA without a need for prior target amplification. A new approach integrating this invasive cleavage assay and surface DNA array technology has been developed for potentially large-scale SNP scoring in a parallel format. Two surface invasive cleavage reaction strategies were designed and implemented for a model SNP system in codon 158 of the human ApoE gene. The upstream oligonucleotide, which is required for the invasive cleavage reaction, is either co-immobilized on the surface along with the probe oligonucleotide or alternatively added in solution. The ability of this approach to unambiguously discriminate a single base difference was demonstrated using PCR-amplified human genomic DNA. A theoretical model relating the surface fluorescence intensity to the progress of the invasive cleavage reaction was developed and agreed well with experimental results.     

Volatile evolution from room temperature cured polysiloxane rubber induced by irradiation with He ions

A room temperature cured polysiloxane rubber (Rhodorsil RTV5370) has been irradiated using an accelerated beam of He²⁺ ions. Such an irradiation simulates the effects of large alpha radiation doses. A mass spectrometer linked directly to the sample chamber allowed the analysis of volatile species evolved as a result of exposure. The polydimethylsiloxane rubber showed high resistance to radiation damage when exposed to He²⁺ ions at doses up to 3.5 MGy. At higher doses, the cyclic hexamethylcyclotrisiloxane was evolved and is indicative of damage to the main chain. The cyclic octamethylcyclotetrasiloxane was only observed at very high doses (10 MGy and above) and is indicative of significant head-to-tail unzipping reactions. Methane, benzene and carbon dioxide were the three main gases evolved. The ratio of phenyl (2%) to methyl groups (93%) within RTV5370 rubber is very small but the amount of benzene evolved was found to be significant. The results suggest that the aromatic groups within the rubber appear to have a much greater susceptibility to radiation induced volatile evolution than other groups making up the polymer structure. In addition, the depletion of phenyl groups (from the reduction in evolution of benzene) from the irradiated zone corresponds to an increase in damage of the siloxane linkages (from the increased evolution of octamethylcyclotetrasiloxane) suggesting the aromatic groups offer a protective action from the incident radiation.     

The Application of Diffusing-Wave Spectroscopy to Monitor the Phase Behavior of Emulsion-Polysaccharide Systems

Droplet aggregation is an important cause of instability in emulsions because it may, on one hand, lead to an increased creaming rate, resulting in fast separation of a concentrated emulsion phase (creamed layer). On the other hand, it may also lead to the formation of a stabilizing, droplet-based network. Early detection of instability is often difficult due to the high turbidity and viscosity of more concentrated food emulsions. The applicability of diffusing-wave spectroscopy (DWS) for monitoring droplet aggregation and creaming was studied using a model system consisting of a protein-stabilized emulsion, to which a soluble polymer ("thickener") was added. This addition leads to an increased solvent viscosity and may induce droplet aggregation. In addition, the redistribution process of emulsion droplets in aggregating concentrated emulsions was directly observed by confocal scanning laser microscopy (CSLM). By DWS the decrease of the droplet mobility caused by the viscosity increase of the continuous phase could be separated from the effect of droplet aggregation. Moreover, a distinction could be made between aggregation, leading to increased creaming rates and that leading to the formation of a stabilizing droplet network. The potential of DWS for in situ measurement of the stability of concentrated emulsions is discussed. Copyright 2000 Academic Press.     

X-ray diffraction studies and phase transformations of CeNbO4+δ using in situ techniques

Investigation of CeNbO_4±δ has revealed that the previously determined phase transformations should be revised. Whereas previous studies have indicated that a reduced tetragonal modification of CeNbO₄ is produced on heating in vacuum the present study shows no evidence for this phase transformation. In contrast, a monoclinic–tetragonal phase transformation on heating in air was observed, indicating that the high temperature phase (800 °C) was a stable, oxygen excess tetragonal phase with a similar structure to the Scheelite mineral, CaWO₄. Lattice parameters for this phase were calculated to be a=5.3839(1) Å and c=11.6168(3) Å.     

Analytical characterisation of nanoscale zero-valent iron: A methodological review

Zero-valent iron nanoparticles (nZVI) have been widely tested as they are showing significant promise for environmental remediation. However, many recent studies have demonstrated that their mobility and reactivity in subsurface environments are significantly affected by their tendency to aggregate. Both the mobility and reactivity of nZVI mainly depends on properties such as particle size, surface chemistry and bulk composition. In order to ensure efficient remediation, it is crucial to accurately assess and understand the implications of these properties before deploying these materials into contaminated environments. Many analytical techniques are now available to determine these parameters and this paper provides a critical review of their usefulness and limitations for nZVI characterisation. These analytical techniques include microscopy and light scattering techniques for the determination of particle size, size distribution and aggregation state, and X-ray techniques for the characterisation of surface chemistry and bulk composition. Example characterisation data derived from commercial nZVI materials is used to further illustrate method strengths and limitations. Finally, some important challenges with respect to the characterisation of nZVI in groundwater samples are discussed.     

Novel methods for characterizing a decoupler channel using "undetectable" quantum coherences.

Exact solutions for the effect of time-independent RF pulses on any initial configuration of an IS J-coupled system demonstrate that on-resonance CW decoupling yields signals whose frequency depends on RF field strength and homogeneity. These signals are enhanced starting with "undetectable" antiphase and multiple quantum coherences, which can also produce centerband intensity to mimic the signal from decoupled Sx. Conversely, these coherences can be generated from Sx using a low-power pulse, B1 = J/2, of length (2J)-1, dubbed a "90J pulse" since it is the selective equivalent of {(2J)-1-90[I]}. Utilizing 90J pulses, new characterization-of-decoupler (COD) pulse sequences can determine the performance of an insensitive I-spin channel by observing large signals from either antiphase or multiple quantum coherences with the S-spin channel, allowing, in minutes rather than hours: (i) frequency calibration to an accuracy of 0.1 Hz; (ii) measurement of RF amplitudes over a 500-fold variation; and (iii) mapping of RF homogeneity along the sample axis with a single 1D B1 spectrum. These 90J coherence transfer pulses are of potential general use for selective spectroscopy.     

外电场下的TCNQ电子转移过程研究

自制了紫外/拉曼两用的电化学薄层池。观测到了TCNQ在外电场作用下转变为TCNQ－而后又转变为TCNQ2－的紫外-可见吸收光谱变化的电子转移过程, 并且当有氧气存在时, TCNQ2－又被氧化而形成DCTC－的过程。还观测到了TCNQ在外电场作用下转变为TCNQ－的傅里叶变换拉曼光谱发生频移的电子转移过程。     

On the Dissection of Rectangles into Right-Angled Isosceles Triangles

We consider the problem of dissecting a rectangle or a square into unequal right-angled isosceles triangles. This is regarded as a generalization of the well-known and much-solved problem of dissecting such figures into unequal squares. There is an analogous “electrical” theory but it is based on digraphs instead of graphs and has an appropriate modification of Kirchhoff's first law. The operation of reversing all edges in the digraph is found to be of great help in the construction of “perfect” dissected squares.     

邻苯二酚显色树脂相分光光度法同时测定地下水中微量铁(Ⅲ)和钼(Ⅵ)

研究了铁（Ⅲ）和钼（Ⅵ）与邻苯二酚在ｐＨ ６．２０ 微酸性介质中反应生成的有色配合物与７１７型强碱性阴离子交换树脂的交换吸附,探讨了树脂相分光光度法同时测定铁（Ⅲ）和钼（Ⅵ）的实验条件。铁（Ⅲ）和钼（Ⅵ）树脂相有色配合物的最大吸收波长分别为５２０ ｎｍ 和４００ ｎｍ ,表观摩尔吸光系数ε为４．１×１０４ Ｌ／（ｍ ｏｌ·ｃｍ ）和９．０×１０４ Ｌ／（ｍ ｏｌ·ｃｍ ）,符合Ｂｅｅｒ定律的范围为０～２．２ ｍ ｇ·Ｌ－ １和０～１．６ ｍ ｇ·Ｌ－ １。此法用于地下水中微量铁和钼的测定,相对标准偏差为３．３ ％ 和３．２ ％ 。