Synthesis of novel crown ethers. Part 1. Coumestan and coumestan analog derivatives of crown ethers

The presented ethylenedioxy compounds5a,5d,6a and6c are examples of novel cyclic ethers, while macrocyclic polyethers represent new crown ether analogues. New coumestan-crowns5a-f, derivatives of 6,7-dihydroxy-3,4-dihydro-2H-dibenzofuran-1-one and 6,7-dihydroxy-3,3-dimethyl-3,4-dihydro-2H-dibenzofuran-1-one6a-e were synthesized from the correspondingo-dihydroxy compounds3a-b,4a-b and ditosylates or dichlorides of di- or triethylene glycol in the presence of K₂CO₃, in DMF/H₂O (15/1) solutions at 65–75 °C for 35 hours. The structure of the macrocyclic ethers obtained were confirmed by¹H-NMR,¹³C-NMR, IR spectra and elemental analyses.Presented at the Sixth International Seminar on Inclusion Compounds, Istanbul, Turkey, 27–31 August, 1995.     

Spectroscopic studies of new Co(II), Cu(II), and Ni(II) complexes with 1,2-Bis(<Emphasis Type="Italic">m</Emphasis>-aminophenoxy)ethane

1,2-Bis(m-aminophenoxy)ethane was prepared in a one-stage process. In this reaction, Pd/C was used as a catalyst. 1,2-Bis(m-aminophenoxy)ethane was synthesized from 1,2-bis(m-nitrophenoxy)ethane. Diamine complexes [CoLCl₂], [CuLCl₂] and [NiL₂]Cl₂ have been synthesized and characterized by elemental analyses, Λ_M, IR, UV-Vis, ¹H NMR and magnetic measurements.     

Moisture diffusion into epoxy adhesive: testing and modeling

Moisture diffusion into epoxy adhesive is investigated through utilizing complete fluid immersion tests in distilled water. Apparent diffusivity for each specimen is determined by two methods, one using the diffusion data at early times (at low loading) and the other using the data at large times (close to the saturation point). The results of the two methods are quite different, indicating that diffusivity is concentration dependent. The apparent diffusivity values obtained through the method using the early data points are about twice those obtained through the method utilizing the data points at large diffusion times. Variance of diffusivity with concentration is also considered as the third method of analysis to determine the concentration dependency. A good agreement is observed between the resultant Fickian model solved numerically and the experimental data. The latter result appears to indicate a change in the excess volume of mixing during the sorption process.     

Lossless single-photon shaping via heralding

Using spontaneous optical parametric downconversion, we experimentally demonstrate heralded generation of shaped single photons, whose modes are tailored indirectly by applying amplitude modulation on the pump field that drives the downconversion process. Our experiment opens a door to creating high-quality, mode-shaped single photons at a substantially higher efficiency than is possible with the existing method of direct single-photon shaping.     

On the Quaternionic B 2-Slant Helices in the Euclidean Space E 4

In this paper we give a new definition of harmonic curvature functions in terms of B ₂ and we define a new kind of slant helix which we call quaternionic B ₂–slant helix in 4–dimensional Euclidean space E ⁴ by using the new harmonic curvature functions. Also we define a vector field D which we call Darboux quaternion of the real quaternionic B ₂–slant helix in 4–dimensional Euclidean space E ⁴ and we give a new characterization such as: "a: I ì \mathbb R ? E⁴{``\alpha : I \subset {\mathbb R} \rightarrow E^4} is a quaternionic B ₂–slant helix ${\Leftrightarrow H^\prime_2 -KH_{1} = 0"}${\Leftrightarrow H^\prime_2 -KH_{1} = 0"} where H ₂, H ₁ are harmonic curvature functions and K is the principal curvature function of the curve α.     

Differential separation of protein mixtures using convective assembly and label-free detection with surface enhanced Raman scattering

Differential separation and label-free detection of proteins using SERS from their mixtures after a convective assembly process is reported. Binary and ternary mixtures of proteins are mixed with AgNPs and assembled into ordered structures. The spectra acquired from the assembled area indicate that the proteins are differentially distributed.     

Towards single-microorganism detection using surface-enhanced Raman spectroscopy

The identification and discrimination of microorganisms is important not only for clinical reasons but also for pharmaceutical clean room production and food-processing technology. Vibrational spectroscopy such as IR, Raman, and surface-enhanced Raman scattering (SERS) can provide a rapid ‘fingerprint’ on the chemical structure of molecules and is used to obtain a ‘fingerprint’ from microorganisms as well. Because of the requirement that a single bacterium cell and noble metal nanoparticles must be in close contact and the lack of a significant physical support to hold nanoparticles around the single bacterium cell, the acquisition of SERS spectra for a single bacterium using colloidal nanoparticles could be a challenging task. The feasibility of SERS for identification down to a single bacterium is investigated. A Gram-negative bacterium, Escherichia coli, is chosen as a model for the investigation. Because the adsorption of silver nanoparticles onto the bacterial cell is an exclusive way for locating nanoparticles close to the bacterium cell, the absorption characteristics of silver nanoparticles with different surface charges are investigated. It is demonstrated that the citrate-reduced colloidal silver solution generates more reproducible SERS spectra. It is found that E. coli cells aggregate upon mixing with silver colloidal solution, and this may provide an additional benefit in locating the bacterial cell under a light microscope. It is also found that a laser wavelength in the UV region could be a better choice for the study due to the shallow penetration depth. It is finally shown that it is possible to obtain SERS spectra from a single cell down to a few bacterial cells, depending on the aggregation properties of bacterial cells for identification and discrimination.     

Slurry sampling electrothermal atomic absorption spectrometric determination of chromium after separation/enrichment by mercaptoundecanoic acid modified gold coated TiO2 nanoparticles

In this study, a novel preconcentration/separation technique based on the slurry analysis of chromium loaded on mercaptoundecanoic acid modified TiO₂ core-Au shell nanoparticles prior to its determination by electrothermal atomic absorption spectrometry was described. For this purpose, at first, TiO₂ nanoparticles were coated with gold shell and then modified with mercaptoundecanoic acid (MUA). Cr (III) was collected on the prepared sorbent by conventional batch technique. After separation of liquid phase, slurry of the sorbent was prepared and directly introduced into graphite furnace of atomic absorption spectrometry. By this way, all drawbacks due to elution procedure were eliminated. Optimum conditions for quantitative sorption and preparation of the slurry were investigated. The chromium in certificated sea-water and spiked drinking water was recovered in the range of 95% confidence level. The proposed technique was fast and simple as well as the risks of contamination and loss during elution were low. The limit of detection (3σ, N = 10) was 0.34 μg L^{− 1}.     

FAAS slurry analysis of lead and copper ions preconcentrated on titanium dioxide nanoparticles coated with a silver shell and modified with cysteamine

We report on the separation and preconcentration of lead(II) and copper(II) ions using silver-coated titanium dioxide nanoparticles modified with cysteamine, and their determination by slurry analysis via flame atomic absorption spectrometry. The ions were adsorbed via a conventional batch technique, and the ion-loaded slurry was separated and directly introduced into the spectrometer, thereby eliminating a number of drawbacks. The effects of pH, amount of sorbent, slurry volume, sample volume and other ions on the recovery were investigated. Under optimized experimental conditions, copper and lead can be recovered within the 95% confidence level in certificated waste water, but also in spiked sea water samples. The technique is fast, simple, and leads to complete elution. The limit of detection (3δ, at n?=?10) was 0.37 μg L^?1 for Cu(II), and 0.38 μg L^?1 for Pb(II).

Preparation of fluorine containing hybrid coatings: investigation of coating performance onto ABS and PMMA substrates

UV‐curable fluorinated organic–inorganic hybrid coatings were prepared by the sol–gel technique. Perfluorinated urethane modified alkoxysilane was synthesized by the reaction between perfluoro alcohol and 3‐isocyanatopropyltrimethoxysilane. The prepared formulations were applied onto poly(methyl methacrylate) (PMMA) and acrylonitrile butadiene styrene (ABS) panels and polymerized by UV‐curing. The properties of the hybrid coatings such as hardness, chemical resistance, thermal stability, surface morphology, double bond conversion, and also contact angle measurements were investigated. Contact angle measurements have shown that the addition of fluorinated silane precursor to the hybrid system improved the water repellency and increased the contact angle from 65° to 106°. Copyright © 2009 John Wiley & Sons, Ltd.