Search results for "Solid"

New ferrocene-containing copolyesters

1995

We have synthesized four new ferrocene monomers (three diols and one diester). The redox potential of these ferrocene derivatives varies between 0 mV and 230 mV due to different degrees of ring alkylation. Amorphous and liquid crystalline copolyesters were prepared with these monomers in the polymer main chain. Cyclovoltammetric measurements show that the redox potential of the ferrocene units is increased by about 40 mV upon polymer formation (esterification). Since the ester group is 4 to 6 σ-bonds away from the ferrocene unit this increase is probably caused by some charge-transfer interaction through space. First rheological measurements show an unusual rubber-like behaviour of the ferr…

Impedance spectroscopy characterization of functionalized alumina membranes

2005

Abstract Anodic alumina membranes have been impregnated with a protonic conductor either by immersion or by vacuum permeation of a saturated aqueous solution of CsHSO4 for different times. Synthetized salt, obtained through the reaction of cesium carbonate with sulphuric acid (in excess), contained a small quantity of Cs2SO4. Unmodified membranes consist of amorphous Al2O3 with a regular distribution of pores (average diameter: 200 nm) and are stable up to 850 °C. Long impregnation times caused partial dissolution of alumina, with formation of Al(HSO4)3 on the front surfaces as well as into pore walls. From the frequency dispersion of the impedance, the “macroscopic conductivity” of membran…

Dynamics of cross polarization in solid state nuclear magnetic resonance experiments of amorphous and heterogeneous natural organic substances

2008

Nuclear magnetic resonance (NMR) experiments on carbon-13 in the solid state were done with cross polarization (CP) and magic angle spinning (MAS) in order to overcome the low NMR sensitivity of (13)C and the chemical shift anisotropy, respectively. In the present research, CPMAS (13)C-NMR spectra were collected by modulating the contact time needed for cross polarization (variable contact times experiments, VCT) on two different humic acids (a soil-HA and a coal-HA). VCT data were fitted by a model containing either a monotonic or a non-monotonic cross polarization term. The non-monotonic model, which fitted the experimental results better than the monotonic one, provided two cross-polariz…

1990

This lecture summarizes some recent results and ideas about interrelations between degradation and mechanical behaviour of polyolefins. Aspects of the heterogeneous nature of oxidative degradation in the solid state, the feedback mechanism in degradation, effects of morphology, particularly orientation, on the degradation process, and the influence of degradation on plasticity and on the ultimate mechanical behaviour are discussed.

Study of the conformations of the molecules in amorphous polymers by computer simulation

2008

It is investigated by computer simulation whether space problems prevent a closing packing of chain molecules if the chain molecules are randomly coiled. Chains consisting of 100 beads were introduced into a primitive cubic lattice in such a way that each lattice point is occupied by not more than one bead. It was possible to occupy up to 88% of the lattice points. The average square end-to-end distance of the chains in the concentrated system is the same as for a single chain. Neither perfect chain bundles nor imperfect chain bundles occur in a considerable amount. This shows that it is possible to pack closely randomly coiled chains.

Effect of t-BuS vs. n-BuS on the topology, Cu⋯Cu distances and luminescence properties of 2D Cu4I4/RS(CH2)4SR metal–organic frameworks

2011

CuI reacts with RS(CH2)4SR (R = n-Bu (L1); t-Bu (L2)) to afford the 2D coordination polymers [Cu4I4{μ-RS(CH2)4SR}2]n (R = n-Bu (1); t-Bu (2)). Their grid networks exhibit nodal Cu4(μ3-I)4 clusters interconnected by dithioethers with mean Cu⋯Cu distances of 2.7265(10) and 2.911(2) A for 1 and 2, respectively. This difference translates in a blue shift of the solid state emission bands and a decrease in emission lifetimes when trading R = n-Bu to the bulky t-Bu.

Ethanedithiol diacetate

2001

Ethane-1,2-diyl S,S′-bis­(thio­acetate), H3CC(O)SCH2CH2SC(O)CH3 or C6H10O2S2, forms centrosymmetric mol­ecules in the solid state and the molecular structure determined by X-ray crystallography is in good agreement with that obtained by density functional geometry optimization. The planarity of the O=C—S—C fragment, which is also found in structures of other thio­acetates, is attributed to a strong np(S)–π*(C—O) orbital interaction.

In-tube solid-phase microextraction coupled by in valve mode to capillary LC-DAD: Improving detectability to multiresidue organic pollutants analysis…

2009

Abstract A simple and fast capillary chromatographic method has been developed to identify and quantify organic pollutants at sub-ppb levels in real water samples. The major groups of pesticides (organic halogens, organic phosphorous, and organic nitrogen compounds), some hydrocarbons (polycyclic aromatic hydrocarbons), phthalates and some phenols such as phenol and bisphenol A (endocrine disruptors) were included in this study. The procedure was based on coupling, in-tube solid-phase microextraction (IT-SPME) by using a conventional GC capillary column (95% methyl–5% phenyl substituted backbone, 80 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve to capillary liquid chromatog…

Indirect analysis of urea herbicides from environmental water using solid-phase microextraction.

2000

We described here a solid-phase microextraction procedure used to extract six urea pesticides-- chlorsulfuron, fluometuron, isoproturon, linuron, metobromuron and monuron--from environmental samples. Two polydimethylsiloxanes and a polyacrylate fiber (PA) are compared. The extraction time, pH control, addition of NaCl to the water and the influence of organic matter such as humic acid on extraction efficiency were examined to achieve a sensitive method. Determination was carried out by gas chromatography with nitrogen-phosphorus detection. The proposed method requires the extraction of 2 ml of sample (pH 4, 14.3%, w/v, NaCl) for 60 min with the PA fiber. The limits of detection range from 0…

Host-guest interactions for extracting antibiotics with a γ-cyclodextrin poly(glycidyl-co-ethylene dimethacrylate) hybrid sorbent

2021

Abstract A procedure for the solid-phase extraction of antibiotics (enoxacin, ofloxacin, norfloxacin, ciprofloxacin, and sparfloxacin) in water has been developed. The sorbent used is based on a poly(glycidyl-co-ethylene dimethacrylate) network, whose previously modified surface has been functionalized with γ-cyclodextrin through a click-chemistry reaction. The architecture of the material has been characterized by thermogravimetric analysis, N2 adsorption-desorption, Raman spectroscopy, confocal microscopy, and scanning electron microscopy, showing good capability to be used as a filler for extraction cartridges. The optimization of the extraction methodology shows good intra-day and inter…