We report here on an integrated microfabricated device dedicated to the preparation of biological samples prior to their on-line analysis by electrospray ionization-mass spectrometry (ESI-MS). This microfluidic device is fabricated using the negative photoresist SU-8 by microtechnology techniques. The device includes a chromatographic module plus an ESI interface for MS. The chromatographic module is dedicated to sample purification and is based on a polymer monolithic phase which includes hydrophobic moieties. The ESI interface is integrated onto the chip and is based on a capillary slot. We present here the integration of these different modules onto a single system that is fabricated via a SU-8-based microtechnology route. We present also their testing for the purification of peptide samples. This started with a partial integration step with the combination of at least two of the modules (microsystem + monolith; microsystem + nib) and their test before the fabrication and testing of fully integrated microsystems. 相似文献
The host-guest interaction between orthophosphate, pyrophosphate and triphosphate anions and four cyclen based bis-macrocycles ligands possessing ortho-(BOC), meta-(BMC), para-xylenyl (BPC) or 2,6-pyridinyl (BPyC) linker was investigated by potentiometric measurements and NMR spectroscopy. Each ligand gave protonated species in aqueous solution that further formed ternary complexes after binding with anions; these complexes were analyzed as a result of hydrogen bond formation and Coulombic attraction between the organic host and the inorganic guest. The equilibrium constants for all the detected species are reported and the selectivity, illustrated with species distribution diagrams, is discussed. The results unambiguously showed the importance of the distance between the two cyclen cores and underlined, especially for the triphosphate species, the contribution of the nitrogen atom of the pyridinyl spacer as a supplementary anchoring point in acidic medium. 相似文献
Normal state conductivity and superconductivity together with bulk magnetic susceptibility and magnetization measurements have been measured for two molecular charge-transfer salts: beta' '-(ET)4[(H3O)Ga(C2O4)3]G (ET = bis(ethylenedithio)tetrathiafulvalene, G = pyridine for compound I and nitrobenzene for compound II). With the exception of the included guest molecules (G) the crystal structures are almost identical. Both show minima in their electrical transport at 130 K for I and at 160 K for II, but at lower temperatures their behaviors differ markedly. The resistance of I reaches a maximum at 50 K with a further small peak at 2 K and possible superconductivity only below 2 K, whereas that of II increases continuously down to 7.5 K, where an abrupt transition to a superconducting state occurs. 相似文献
The objective of the present article was to study the thermal degradation behavior and flame retardancy of flexible polyvinyl chloride (PVC) composites containing TiO2/SO2?4 solid superacid because of its strong catalytic ability for esterification and dehydration. The TiO2/SO2?4 solid superacid was synthesized by using precipitation immersion method, and its structure was investigated by X-ray diffraction. As expected, the value of limiting oxygen index for PVC/Sb2O3/(TiO2/SO2?4) composite was 32.5% and the char yield of PVC/Sb2O3/(TiO2/SO2?4) composite was significantly improved compared to neat PVC in thermogravimetry tests. In addition, the peak heat release rate and smoke production rate of PVC/Sb2O3/(TiO2/SO2?4) decreased by 14% and 42%, respectively, compared with neat PVC. Moreover, the results of cone calorimetry tests and electron micrograph of char residue showed that the char yield of TiO2/SO2?4 was enhanced, resulting in a strong char layer structure with outstanding fire retardance cone. In conclusion, the results of this work showed that the addition of solid superacid promoted the decomposition and dehydration of PVC, which formed a compact and continuous char layer on the surface of the material. Hence, the study provides a new perspective for producing composites with excellent flame retardancy and smoke suppression properties of PVC.
Room temperature ionic liquid (bmim)PF6 was evaluated for recycling an organocatalyst (4S)-phenoxy-(S)-proline for direct asymmetric aldol reactions. The desired aldol products were obtained with good yields up to 93.2% and enantioselectivities up to 88.5%, and isolation of the products by simple extraction allowed recycling the ionic liquid containing the immobilized catalyst in subsequent reactions without significant decrease of yields and enantioselectivities. 相似文献
We focused our work on the separation of phenothiazines that are important drugs used for the treatment of psychic diseases. For a better understanding of the metabolism of these solutes, we wanted to separate not only a mixture of 12 phenothiazines but also a mixture containing phenothiazines and their N-demethyl metabolites by capillary electrophoresis. Separations in capillary zone electrophoresis were performed using 3 x 10(-2) mol/L H3PO4 (pH 2.5) but the obtained resolutions were not entirely satisfactory especially with regard to phenothiazine -N-demethyl derivative pairs. To improve the obtained results, we have performed separations by using micellar electrokinetic chromatography. In this approach, we used a running electrolyte containing 3 x 10(-2) mol/L H3PO4 electrolyte (pH 2.5) and octaethylene glycol monododecyl ether (C12E8) as neutral surfactant. By introducing 2 x 10(-3) mol/L C12E8 in the electrolyte, 11 out of 12 phenothiazines have been baseline separated. With respect to the separation of a mixture containing 3 phenothiazines and their 3 demethyl derivatives, we obtained an excellent separation by using a running electrolyte prepared with 7.5 x 10(-4) mol/L C12E8 and 3 x 10(-2) mol/L H3PO4. 相似文献
The equilibrium parameters for the adsorption of Mo(VI) on gamma-Al(2)O(3) and of Co(II) and Pt(IV) on MoO(3)/gamma-Al(2)O(3) were determined. The adsorption isotherms were performed from aqueous solutions of the corresponding precursors on two different alumina supports. According to the classification given by Giles, L-type-shaped, subgroup 2, adsorption curves were found for the system Mo on gamma-Al(2)O(3), L-type, subgroup 1, for the Pt on MoO(3)/gamma-Al(2)O(3), and S-type for Co on the MoO(3)/gamma-Al(2)O(3) system. Numerical calculations were carried out for all the isotherms to find the equilibrium parameters. These constants are being used to model the development of Pt, Co, and Mo profiles on MoO(3)/gamma-Al(2)O(3) or gamma-Al(2)O(3) extrudates, respectively, which belong to the new generation of noble-metal-MoO(3)/gamma-Al(2)O(3)-supported catalysts to be used in oil-refining processes. Copyright 2001 Academic Press. 相似文献