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51.
Inverse gas chromatography (IGC) was applied to characterize the surface of sepiolite. The adsorption thermodynamic parameters (the standard enthalpy (ΔH 0), entropy (ΔS 0) and free energy of adsorption (ΔG 0)), the dispersive component of the surface energy (γ S d ), and the acid/base character of sepiolite surface were estimated by using the retention time of different non-polar and polar probes at infinite dilution region. The specific free energy of adsorption (ΔG sp ), the specific enthalpy of adsorption (ΔH sp ), and the specific entropy of adsorption (ΔS sp ) of polar probes on sepiolite were determined. ΔH sp were correlated with the donor and modified acceptor numbers of the probes to quantify the acidic K A and the basic K D parameters of the sepiolite surface. The values obtained for the parameters K A and K D indicated an acidic character for sepiolite surface. 相似文献
52.
M. Mintas Z. Orhanović K. Jakopčić H. Koller G. Stühler A. Mannschreck 《Tetrahedron》1985,41(1):229-233
N-Aryl-4-pyridones 1–6 were synthesized by condensation of the corresponding 4-pyrone with anilines. The enrichment of the enantiomers was achieved by liquid chromatography on triacctylcellulose, enantiomeric purities of(+)-1 and (+ )-2 being measured by 1H-NMR in the presence of an optically active auxiliary. Barriers to partial rotation about the C-N bond in 1-4 were determined and compared with corresponding biphenyls. 相似文献
53.
Abdurrahmanoğlu S Ozkaya AR Bulut M Bekaroğlu O 《Dalton transactions (Cambridge, England : 2003)》2004,(23):4022-4029
A new sandwich-tpype dilutetium tetraphthalocyanine 4 has been synthesized by the reaction of dimeric lutetium(III) phthalocyanine 3 with two equiv. of dilithium octakishexylthiophthalocyanine in amyl alcohol. Compound 3 was prepared from 4',5',4",5"-tetraiminoisoindoline(1,4,7,10-tetrathia-12-crown-4) 1, 4,5-bis(hexylthio)-1,2-diiminoisoindoline and lutetium acetate in amyl alcohol. Compounds 3 and 4 were characterized by elemental analysis, UV/visible, IR, (1)H NMR and ESR spectroscopy. The electrochemical and electrochromic properties of 3 and 4 have been examined by cyclic voltammetry. Both 3 and 4 displayed well-defined electrochromic behavior. 相似文献
54.
The method of hydride generation atomic fluorescence spectrometry (HG-AFS) was optimised for determination of selenium in food supplements. Due to the high and varied content of Cu, Mg and Zn in the samples, the standard addition method was found to be the most appropriate. The reliability of the method was checked by the independent method of radiochemical neutron activation analysis, and good agreement was found between the two methods. HG-AFS is simple and rapid for Se determination in food supplements based on minerals. Agreement between the selenium values found and declared was worse than 10% in 9 out of 13 supplements. Furthermore, 2 of the 14 supplements did not comply with the recommendations stated in the 27th edition of the U.S. Pharmacopoeia, which states that minerals and vitamins in food supplements should be in the range of 90 and 200% of the declared value. 相似文献
55.
Surface modification of pyrophyllite with amino silane coupling agent for the removal of 4-nitrophenol from aqueous solutions 总被引:2,自引:0,他引:2
Sayilkan H Erdemoğlu S Sener S Sayilkan F Akarsu M Erdemoğlu M 《Journal of colloid and interface science》2004,275(2):530-538
The surface of naturally hydrophobic mineral pyrophyllite was modified to hydrophilic by treatment with prehydrolyzed N-(2-aminoethyl)-3-aminopropyltrimethoxysilane (APEO) coupling agent to prepare a novel and effective adsorbent for the removal of 4-nitrophenol (4-NP) from aqueous solutions. XRD, FTIR, and SEM analyses were used to characterize the surface modification. It was found that after the grafting procedure, heat treatment at 110 degrees C results in condensation reaction between the OH groups of the APEO molecule and the hydroxyl groups and/or oxygen atoms on the pyrophyllite surface and the adsorption of 4-NP by APEO-modified pyrophyllite involves interactions between dissociated 4-NP molecules and protonated amine groups of APEO molecules attached to the mineral surface. Adsorption equilibrium data for 4-NP adsorption on APEO-treated and untreated pyrophyllite were most satisfactorily fitted using the Freundlich adsorption isotherm and adsorption capacity was found to be 0.268 mg/g for modified pyrophyllite whereas it was only 0.105 mg/g for untreated pyrophyllite. 相似文献
56.
Zusammenfassung Durch elektrolytische Oxydation einer Bi-Anode in gesättigter NaCl-Lösung können Bi3+-Ionen in Lösung gebracht werden. Dieser Prozeß ermöglicht die coulometrische Bestimmung anwesender Anionen, die schwerlösliche Bi-Verbindungen bilden.Es wurden Semimikro- und Mikrobestimmungen von Phosphationen durch elektrolytisch erzeugte Bi3+-Ionen bei konstanter Stromstärke ausgeführt. Die Endpunktbestimmung erfolgte amperometrisch bei konstantem Potential mit einer Indikatorelektrode — tropfende Quecksilberelektrode — und mit einer gesättigten Kalomelelektrode als Bezugselektrode. Die coulometrische Wismutometrie bietet eine weitere Möglichkeit der coulometrischen Eichung volumetrischer Lösungen im Sinne des seinerzeitigen Vorschlags vonTutundi.
Vorgetragen beim Symposium für analytische Chemie in Graz, 29. September bis 1. Oktober 1965.
Wir danken Herrn Dipl.-Ing.Vladimir Pantovi für seine Hilfe bei unserer experimentellen Arbeit. 相似文献
Summary Bi3+ ions can be brought into solution through electrolytic oxidation of a Bi-anode in saturated NaCl solution. This process makes possible the coulometric determination of the anions present that yield difficulty soluble bismuth compounds.Semimicro- and micro-determinations of phosphate ions were made via Bi3+-ions produced electrolytically at constant current strength. The endpoint was determined amperometrically at constant potential with an indicator electrode-dropping mercury electrode-and with a saturated calomel electrode as reference electrode. The coulometric bismuthometry affords a further possibility of the coulometric standardization of volumetric solutions in the sense of the proposal previously advanced byTutundi.
Résumé On peut utiliser les ions Bi3+ en solution par oxydation électrolytique d'une anode en bismuth, en solution de chlorure de sodium saturée. Ce procédé permet le dosage coulométrique des anions présents qui forment des composés peu solubles avec le bismuth.On a mis au point le dosage semimicro et micro des ions phosphates par les ions Bi3+ formés électrolytiquement sous intensité constante. On détermine par ampérométrie le point équivalent à potentiel constant à l'aide d'une électrode indicatrice — électrode de mercure à goutte pendante —et avec une électrode au calomel saturée comme électrode de référence. La «bismuthométrie» coulométrique offre de grandes possibilités pour l'étalonnage coulométrique de solutions volumétriques, suivant l'idée queTutundi a émise en son temps.
Vorgetragen beim Symposium für analytische Chemie in Graz, 29. September bis 1. Oktober 1965.
Wir danken Herrn Dipl.-Ing.Vladimir Pantovi für seine Hilfe bei unserer experimentellen Arbeit. 相似文献
57.
Djaković-Sekulić Tatjana Perišić-Janjić Nada Sârbu Costel Lozanov-Crvenković Zagorka 《平面色谱法杂志一现代薄层色谱法》2007,20(4):251-257
JPC – Journal of Planar Chromatography – Modern TLC - Reversed-phase (RP) HPTLC with aqueous ammonia-organic modifier (acetonitrile, dioxane, acetone) mobile phases has been used to... 相似文献
58.
Mustafa Odabaolu idem Albayrak Reit
zkanca Fatma Zehra Aykan Peter Lonecke 《Journal of Molecular Structure》2007,840(1-3):71-89
Some new substituted polyhydroxy azo–azomethine compounds were prepared by reaction of tris(hydroxymethyl)aminomethane with (E)-2-hydroxy-5-(phenyldiazenyl) benzaldehyde and its substituted derivatives. The structures of azo and azo–azomethine compounds were determined by IR, UV–vis, 1H NMR and 13C NMR spectroscopic techniques, and/or X-ray diffraction studies. According to IR spectra, all azo–azomethine compounds adopt keto form in solid state. UV–vis analysis has shown the presence of keto–enol tautomerism in solution for all azo–azomethine compounds, except that for nitro substituted derivative, enol form is dominantly favored in solution. At the same time, above mentioned derivative compounds were studied in vitro for their antimicrobial properties. Among the phenylazosalicylaldehyde series compound tested, 4-phenylazosalicylaldehyde, 4-(3-chlorophenylazo)salicylaldehyde, 4-(2-chlorophenylazo)salicylaldehyde, 4-(4-fluorophenylazo)salicylaldehyde, 4-(3-chlorophenylazo)salicylaldehyde and 4-(4-ethylphenylazo)salicylaldehyde showed a weak antimicrobial activity only against gram positive bacteria. On the contrary, phenylazosalicylaldehyde series compounds were reacted tris(hydroxmethyl)aminomethane, that exhibited a strong antimicrobial activity against gram positive bacteria, yeast and mould. Moreover, while the 2-{[1,3-dihydroxy-2-(hydroxymethyl)propan-2-ylimino]methyl}phenol did not show an inhibition on tested microorganism, the addition of phenyldiazine groups to 2-{[1,3-dihydroxy-2-(hydroxymethyl)propan-2-ylimino]methyl}phenol resulted in a strong increases in antimicrobial activity. 相似文献
59.
The rapid determination of chloride and inorganic phosphate in blood serum based on continuous flow spectrophotometry was adapted to Flow Injection Analysis by applying dialysis as well as differential dilution of the injected samples. In addition to the manual injection procedure, an automated microsampling unit was developed and used. By continuous dialysis, chloride could be determined reproducibly at a sampling rate of 125 samples per hour at sample volumes of 60 μl or less. A similar sampling rate and high precision were obtained for the determination of inorganic phosphate by using differential dilution. 相似文献
60.
The basic principles of Flow Injection Analysis are outlined. The parameters governing the dispersion of the injected sample zone in the system are discussed, and it is demonstrated how these parameters can be manipulated in order to suit the requirements of an individual analytical procedure. A number of examples illustrating the practical application of f.i.a. are described, comprising the use of automated, stopped-flow, merging-zones, extraction techniques as well as f.i.a. scanning and methods based on intermittent pumping. Updated lists on f.i.a. procedures published and species that can be determined by f.i.a. are included. 相似文献