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111.
Jo?o L M Santos Arnaud Clausse José L F C Lima M L M F S Saraiva António O S Rangel 《Analytical sciences》2005,21(4):461-464
A new flow methodology exploiting the multi-pumping approach was developed for the spectrophotometric determination of ambroxol hydrochloride in pharmaceutical preparations. The flow manifold was implemented by using, exclusively, multiple solenoid-actuated micro-pumps, which acted simultaneously as sample insertion, solutions propelling and reagents commutation units. Linear calibration plots were obtained over an ambroxol concentration ranging from 10 to 200 mg l(-1) (r.s.d. < 0.5%, n = 15) and a sampling rate of about 60 samples per hour (flow rate = 1.92 ml min(-1), sample volume = 80 microl). 相似文献
112.
Summary A method is reported for the determination of dibutyltin (DBT), diphenyltin (DPhT), tributyltin (TBT), and triphenyltin (TPhT)
species at the nanogram per litre concentration level in natural water samples. Analytes were isolated from samples by solid-phase
extraction and analysed both off-line and on-line by reversed-phase high-performance liquid chromatography with post-column
derivatization and fluorimetric detection. Several SPE cartridges and eluents were evaluated; C18 enrichment and elution with a mixture of methanol, acetic acid, and water was found most suitable. Preconcentration factors
up to 250 can be achieved when a 500-mL sample is processed. Detection limits, recovery rates, and the precision of the whole
process have been determined. The method has been applied to the determination of organotin species in spiked natural water
samples collected on the NW Mediterranean coast. Recovery rates range from 75 to 110% and detection limits are at the low
ng L−1 level (1–3 ng Sn L−1 for DPhT, DBT, and PhT and 40 ng Sn L−1 for TBT when 250 mL spiked sea water is processed.) 相似文献
113.
J. V. Kunzler W. Schreiner A. Bristoti D. E. BrandÃo 《Journal of Thermal Analysis and Calorimetry》1977,11(1):81-86
Saturation magnetization measurements as a function of temperature were performed on Cu2Mn(Al1–xSnx) Heusler alloys to study the existence of stable structures. The derivatograph was applied to study the thermal effects.
Work supported in part by Conselho Nacional de Desenvolvimento Cientifico e Tecnologico and Banco Nacional de Desenvolvimento Economico, Brasil. 相似文献
Zusammenfassung Sättigungsmagnetisierungsmessungen als Funktion der Temperatur sowie Derivatographie wurden an Heusler-Legierungen der Formel Cu2Mn(Al1–xSnx) zu Untersuchungen der Existenz einer stabilen Struktur vorgenommen.
Résumé Etude de l'existence d'une structure stable dans les alliages de Heusler Cu2Mn(Al1–xSnx), à l'aide d'un Derivatograph et par des mesures de magnétisation à saturation en fonction de la température.
XecnepaCu2Mn(Al1–xSnx), , , . .
Work supported in part by Conselho Nacional de Desenvolvimento Cientifico e Tecnologico and Banco Nacional de Desenvolvimento Economico, Brasil. 相似文献
114.
H. Langfelderová L'. Macášková K. Otrubová J. Gažo 《Journal of Thermal Analysis and Calorimetry》1986,31(5):1143-1151
The thermal decompositions of Cu(en)2(NCS)X. where X–=Cl–, Br–, NO
3
–
, BF
4
–
and ClO
4
–
, have been studied in comparison with the courses of Cu(en)2(SCN)2 and Cu(en)2X2 decomposition. It is shown that the presence of the thiocyanate group in the complexes Cu(en)2(NCS)X is the most important factor in the decomposition course, in agreement with the fact that the anions X– are not coordinated. or are only semicoordinated. Significant differences were found in the courses of thermal decomposition of two forms of Cu(en)2(NCS)(BF4) differing in the structure of their coordination polyhedra.
Zusammenfassung Die thermische Zersetzung von Cu(en)2(NCS)X (X=Cl Br, NO3, BF4 und ClO4) wurde untersucht und mit der von Cu(en2(SCN)2 und Cu(en)2X2 verglichem. Der den Verlauf der Zersetzung entscheidend bestimmende Faktor isi die Anw esenheit der Thiocyanat-Gruppe in den Cu(en)2(NCS)X-Komplexen, was in Übereinstimmung damit steht,. daß die Anionen X nicht oder nur teilweise koordiniert sind. Es wurden signifikante Unterschiedeim Verlauf der thermischen Zersetzung von zwei sich in der Struktur ihrer Kordinationspolyeder unter-, heidenden Formen von Cu(en)2(NCS)(BF4) gefunden.
Cu(en)2(NCS)X (X–=Cl–, Br–, NO 4 – , NO 3 – , BF4 ClO4, Cu(en)2(SCN)2 Cu(en)2(X)2. , Cu(en)2(NCS)X X Cu(en) (NCS)BF4 i .相似文献
115.
Guimarães KL Castro RH Gouvêa D 《Langmuir : the ACS journal of surfaces and colloids》2005,21(25):11645-11650
The standard methods for obtaining adsorption isotherms on colloidal suspensions are usually very time consuming and involve a large number of steps and assumptions that increase the experimental errors. In this work, an alternative method is proposed to evaluate the adsorption behavior of electrosteric-stabilized systems based on electrokinetic sonic amplitude signal measurements. The new method, entitled "zeta-sorption", is noticeably less time-consuming when compared to conventional procedures but showed great precision and reliability confirmed by comparison with data obtained from conventional routes on alumina-polyacrylate and alumina-citric acid aqueous suspensions. The experimental conditions that restrict the applicability of the new method were identified and justified by discussing the possible ion exchanges. 相似文献
116.
The main features of transition structures associated with eight-electron electrocyclic reactions have been studied with Density Functional Theory. It is found that conrotatory electrocyclization reaction of (3Z,5Z)-octa-1,3,5,7-tetraenes takes place via M?bius aromatic transition structures of helical conformation. The reaction is completely periselective. In general, transition structures having outward substituents are preferred with respect to the inward transition structures, irrespective of the pi-donor or pi-acceptor character of the substituent. In contrast with four-electron thermal conrotatory electrocyclic reactions, there is no satisfactory correlation between the difference in energy of activation between inward and outward substituents and the Taft resonance sigma(R) parameter. 相似文献
117.
AurelioG. Cskÿ Rocío Medel M.Carmen Murcia Joaquín Plumet 《Helvetica chimica acta》2005,88(6):1387-1396
A new method for the synthesis of spiro‐β‐lactams tethered to tetrahydrofuran rings is described. The procedure is based on Ru‐catalyzed metathesis sequences with oxanorbornene precursors easily obtained by the Staudinger [2+2] cycloaddition of related imines. 相似文献
118.
Immobilization of protein on ferromagnetic Dacron 总被引:1,自引:0,他引:1
A. M. A. Carneiro LeÃo E. A. Oliveira L. B. Carvalho 《Applied biochemistry and biotechnology》1991,31(1):53-58
Ferromagnetic Dacron (polyethyleneterephthalate) is proposed as a matrix to immobilize proteins covalently. Dacron in powder was magnetized by reacting ferrous (Fe+2) and ferric (Fe+3) ions with its hydrazide form at pH 8.3. Ferromagnetic hydrazide Dacron was converted to ferromagnetic azide Dacron and amyloglucosidase (E.C. 3.2.1.3) was covalently bound through the latter group. The catalytic property of the enzyme was preserved (8% of the specific activity estimated for the soluble enzyme) and all the magnetic amyloglucosidase Dacron derivative was recovered by using a magnetic field. No activity was detected in the supernatant. 相似文献
119.
de Oliveira PR Rittner R 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2005,62(1-3):30-37
The conformational equilibria of 3-X-cyclohexanol [X=F (1), Cl (2), Br (3), I (4), Me (5), NMe(2) (6) and MeO (7)] and of 3-X-methoxycyclohexane [X=F (8), Cl (9), Br (10), I (11), Me (12), NMe(2) (13) and MeO (14)] cis isomers were determined from low temperature NMR spectra and PCMODEL calculated coupling constants. The energy differences between aa and ee conformers were obtained from these data (DeltaG(J)(av) and DeltaG(PC)(av), respectively) and also by the additivity principle from data for the monosubstituted cyclohexanes (DeltaG(Ad)). H-1 and H-3 hydrogen vicinal coupling constants and DeltaG(J)(av) values showed that the diequatorial conformer is predominant in the conformational equilibrium of the compounds studied at low temperature. However, DeltaG(PC)(av) data show that compounds 6 and 7 constitute an exception, since they are almost equally populated by ee and aa at room temperature, due to stabilization of their aa conformer by an intramolecular hydrogen bond. DeltaG(Ad) values, obtained according to the additivity principle, show a better agreement for compounds 2 and 3, since the 1,3-diaxial steric effect is counterbalanced by the formation of an intramolecular hydrogen bond (IAHB). For the remaining compounds, DeltaG(Ad) values underestimate the energy differences, since the 1,3-diaxial steric effect, between X and OH or OCH(3), is absent in the monosubstituted compounds used as references. Moreover, the DeltaG(PC)(av), calculated from the coupling constants, obtained through the PCMODEL program, are rather smaller than the DeltaG(J)(av) values, since the program does not have parameters for the effect, observed in this report, of a substituent at gamma position on coupling constants values for the hydrogen under consideration. 相似文献
120.
Zanolari B Wolfender JL Guilet D Marston A Queiroz EF Paulo MQ Hostettmann K 《Journal of chromatography. A》2003,1020(1):75-89
The bark of catuaba (Erythroxylum vacciniifolium Martius, Erythroxylaceae), a tree native to the northern part of Brazil, was investigated for its alkaloid content. With the aim of obtaining preliminary structure information on-line, the alkaloid extract was analysed by high-performance liquid chromatography coupled to diode array UV detection, to mass spectrometry and to nuclear magnetic resonance. Interpretation of on-line spectroscopic data obtained from this extract led to structural elucidation of six new alkaloids and partial identification of 18 potentially original alkaloids bearing the same tropane skeleton esterified in positions 3 and 6 by 1-methyl-1H-pyrrol-2-carboxylic acid and/or 4-hydroxy-3,5-dimethoxybenzoic acid. 相似文献