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31.
In this work, a capillary electrophoresis (CE) method using indirect UV detection (214nm) for the simultaneous determination of monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), diethylethanolamine (DEEA), monocyclohexylamine (MCHA) and dicyclohexylamine (DCHA) in water/ethanol extracts of wrapping materials containing volatile corrosion inhibitors (VCIs) was described. A running buffer consisting of 0.010 molL(-1) imidazole, 0.010 molL(-1) 2-hydroxyisobutyric acid (HIBA) and 0.010 molL(-1) 18-crown-6 ether enabled separation of the analytes in less than 7 min. A few method validation parameters were determined revealing good migration time repeatability (<0.7% RSD) and area repeatability (< 1.8% RSD). Limits of detection were in the range of 0.52-1.54 mg L(-1). Recovery values were in the range of 94.8-100.9%. The methodology was successfully applied to the analysis of three commercial products (VCI treated paper, foam and plastic). The concentration of amines in these materials varied from 0.050 to 22.3% (w/w). 相似文献
32.
Diana Cruz-Garritz Juventino Garcia-Alejandre Hugo Torrens Cecilio Alvarez Raul A. Toscano Rene Poilblanc Alain Thorez 《Transition Metal Chemistry》1991,16(1):130-135
Summary The thiolato-bridged dinuclear compounds [Rh(-SR)-(COD)]2, where R=p-C6HF4 (1),p-C6H4F (2) and CF3 (3), are obtained from the chloro-bridged analogue by ligand exchange.Compound (1) crystallizes in the space group P1 with a=9.740(3)Å, b=11.642(4)Å, c=13.997(6)Å, =103.87(3)°, =106.98(3)° and =105.10(2)°; z=2. In this dinuclear molecule both Rh atoms have a square planar coordination sharing one edge, namely the two sulphur bridging atoms. The Rh—Rh separation of 2.96 Å is consistent with at most a very weak metal-metal interaction. Upon addition of CO the dimeric [Rh(-SR)(CO)2]2 (4), (5) and (6) are obtained, but addition of PPh3 affords the monomeric species [Rh(SR)(PPh3)-(COD)] (7), (8) and (9). Reactions of the dimeric tetracarbonyl derivatives with PPh3 vary with the nature of R; [Rh(-SR)(PPh3)(CO)]2 is obtained when R=p-C6H4F (10) and CF3 (11) but monomeric [Rh(SR)-(PPh3)(CO)2] (12) is produced when R=p-C6HF4. The latter mononuclear compounds, with R=p-C6H4F (13) and CF3 (14), are also formed by reaction of [Rh(SR)-(PPh3)(COD)] with CO. 相似文献
33.
Joaquim Branco Catarina de Jesus Dias Antnio Pereira Gonalves Teresa Almeida Gasche Antnio Pires de Matos 《Thermochimica Acta》2004,420(1-2):169-173
In our laboratories we have been studying the synthesis and reactivity of binary actinide and lanthanide intermetallic compounds. In this work, the air-oxidation of ThCu2 and AnNi2 (An = Th, U) was followed by thermogravimetry (TG) and the products were characterized by X-ray powder diffraction (XRD). The heterobimetallic oxides obtained are described by the formulas 2MO·ThO2 (M = Cu, Ni) and 2NiO·UO3. The thermogravimetric analysis under hydrogen of these heterobimetallic oxides show one mass loss for 2MO·ThO2 and two mass losses for 2NiO·UO3 over a wide range of temperature (293–1273 K). The characterization by XRD shows that the reduction products are 2M·ThO2 (M = Cu, Ni) and 2Ni·UO2, with all the actinides in the 4+ oxidation state. The actinide heterobimetallic oxides were described as copper or nickel supported catalysts. 相似文献
34.
Nb6.74Ta5.26S4 has been prepared by high temperature techniques. The crystal structure has been determined from single crystal X-ray diffraction data (R/Rw = 0.0588/0.0655). The compound crystallizes in the orthorhombic space group Pnma with unit cell dimensions a = 959.11 (26) pm, b = 336.37 (10) pm, and c = 3282.51 (74) pm. The orthorhombic cell contains four formula units. Its structure is similar to that of Nb-rich sulfides, rather than to that of Ta-rich sulfides. The metal coordinations are capped distorted cubic prisms and pentagonal prisms while the coordinations of sulfur are capped trigonal prisms. 相似文献
35.
Dehydroluciferyl-coenzyme A (L-CoA) was chemically synthesized and characterized by MS, UV-vis spectrometry and RP-HPLC. The identity of the chemically synthesized compound with the one that was produced by firefly luciferase was confirmed. Moreover, the reversibility of the enzymatic conversion of dehydroluciferin ? dehydroluciferyl-adenylate ? L-CoA was also confirmed. The chemical synthesis of L-CoA, described here, may help the clarification of the activator effect of CoA on luciferase bioluminescent assays, in which the enzyme catalyzed formation of L-CoA and the consequent destruction of L-AMP is one of the possible explanations for that effect. 相似文献
36.
The CD spectra of L-2-methylpyrrolidine, L-prolinol, and their N-methylated derivatives have been determined. As in the 2-substituted piperidines, N-methylation results in an inversion of the sign of the Cotton effects (CE). However, the sign of the long-wavelength CE does not follow the simple helicity rule found for 2-substituted piperidines, since the pyrrolidine ring is itself chiral and makes its own contributions to the observed CE's. The rotational contribution due to pyrrolidine ring chirality appears to be opposite in sign to and larger in magnitude than that due to the 2-substituent in both the secondary and the tertiary amines. 相似文献
37.
K. E. Collins M. L. M. M. Granja R. G. Pereira Filho T. A. Anazawa I. C. S. F. Jardim 《Chromatographia》1997,45(1):99-103
Summary Poly(methyloctylsiloxane) (PMOS), sorbed into the pores of HPLC silica particles by solvent evaporation, can function as a
useful stationary phase for reversed-phase chromatography. The present work addresses the question of how the PMOS is distributed
in the pores. Measurements of the surface area (BET, N2) of a series of partially loaded samples (0–40% PMOS, m/m) using a typical batch of HPLC silica (10 μm irregular particles
with 6 nm pores) show that the specific surface area of the samples decreases linearly with the specific loading (mass of
PMOS per gram of silica). This result is not consistent with a “film” model in which the PMOS is deposited uniformly on the
pore walls, but is consistent with a model in which long segmented “plugs” of PMOS are deposited within the pore system.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
38.
39.
G. H. Findenegg K. Gruber J. F. Pereira Friedrich Kohler 《Monatshefte für Chemie / Chemical Monthly》1965,96(2):669-678
Zusammenfassung Es wird der Aufbau eines Kalorimeters zur Bestimmung der spezif. Wärme von Flüssigkeiten beschrieben. Die Messungen werden nach einem kontinuierlichen adiabatischen Aufheizverfahren durchgeführt. Der Fehler in der Molwärme beträgt ca. ±0,4%. Die Methode erlaubt auch innerhalb relativ kleiner Temperaturbereiche eine Aussage über die Temperaturabhängigkeit der Wärmekapazität.Die Molwärme des Systems 1,2-Dibromäthan-Benzol wird zwischen 24 und 29°C über den ganzen Konzentrationsbereich vermessen. Die Mischungen zeigen negative C
p-Werte mit unsymmetrischem Konzentrationsverlauf. Für höhere Temperaturen ist eine Zunahme der Symmetrie zu erwarten.
Mit 3 Abbildungen 相似文献
A calorimeter has been described which serves to determine the heat capacities of liquids. In the measurements the calorimeter and the surroundings are heated continuously, so that adiabatic conditions prevail. The experimental error in the molar heat capacities is ca. ±0,4%. The method also permits the estimation of the temperature dependence of the heat capacities, even within relatively small temperature intervals.The molar heat capacity of the system 1,2-dibromoethane-benzene has been measured between 24° and 29°C for all concentrations. The C p-values of the mixtures are negative and show an asymmetrical dependence on the concentration. For higher temperatures it is expected that the concentration dependence will become more nearly symmetrical.
Mit 3 Abbildungen 相似文献
40.
Huenerbein A Sipoli Marques MA Pereira Ados S de Aquino Neto FR 《Journal of chromatography. A》2003,985(1-2):375-386
The Medical Commission of the International Olympic Committee forbids the use of anabolic androgenic steroids and beta2-agonists to improve athletic performance. In this work we have selected examples of anabolic androgenic compounds and their metabolites to evaluate the GC-MS analysis of some trimethylsilyl derivatives. The aim is to set the best GC conditions to improve the detection within the whole range of analyte elution temperatures. The initial column temperature was changed to 105 or 140 degrees C followed by 40 degrees C min(-1) to 200 degrees C and then 15 degrees C min(-1) to 300 degrees C. Using 140 degrees C as the initial oven temperature it was possible to obtain narrower initial analyte distributions for the compounds that elutes at the beginning of the chromatogram as clenbuterol, mabuterol, epimethylenediol and norandrosterone, without loss of derivatized metabolites signal. Later. eluting analytes, such as the stanozolol metabolites, furazabol and oxandrolone were not affected. Temperatures below 140 degrees C. resulted in partial derivatization for some analytes mainly stanozolol related structures. Therefore evaluation of derivatization conditions as occurring in three steps, the vial, vaporization chamber and capillary column, was thoroughly assessed. The new program temperature improves the signal-to-noise ratio for some compounds and shows adequate resolution for endogenous compounds. Some of the difficult key separations necessary for doping control enforcement were also obtained with the proposed method. 相似文献