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Summary The complexestrans-[Ru(NH3)4(H2O)PPh3](PF6)2 and [Ru(NH3)5L](PF6)2, (L=AsPh3 or SbPh3) have been isolated and characterized by microanalysis, cyclic voltammetry and ultraviolet-visible spectroscopy. The specific rate constants for the aquation of [Ru(NH3)5L]2+ totrans-[Ru(NH3)4L(H2O)]2+ are (2.5±0.1)×10–5s–1 and (1.8±0.1)×10–5s–1 for L=AsPh3 and SbPh3, respectively, at 25.0±0.1°C; =0.10 mol dm–3, NaO2CCF3. Under the same conditions, the second-order rate constants for the substitution of water intrans-[Ru(NH3)4(H2O)L]2+ by isonicotinamide (isn) are 1.2±0.1, (6.3±0.3)×10–2 and (3.8±0.2)×10–2
m
–1s–1 for L=PPh3, AsPh3, and SbPh3, respectively, suggesting that the order of decreasingtrans-effect is: PPh3AsPh3>SbPh3. The formation constants for thetrans-[Ru(NH3)4L(isn)]2+ complexes are 75±3, (1.40±0.01)×103 and (1.80±0.02)×103M–1 for L=PPh3, AsPh3, and SbPh3, respectively, suggesting that the order of increasingtrans-influence is: SbPh33PPh3. 相似文献
84.
The development of microplasmas for spectrochemical analysis by optical methods is discussed. Recent achievements in miniaturization are highlighted, especially for three types of plasmas, namely high-frequency plasmas, dc-discharges and microwave plasmas. The potentials of each of these groups of plasmas as sources for atomic emission spectrometry are discussed. Literature citations and experiments indicate that the plasmas are also very useful as atom reservoirs for atomic absorption spectrometry. Methods of sampling, including feeding with gas chromatography effluents, the use of electrothermal vaporization, and the evolution of gaseous species (as shown for the case of Hg vapor), are discussed as prominent interfaces to make use of these sources for elemental analysis. 相似文献
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Comparison of different fibers for the solid-phase microextraction of phthalate esters from water 总被引:3,自引:0,他引:3
Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been applied to determine six phthalate esters and one adipate ester in water. The SPME parameters were optimized for several commercially available fibers. A 65-microm polydimethylsiloxane-divinylbenzene (PDMS-DVB) was the fiber selected and was applied to analysis of water from the Ebro river and the industrial port of Tarragona. The studied compounds were found at concentrations ranging from 0.4 microg l(-1) for di-n-butyl phthalate ester (DnBP) to 3.2 microg l(-1) for bis(2-ethylhexyl) phthalate ester (DEHP). The linear range for real samples was from 0.1 to 10 microg l(-1) for most phthalates, and the limits of detection of the method were between 3 and 30 ng l(-1). Repeatability and reproducibility between days (n = 5) for 1 microg l(-1) samples were below 13 and 18%, respectively. 相似文献
88.
G. Ortega Zarzosa S. A. Palomares Sánchez J. R. Martánez Facundo Ruiz M. G. Sánchez-Loredo 《Journal of Sol-Gel Science and Technology》2005,35(1):5-11
Composites containing Pd aggregates dispersed in amorphous silica are of interest from both a fundamental and applied point of view because of their attractive catalytic properties. The silica powders added with palladium, prepared by the sol-gel method, were studied using X-ray diffraction, and IR- and UV-Vis-spectrophotometry. Silica xerogel samples were prepared using a ethanol/H2O/TEOS molar ratio of 4:11.6:1 and loaded with sodium tetrachloropalladate. The silica xerogel microstructure of the powders was studied as a function of annealing temperature. Attention was paid to the evolution of the glass matrix as well as the palladium aggregates in the SiO2 matrix. We found in our samples partial crystallization of the glass matrix in form of quartz and cristobalite phases with palladium oxide and metallic palladium phase at 1000∘C. The Rietveld refinement method was used in order to determine the percentage of the phase contents. 相似文献
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A study of the viability of three derivatizing reagents for obtaining amino acid profiles in honey through high performance liquid chromatography (HPLC) is presented. A method using diode array detection based on a reaction with diethyl ethoxymethylene malonate (DEMM) and two other methods using fluorescence detection based on derivatization with fluorenylmethyl chloroformate (FMOC-Cl) and 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) have been developed. The three methods yield detection limits close to the ppb level, but vary in relation to other analytical characteristics. The use of methyl chloroformate derivatives allows the profile to be obtained with the greatest sensitivity within a short time frame. On applying such methods to honey samples of diverse botanical origin, we observe that the proline values obtained are always lower than those found using the official spectrophotometric method, thereby underlining the advisability of using HPLC methods to reduce uncertainty in these results. 相似文献