4 resultados para spectral flow

em Deakin Research Online - Australia


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Thirty-nine CHF patients (New York Heart Association Functional Class = 2.3±0.5; left ventricular ejection fraction 28%±7%; age 65±11 years; 33:6 male:female) underwent 2 identical series of tests, 1 week apart, for strength and endurance of the knee and elbow extensors and flexors, VO2peak, HRV, FBF at rest, and FBF activated by forearm exercise or limb ischemia. Patients were then randomized to 3 months of resistance training (EX, n = 19), consisting of mainly isokinetic (hydraulic) ergometry, interspersed with rest intervals, or continuance with usual care (CON, n = 20), after which they underwent repeat endpoint testing. Combining all 4 movement patterns, strength increased for EX by 21±30% (mean±SD, P<.01) after training, whereas endurance improved 21±21% (P<.01). Corresponding data for CON remained almost unchanged (strength P<.005, endurance P<.003 EX versus CON). VO2peak improved in EX by 11±15% (P<.01), whereas it decreased by 10±18% (P<.05) in CON (P<.001 EX versus CON). The ratio of low-frequency to high-frequency spectral power fell after resistance training in EX by 44±53% (P<.01), but was unchanged in CON (P<.05 EX versus CON). FBF increased at rest by 20±32% (P<.01), and when stimulated by submaximal exercise (24±32%, P<.01) or limb ischemia (26±45%, P<.01) in EX, but not in CON (P<.01 EX versus CON).

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We show how in-line Raman spectroscopy can be used to monitor both reactant and product concentrations for a heterogeneously catalysed Suzuki cross reaction operating in continuous flow. The flow system consisted of an HPLC pump to drive a homogeneous mixture of the reactants (4-bromobenzonitrile, phenylboronic acid, and potassium carbonate) through an oven heated (80°C) palladium catalyst immobilised on a silica monolith. A custom built PTFE in-line flow cell with a quartz window enabled the coupling of an Ocean Optics Raman spectrometer probe to monitor both the reactants and product (4-cyanobiphenyl). Calibration was based on obtaining multivariate spectral data in the range 1530 cm–1 and 1640 cm–1 and using partial least-squares regression (PLSR) to obtain a calibration model which was validated using gas chromatography–mass spectrometry (GCMS) analysis. In-line Raman monitoring of the reactant and product concentrations enable (i) determination of reaction kinetic information such as the empirical rate law and associated rate constant and (ii) optimisation of either the product conversion (61 % at 0.02 mL min–1 generating 17 g h–1) or product yield (14 % at 0.24 mL min–1 generating 53 g h–1).

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The performance of curtain flow chromatography column technology with MS detection was evaluated for the analysis of labile compounds. The curtain flow column design allows for separations that are faster and/or more sensitive than conventional columns, depending on how exactly the curtain flow column is configured. For example, when mass spectral detection is employed, the curtain flow column can yield separations that are 5-times faster than conventional columns when the curtain flow and the conventional columns have the same internal diameter. Or when the internal diameter of the conventional column is reduced in order to yield the same analytical through-put as the curtain flow column, the sensitivity on the curtain flow column can be as much as 66-fold higher than the conventional column. As a consequence of the higher analytical through-put less standardization is required in the analysis of labile compounds because less sample degradation is apparent. Consequently the sample integrity is preserved yielding data of a higher quality.