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91.
Jinglan Wu Qijun Peng Wolfgang Arlt Mirjana Minceva 《Journal of chromatography. A》2009,1216(50):8793-8805
One of the conventional processes used for the recovery of citric acid from its fermentation broth is environmentally harmful and cost intensive. In this work an innovative benign process, which comprises simulated moving bed (SMB) technology and use of a tailor-made tertiary poly(4-vinylpyridine) (PVP) resin as a stationary phase is proposed. This paper focuses on a model-based design of the operation conditions for an existing pilot-scale SMB plant. The SMB unit is modeled on the basis of experimentally determined hydrodynamics, thermodynamics and mass transfer characteristics in a single chromatographic column. Three mathematical models are applied and validated for the prediction of the experimentally attained breakthrough and elution profiles of citric acid and the main impurity component (glucose). The transport dispersive model was selected for the SMB simulation and design studies, since it gives a satisfactory prediction of the elution profiles within acceptable computational time. The equivalent true moving bed (TMB) and SMB models give a good prediction of the experimentally attained SMB separation performances, obtained with a real clarified and concentrated fermentation broth as a feed mixture. The SMB separation requirements are set to at least 99.8% citric acid purity and 90% citric acid recovery in the extract stream. The complete regeneration in sections 1 and 4 is unnecessary. Therefore the net flow rates in all four SMB sections have been considered in the unit design. The influences of the operating conditions (the flow rate in each section, switching time and unit configuration) on the SMB performances were investigated systematically. The resulting SMB design provides 99.8% citric acid purity and 97.2% citric acid recovery in the extract. In addition the citric acid concentration in the extract is a half of its concentration in the pretreated fermentation broth (feed). 相似文献
92.
Florian Lottes Wolfgang Arlt Mirjana Minceva Erling H. Stenby 《Journal of chromatography. A》2009,1216(30):5687-5695
We report on a series of flow velocity and efficiency profiles, which were measured across the cross section of preparative chromatographic columns packed with different stationary phase materials using computed tomography. It is shown that this non-invasive technique is very useful for visualization of the inner part of a packed column and measurement of the spatial resolved column packing properties. For evaluation of the influence of the particle shape on the velocity distribution and column performance, irregular and spherical reversed phases were studied in detail. The results showed a decreasing velocity towards the column wall most certainly due to a lower permeability. This effect was much less pronounced in the case of spherical particles, indicating a more homogenous packing structure. The influence of the column packing pressure, as a possible measure for improvement of the packing homogeneity was also studied. It was shown that under the same packing conditions spherical particles always lead to a more homogeneous packing. The overall results of this work contribute to the origin of the fact that spherical material is superior to irregular one from the hydrodynamic point of view. 相似文献
93.
ABSTRACTWe compare a recently proposed mixed experimental/theoretical procedure for the derivation of molecular equilibrium structures with several commonly used spectroscopic approaches using experimental data for several isotopologues. We also examine the sensitivity of the results from these approaches to the replacement of the commonly employed atomic masses with nuclear masses. This point is of particular importance for ionic species like HCO+ and HOC+ which serve as numerical reference cases. The scatter of molecular equilibrium geometries derived by different approaches is found to exceed stated statistical uncertainties by about an order of magnitude. 相似文献
94.
Nađa Kostić Yannis Dotsikas Anđelija Malenović Biljana Jančić Stojanović Tijana Rakić Darko Ivanović Mirjana Medenica 《Journal of mass spectrometry : JMS》2013,48(7):875-884
In this article, a step‐by‐step optimization procedure for improving analyte response with implementation of experimental design is described. Zwitterionic antiepileptics, namely vigabatrin, pregabalin and gabapentin, were chosen as model compounds to undergo chloroformate‐mediated derivatization followed by liquid chromatography coupled with tandem mass spectrometry (LC‐MS/MS) analysis. Application of a planned stepwise optimization procedure allowed responses of analytes, expressed as areas and signal‐to‐noise ratios, to be improved, enabling achievement of lower limit of detection values. Results from the current study demonstrate that optimization of parameters such as scan time, geometry of ion source, sheath and auxiliary gas pressure, capillary temperature, collision pressure and mobile phase composition can have a positive impact on sensitivity of LC‐MS/MS methods. Optimization of LC and MS parameters led to a total increment of 53.9%, 83.3% and 95.7% in areas of derivatized vigabatrin, pregabalin and gabapentin, respectively, while for signal‐to‐noise values, an improvement of 140.0%, 93.6% and 124.0% was achieved, compared to autotune settings. After defining the final optimal conditions, a time‐segmented method was validated for the determination of mentioned drugs in plasma. The method proved to be accurate and precise with excellent linearity for the tested concentration range (40.0 ng ml?1–10.0 × 103 ng ml?1). Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
95.
Šime Ukić Mirjana Novak Petar Žuvela Nebojša Avdalović Yan Liu Bogusław Buszewski Tomislav Bolanča 《Chromatographia》2014,77(15-16):985-996
New retention methodology that integrates the conventional quantitative structure-retention relationship (QSRR) approach and gradient retention modeling based on isocratic retention data is developed and presented in this paper. Such an integrated approach removes the general QSRR limitation of highly predefined application conditions (i.e., QSRR are generally applicable only under the conditions used during model development) and allows the prediction of retentions over a wide range of different elution conditions (practically for any isocratic or gradient elution profile). At the same time, it retains the ability to predict retention of components unknown to the model, i.e., the components that have not been used in modeling. Ion-exchange chromatography (IC) analysis of carbohydrates was selected as modeling environment. Three regression techniques were applied and compared during QSRR modeling, namely: stepwise multiple linear regression, partial least squares (PLS), and uninformative variable elimination–PLS regression. The obtained prediction results of the best QSRR model (root-mean-square error of prediction = 22.69 %) were similar to those found in the literature. The upgrade from QSRR to the integrated model did not diminish the predictive ability of the model, indicating an excellent potential of the developed methodology not only in IC but also in chromatography in general. 相似文献
96.
Mirjana Milic Vladimir M. Matic Nenad Dj. Lazarov 《Central European Journal of Physics》2011,9(3):690-697
An extended ASYNNNI model, that beside nearest-neighbour and next-nearest neighbour O-O interactions in the basal plane also
includes interactions between the three nearest oxygen atoms, is used to describe the statistics of CuO chain fragmentation
and to calculate doping and T
c
in YBa2Cu3O6+x
. Calculations were made by the Monte Carlo method employing the recently proposed charge transfer model that assumes only
chains whose length is equal to, or exceeds, a characteristic (critical) length, l
cr
, can provide holes to the layers and contribute to doping p. The obtained p(x) is then combined with a universal T
c
versus p relation to yield T
c
(x) characteristics that correlate remarkably with those reported in recent experiments. The best coordination between theoretical
and experimental T
c
(x) characteristics has been achieved for l
cr
= 2, implying that only isolated basal plane oxygen atoms (trivial chains) do not contribute holes to CuO2 layers. 相似文献
97.
Two novel tiazofurin analogues, 2-(2-benzamido-2-deoxy-β-d-ribofuranosyl)thiazole-4-carboxamide 4 and 2-(2-azido-2-deoxy-β-d-ribofuranosyl)thiazole-4-carboxamide 5, have been synthesized starting from d-glucose and evaluated for their in vitro cytotoxicity against several human leukaemia and solid tumour cell lines. 相似文献
98.
Ivan Damljanović Mirjana Vukićević Rastko D. Vukićević 《Monatshefte für Chemie / Chemical Monthly》2006,137(3):301-305
Summary. The conversion of alicyclic and aliphatic carbonyl compounds as well as aromatic aldehydes into the corresponding oximes (up
to quantitative yields) was achieved by simply grinding these reactants, hydroxylamine hydrochloride and sodium hydroxide
without solvent. However, this procedure was unsuccessful in the case of aromatic ketones. In this case it was necessary to
add silica gel as a catalyst. 相似文献
99.
Austin Anderson Mirjana Jovovic Wayne Smith 《Integral Equations and Operator Theory》2014,80(2):275-291
Let f and g be analytic on the unit disk \({\mathbb{D}}\) . The integral operator T g is defined by \({ T_g f(z) = \int_0^z f(t)g'(t) \,dt, z \in \mathbb{D}}\) . The problem considered is characterizing those symbols g for which T g acting on H ∞, the space of bounded analytic functions on \({\mathbb{D}}\) , is bounded or compact. When the symbol is univalent, these become questions in univalent function theory. The corresponding problems for the companion operator, \({ S_g f(z)= \int_0^z f'(t)g(t) \,dt}\) , acting on H ∞ are also studied. 相似文献
100.