Theoretical study of sequential centrifugal partition chromatography

Völkl, J.; Arlt, Wolfgang; Minceva, Mirjana

doi:10.1002/aic.13812

Cited by 25 publications

(15 citation statements)

References 27 publications

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“…A further improvement of the transferred method could follow by applying the space between the peaks method [13] or additional simulations as part of theoretical parameter studies. This can be done by a parameter study, where different flow rates and injection volumes can be evaluated by applying the linear correlations of S F and N i from the short-cut method as input, e.g., as part of a simulation study based on the equilibrium cell model [30,45]. In this context, individual requirements such as purity, yield, productivity, and solvent consumption can be assessed.…”

Section: Discussionmentioning

confidence: 99%

Evaluation of Inter-Apparatus Separation Method Transferability in Countercurrent Chromatography and Centrifugal Partition Chromatography

Roehrer

Minceva

2019

Separations

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In the countercurrent chromatography and centrifugal partition chromatography, separation method transfer and scale-up is often described as an easy and straightforward procedure. Separation methods are usually developed on lab scale columns and subsequently transferred using linear scale-up factors to semi-preparative or preparative columns of the same column design. However, the separation methods described in the literature have been developed on various columns of different design and size. This is accompanied by differences in the separation behavior of the columns and therefore makes separation method transfer difficult. In the current study, the separation performances of different columns were evaluated and compared. Linear correlations of stationary phase retention and column efficiency as a function of flow rate were found to be applicable for the calculation of separation resolution in the typical operating range of each column. In this context, a two-point short-cut approach for a fast column characterization is recommended. This allows a quick prediction of the separation method transferability between columns, which saves experimental time and effort. In the current study, the transferability between five different columns from lab scale countercurrent chromatography (CCC) (18 mL) to semi-preparative centrifugal partition chromatography (CPCs) (250 mL) with different cell numbers and design is investigated.Separations 2019, 6, 36 2 of 16 often differ significantly in column design as well as size. Consequently, suitable operating parameters (e.g., flow rate, rotational speed) and separation performances (e.g., stationary phase retention, column efficiency) between the columns are also different. Therefore, efficient and systematic strategies are needed to quickly transfer separation methods between different apparatuses.In conventional liquid chromatography (LC), e.g., High-performance liquid chromatography (HPLC), clear rules exist on how to transfer batch separation methods between columns. Here, columns are of cylindrical shape and packed with a solid stationary phase. The design parameters are column diameter, length and stationary phase particle size. In general, sample load, i.e., the feed sample concentration and relative volumetric column loading, is kept constant and the same or a better number of theoretical stages is aimed for. To achieve these criteria when transferring a separation method, usually the particle size and the column length are kept the same, while the cross sectional area and the mobile phase flow rate are adjusted in order to guarantee the same mobile phase velocity in both columns [6]. In literature, this approach was studied also for applicability in CCC and CPC. The same mobile phase linear velocity was used in both columns when transferring the separation method between columns [7]. However, this is difficult, especially in CPC, since the cross-sectional area of the CPC cells is not constant and changes along the cells of different geometries. It was shown, that an av...

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Section: Discussionmentioning

confidence: 99%

Evaluation of Inter-Apparatus Separation Method Transferability in Countercurrent Chromatography and Centrifugal Partition Chromatography

Roehrer

Minceva

2019

Separations

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“…This is in agreement with the theory behind the derived constraints on the TMB CPC operating parameters. According to these, the time needed to reach CSS is the same for all (t Des , t As ) pairs inside the separation region giving the same t Des /t As ratio [8].…”

Section: Influence Of the Cycle Duration On The Scpc Separationmentioning

confidence: 92%

“…It should be mentioned that, for a selected feed flow rate, in each step of the cycle the mobile phase flow rate should be adopted in a way that the flow rates in the two columns are below the maximum allowed mobile phase flow rate. This issue is commented on in more detail in [8].…”

Section: Restrictions Operating Parameters Constraintsmentioning

confidence: 96%

“…2. More details about the derivation of the operating parameters constraints can be found elsewhere [8].…”

Section: Selection Of the Operating Parametersmentioning

confidence: 99%

“…The proposed approach is systematic and includes minimal experimental effort. The starting point is a set of implicit constraints on the operating parameters to achieve complete separation of a binary feed mixture, which were derived based on the assumption of instantaneous solute partition equilibrium [8]. To select the unit operating parameters (four flow rates and two step times), the only parameters that should be determined experimentally are the partition coefficients of the solutes and the column hydrodynamics (i.e., stationary phase retention).…”

Section: Introductionmentioning

confidence: 99%

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Sequential Centrifugal Partition Chromatography: A New Continuous Chromatographic Technology

2011

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In solid-support-free liquid-liquid chromatography, both phases can be used as a mobile phase and, moreover, their role and flow direction can be reversed during the course of the separation. This is the background of the concept of sequential centrifugal partition chromatography (sCPC) developed to perform a continuous separation in a cyclic manner. The feed is continuously introduced between two centrifugal partition chromatographic columns and two products are alternately collected at the opposite ends of the columns. In this work, a method is presented to select the operating parameters of an sCPC unit for the complete separation of a binary feed mixture. The method uses, as a basis, a restricted number of experiments needed to determine the distribution equilibrium of the components to be separated and to evaluate the column hydrodynamics. The method was validated experimentally for the separation of a binary mixture of hydroquinone and pyrocatechol.

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Continuous fractionation of multicomponent mixtures with sequential centrifugal partition chromatography

Goll

Minceva

2016

AIChE Journal

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The applicability of sequential centrifugal partition chromatography for continuous fractionation of multicomponent mixtures, represented here by a mixture of four parabens with very similar molecular structure, was studied. The fractionation of the quaternary feed mixture was regarded as a separation of a pseudo-binary mixture. The model-based approach was used to select the biphasic liquid system and the unit operating parameters. All desired fractions were recovered with purities >99%. The influence of the solute concentration on the density, viscosity and volume ratio of the phases as well as on the partitioning of the solutes between the two phases was investigated. According to these results, possibilities for increasing the throughput were proposed and validated experimentally. For example, butyl paraben with a purity !99% was continuously separated from the rest of the parabens in a 250 mL unit with a throughput of 3.24 g h 21 and a solvent consumption of 0.33 L g 21 .sCPC unit operating parameters: F U;1 5 18 mL min 21 , F L;2 5 18 mL min 21 , F U:F 5 3 mL min 21 , F L:F 5 3 mL min 21 , S F 5 0.50, c i;As 5 4.5 mg mL 21 , c i;Des 5 4.5 mg mL 21 , R 5 1700 rpm, V C 5 247 mL, t As 5 4 min, t Des 5 9.25 min.

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Theoretical study of sequential centrifugal partition chromatography

Cited by 25 publications

References 27 publications

Evaluation of Inter-Apparatus Separation Method Transferability in Countercurrent Chromatography and Centrifugal Partition Chromatography

Evaluation of Inter-Apparatus Separation Method Transferability in Countercurrent Chromatography and Centrifugal Partition Chromatography

Sequential Centrifugal Partition Chromatography: A New Continuous Chromatographic Technology

Continuous fractionation of multicomponent mixtures with sequential centrifugal partition chromatography

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