Analysis of packing microstructure and wall effects in a narrow-bore ultrahigh pressure liquid chromatography column using focused ion-beam scanning electron microscopy

Reising, Arved E.; Schlabach, Sabine; Baranau, Vasili; Stoeckel, Daniela; Tallarek, Ulrich

doi:10.1016/j.chroma.2017.07.049

Cited by 44 publications

(28 citation statements)

References 70 publications

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“…Quantitative differences between column edge and centre were detected, as has been found in various other studies [4], [31], [38], [39] that will be more prominent in small diameter columns such as these but are insufficient in providing wall support in larger, manufacturing scale columns that are susceptible to compression. Whilst there were obvious changes to measured values 'during' compressive flow, it was of interest that there were slight changes observed in variance between 'before' and 'after' measurements.…”

Section: Figuresupporting

confidence: 70%

Packed bed compression visualisation and flow simulation using an erosion-dilation approach

Johnson

Iacoviello

Hayden

et al. 2020

Journal of Chromatography A

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X-ray computed tomography has been demonstrated to be capable of imaging 1 mL (5 mm diameter, 50 mm height) chromatography packed beds under compression, visualising the 3D structure and measuring changes to geometry of the packing. 1 mL pre-packed columns did not exhibit any structural changes at vendor specified flow rate limits, however cellulose beds did compress at higher flow rates, which was imaged before, during and after flow. This was used to visualise and quantitate changes to porosity, tortuosity and permeability based on simulation of flow through the packed bed structure using the imaging data. When using a high flow rate it was found that a decrease in porosity could be measured during compression before reverting after flow had ceased, with corresponding changes to tortuosity and permeability also occurring. X-ray CT imaging of packed beds and individual beads exposed to foulant-rich process streams resulted in considerable image quality loss, associated with residual biological material. In order to address this, digital processing using an erosion-dilation method was applied at bead and bed scales to computationally alter the porosity by adding or removing material from the existing surface to calculate the impact upon tortuosity factor. The eroded

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Section: Figuresupporting

confidence: 70%

Packed bed compression visualisation and flow simulation using an erosion-dilation approach

Johnson

Iacoviello

Hayden

et al. 2020

Journal of Chromatography A

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“…Fronting peaks are usually observed in column development research because of a poor flow profile in the column . Tailing peaks which are far more common arise because of different radial velocities inside the columns . The band travelling in the wall region has a lower velocity than the center, which results in a tail of an otherwise Gaussian peak .…”

Section: Resultsmentioning

confidence: 99%

The utility of statistical moments in chromatography using trapezoidal and Simpson's rules of peak integration

Misra

Wahab

Patel

et al. 2019

J of Separation Science

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Modern chromatographic data acquisition softwares often behave as black boxes where the researchers have little control over the raw data processing. One of the significant interests of separation scientists is to extract physico-chemical information from chromatographic experiments and peak parameters. In addition, column developers need the total peak shape analysis to characterize the flow profile in chromatographic beds. Statistical moments offer a robust approach for providing detailed information for peaks in terms of area, its center of gravity, variance, resolution, and its skew without assuming any peak model or shape. Despite their utility and theoretical significance, statistical moments are rarely incorporated as they often provide underestimated or overestimated results because of inappropriate choice of the integration method and selection of integration limits. The Gaussian model is universally used in most chromatography softwares to assess efficiency, resolution, and peak position. Herein we present a user-friendly, and accessible approach for calculating the zeroth, first, second, and third moments through more accurate numerical integration techniques (Trapezoidal and Simpson's rule) which provide an accurate estimate of peak parameters as compared to rectangular integration. An Excel template is also provided which can calculate the four moments in three steps with or without baseline correction.

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“…The 3D reconstruction of real packings enables the geometric analysis of their structure 20,21 or their use in posterior computer simulations. 22 Additionally, granular simulations of in silico generated packings permit the study of events difficult to access in real packings, 23 thus enabling the study of timedependent processes such as structure evolution under operation or particle migration. Among several works following this approach, 6,13 the effect of the slurry concentration during packing on the bed structure and efficiency was studied.…”

Section: Introductionmentioning

confidence: 99%

Improved packing of preparative biochromatography columns by mechanical vibration

Martinez

Knaub

Monter

et al. 2019

Biotechnology Progress

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The bioprocessing industry relies on packed-bed column chromatography as its primary separation process to attain the required high product purities and fulfill the strict requirements from regulatory bodies. Conventional column packing methods rely on flow packing and/or mechanical compression. In this work, the application of ultrasound and mechanical vibration during packing was studied with respect to packing density and homogeneity. We investigated two widely used biochromatography media, incompressible ceramic hydroxyapatite, and compressible polymethacrylatebased particles, packed in a laboratory-scale column with an inner diameter of 50 mm.

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Analysis of packing microstructure and wall effects in a narrow-bore ultrahigh pressure liquid chromatography column using focused ion-beam scanning electron microscopy

Cited by 44 publications

References 70 publications

Packed bed compression visualisation and flow simulation using an erosion-dilation approach

Packed bed compression visualisation and flow simulation using an erosion-dilation approach

The utility of statistical moments in chromatography using trapezoidal and Simpson's rules of peak integration

Improved packing of preparative biochromatography columns by mechanical vibration

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