Experimental characterization and modelling of analytical monolithic column

A monolithic capillary column containing a composite of metal-organic framework MIL-53(Al) incorporated into hexyl methacrylate-co-ethylene dimethacrylate was prepared to enhance the separation of mixtures of small aromatic compounds by using capillary liquid chromatography. The addition of 10 mg/mL MIL-53(Al) microparticles increased the micropore content in the monolithic matrix and increased the Brunauer-Emmett-Teller surface area from 26.92 to 85.12 m(2) /g. The presence of 1,4-benzenedicarboxylate moieties within the structure of MIL-53(Al) as an organic linker greatly influenced the separation of aromatic mixtures through π-π interactions. High-resolution separation was obtained for a series of alkylbenzenes (with resolution factors in the range 0.96-1.75) in less than 8 min, with 14 710 plates/m efficiency for propylbenzene, using a binary polar mobile phase of water/acetonitrile in isocratic mode. A reversed-phase separation mechanism was indicated by the increased retention factor and resolution as the water percentage in the mobile phase increased. A stability study on the composite column showed excellent mechanical stability under various conditions. The higher resolution and faster separation observed at increased temperature indicated an exothermic separation, whereas the negative values for the free energy change of transfer indicated a spontaneous process.

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“…Darcy's equation was used to calculate the permeability ( K °) of the prepared columns :

K^{\circ} = \frac{u η L}{Δ P}

where Δ P is the pressure drop, L is the column length, η and u are the mobile phase viscosity and mean velocity, respectively.…”

Section: Methodsmentioning

confidence: 99%

Monolithic metal–organic framework MIL‐53(Al)‐polymethacrylate composite column for the reversed‐phase capillary liquid chromatography separation of small aromatics

Yusuf

Badjah‐Hadj‐Ahmed

Aqel

et al. 2016

J of Separation Science

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“…The average diameter of the monolith channels (R) was estimated using the Hagen-Poiseuille equation [26,27]:…”

Section: Hydrodynamic Properties Calculationsmentioning

confidence: 99%

Fabrication of zeolitic imidazolate framework-8-methacrylate monolith composite capillary columns for fast gas chromatographic separation of small molecules

Yusuf

Badjah‐Hadj‐Ahmed

Aqel

et al. 2015

Journal of Chromatography A

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“…The average velocity of mobile phase over the channel section (m) is obtained from integration of the momentum transport equation that derived on the basis of Navier-Stokes equation [36]:…”

Section: Porosity and Bed Permeabilitymentioning

confidence: 99%

Preparation and Evaluation of Long Chain Alkyl Methacrylate Monoliths for Capillary Chromatography

et al. 2011

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This work describes the fabrication of long chain alkyl methacrylate monolithic materials for use as stationary phases in capillary liquid chromatography. After capillary inner wall surface activation with 3-(trimethoxysilyl)propyl methacrylate, monoliths were formed by copolymerization of either lauryl or stearyl methacrylate (LMA or SMA) with ethylene dimethacrylate (EDMA) as crosslinker, in the presence of azobisisobutyronitrile (AIBN) as initiator and a mixture of porogenic solvents including water, 1-propanol and 1,4-butanediol. The composition of the polymerization mixture was changed in terms of monomer, crosslinker and porogen ratio composition, in order to compare the influence of these parameters. The monoliths were prepared in 320 lm i.d. and 200 mm length capillaries. The column morphology was characterized by optical microscopy and scanning electron microscopy (SEM). Total porosity and permeability of each column were calculated using uracil as unretained material by measuring the pressure drop across the columns as a function of linear velocity. The microglobule average size for each column was also determined using Hagen-Poiseuille equation and compared with the SEM images. As expected, a decrease of the porogen to monomer ratio corresponded to smaller microglobules and a lower total porosity. The columns were then chromatographically evaluated; good results were obtained when these capillaries were used to separate mixtures of phenols, aromatics and drug compounds.

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Experimental characterization and modelling of analytical monolithic column

Cited by 22 publications

References 48 publications

Monolithic metal–organic framework MIL‐53(Al)‐polymethacrylate composite column for the reversed‐phase capillary liquid chromatography separation of small aromatics

Monolithic metal–organic framework MIL‐53(Al)‐polymethacrylate composite column for the reversed‐phase capillary liquid chromatography separation of small aromatics

Fabrication of zeolitic imidazolate framework-8-methacrylate monolith composite capillary columns for fast gas chromatographic separation of small molecules

Preparation and Evaluation of Long Chain Alkyl Methacrylate Monoliths for Capillary Chromatography

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