Organic monolith frits encased in polyether ether ketone tubing with improved durability for liquid chromatography

Park, Sin-Young; Cheong, Won Jo

doi:10.1002/jssc.201500465

Cited by 7 publications

(15 citation statements)

References 23 publications

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“…It is interesting to note that no other reports appear in the literature in which the work of Shu et al [35] has successfully been repeated. However, during the preparation of this manuscript, a report has recently emerged in the literature in which the combination of sodium and vanadium(V) as catalysts during the PEEK sulphonation step significantly increases the yield of surface anchoring ligands [40], and this technique will be the subject of further research within our group. The remainder of our studies therefore involved the use of alternative column housings with more readily modifiable surface chemistry.…”

Section: Resultsmentioning

confidence: 99%

Polystyrene-co-Divinylbenzene PolyHIPE Monoliths in 1.0 mm Column Formats for Liquid Chromatography

et al. 2016

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Abstract:The reversed phase liquid chromatographic (RP-HPLC) separation of small molecules using a polystyrene-co-divinylbenzene (PS-co-DVB) polyHIPE stationary phases housed within 1.0 mm i.d. silcosteel columns is presented within this study. A 90% PS-co-DVB polyHIPE was covalently attached to the walls of the column housing by prior wall modification with 3-(trimethoxysilyl) propyl methacrylate and could withstand operating backpressures in excess of 200 bar at a flow rate of 1.2 mL/min. Permeability studies revealed that the monolith swelled slightly in 100% acetonitrile relative to 100% water but could nevertheless be used to separate five alkylbenzenes using a flow rate of 40 µL/min (linear velocity: 0.57 mm/s). Remarkable column-to-column reproducibility is shown with retention factor variation between 2.6% and 6.1% for two separately prepared columns.

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Section: Resultsmentioning

confidence: 99%

Polystyrene-co-Divinylbenzene PolyHIPE Monoliths in 1.0 mm Column Formats for Liquid Chromatography

et al. 2016

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“…Sulfonation was carried out according to the method of previous study with some modification. The PEEK tubing (1/16 inch od, 0.25 mm id) was filled with 50% v/v sulfuric acid (10.0 mL) in the presence of vanadium oxide (0.0005 g) and sodium sulfate (0.001 g) and kept for 6 h at 50°C, then for 24 h at room temperature.…”

Section: Methodsmentioning

confidence: 99%

“…The method of previous study was carried out with some modification. The reaction mixture composed of 0.9 mL LMA, 0.1 mL EDMA, 10 mg AIBN, 0.955 mL 1‐propanol, and 0.545 mL 1,4‐butandiol was prepared and purged with N 2 for 10 min.…”

Section: Methodsmentioning

confidence: 99%

“…For such purposes, Teflon‐encased organic monolith frits were prepared as cheap frits in our laboratory by forming organic monolith in common Teflon tubing followed by cutting it into slices . In the next study, polyether ether ketone (PEEK) encased monolith frits were prepared by catalytic sulfonation of a piece of PEEK tubing (0.5 mm id) followed by in situ formation of organic monolith and cutting the tubing into slices to yield disposable frits of improved physical durability . The method of sulfonation of PEEK tubing to prepare PEEK‐encased monolith columns and the method of improved sulfonation yield with catalysts were combined to make frits of improved properties.…”

Section: Introductionmentioning

confidence: 99%

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Polyether ether ketone encased monolith frits made of polyether ether ketone tubing with a 0.25 mm opening resulting in an improved separation performance in liquid chromatography

Park

Cheong

2016

J of Separation Science

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Tiny polyether ether ketone encased monolith frits have been prepared by modified catalytic sulfonation of the inner surface of polyether ether tubing (1.6 mm od, 0.25 mm id) followed by modified formation of organic monolith and cutting of the tubing into slices. The frit was placed below the central hole of the column outlet union and supported by a combination of a silica capillary (0.365 mm od, 0.05 mm id) and a polyether ether ketone sleeve (1.6 mm od, 0.38 mm id) tightened with a nut and a ferrule when the column was packed to prevent sinking of the frit element into the union hole (0.25 mm opening) otherwise. The column packed this way with the frits investigated in this study has shown better separation performance owing to the reduced frit volume in comparison to the column packed with a commercial stainless-steel screen frit. This study establishes the strategy of disposable microcolumns in which cheap disposable frits are used whenever the column is re-packed to yield columns of even better chromatographic performance than the columns with commercial frits.

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“…Polymer monolith frits are prepared using in situ polymerization of methacrylates and other monomer solutions to form a porous polymer monolith within the capillary . A key advantage of polymer frits compared to silica frits is the ability to tune the frit pore size, and thus fluid permeability, based on the monomer solution composition .…”

Section: Introductionmentioning

confidence: 99%

Rapid formation of polymer frits in fused silica capillaries using spatially defined thermal free‐radical initiated polymerization

Sandy

Condarcure

Sutton

et al. 2018

Separation Science Plus

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Column preparation in capillary chromatography commonly relies upon the generation of on‐column porous frits. Here, we report a simple, robust and low‐cost approach for preparing polymer frits on‐column, in a rapid and spatially controlled manner using thermal free‐radical initiated polymerization. In this approach, a simple, temperature‐controlled heating apparatus is positioned adjacent to a 100 μm i.d. fused‐silica capillary for a defined duration. Frits were synthesized in 3‐(trimethoxysilyl)propyl methacrylate modified capillaries using a monomer solution of 2,2‐azobisisobutyronitrile, glycidyl methacrylate, ethylene glycol dimethacrylate, and decanol. Frit length and stability were investigated as a function of polymerization time, temperature, and position. Frit length was easily controlled via a combination of polymerization time and temperature and position was readily controlled using a simple mechanical placement jig. Thermally initiated frits were stable throughout column packing and did not require removal of the capillary polyimide coating. The thermal initiation approach offers higher throughput, with polymerization times of <2 min compared to ≥30 min for UV‐initiated polymerization and significantly reduces the cost, enabling broader access to on‐column frit technology for a variety of capillary separation applications.

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Organic monolith frits encased in polyether ether ketone tubing with improved durability for liquid chromatography

Cited by 7 publications

References 23 publications

Polystyrene-co-Divinylbenzene PolyHIPE Monoliths in 1.0 mm Column Formats for Liquid Chromatography

Polystyrene-co-Divinylbenzene PolyHIPE Monoliths in 1.0 mm Column Formats for Liquid Chromatography

Polyether ether ketone encased monolith frits made of polyether ether ketone tubing with a 0.25 mm opening resulting in an improved separation performance in liquid chromatography

Rapid formation of polymer frits in fused silica capillaries using spatially defined thermal free‐radical initiated polymerization

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