Synthesis of Porous Zirconia Spheres for HPLC by Polymerization-Induced Colloid Aggregation (PICA)

Sun, Lifang; Annen, Michael J.; Lorenzano-Porras, Francisco; Carr, Peter W.; McCormick, Alon V.

doi:10.1006/jcis.1994.1125

Cited by 60 publications

(46 citation statements)

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“…6.25 mL of 37% formaldehyde solution was added and mixed for an additional minute. 25 Af ter 2 h of polymerization, the reaction was quenched with 300 mL or a sixfold amount of DI water. 25 The mi crometer scale aggregates of colloids were separated by batch centrifugation at 1500 rpm for 12 min.…”

Section: Methodsmentioning

confidence: 99%

“…25 Af ter 2 h of polymerization, the reaction was quenched with 300 mL or a sixfold amount of DI water. 25 The mi crometer scale aggregates of colloids were separated by batch centrifugation at 1500 rpm for 12 min. Pre cipitated aggregates were resuspended in 2propanol, collected, and dried in a vacuum oven at 90°C/12 h and 175°C/16 h. Further heat treatment was com prised of calcination and sintering in a muffle furnace at 375°C/2 h, 750°C/6 h, and 900°C/3 h. A 20°C/min ramp was used between 375°C and 750°C, while 40°C/ min was used to reach 900°C.…”

Section: Methodsmentioning

confidence: 99%

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Impact of Porogens on the Pore Characteristics of Zirconia Particles Made by Polymer-Induced Colloid Aggregation

Pattanayak

Subramanian

2009

International Journal of Applied Ceramic Technology

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Zirconia particles were prepared from a 20% colloidal sol (ZrO2) by the polymer‐induced colloid aggregation (PICA) process, both in the presence and absence of porogens. Specifically, porous zirconia particles having varying porosity were prepared by a two‐step protocol wherein a porogen was first embedded during the particle synthesis, followed by its removal in a subsequent step. In this research study, the ability of four different types of porogens, viz. fumed silica, micronized high molecular weight polyethylene emulsion ME09730, and microcrystalline waxes ME48040M2 and ME98040M1, to impact the pore size, porosity, and pore area were investigated. Particle morphology and porosity of the resultant particles were characterized by scanning electron microscopy, mercury intrusion–extrusion porosimetry, and the nitrogen adsorption–desorption sorptometry. Optimal ratios of zirconia sol and porogen to yield the largest unimodal distribution of pores were determined. Porous zirconia particles were obtained after the removal of porogen, followed by a calcination and sintering protocol. Particle aggregates were typically 7–45 μm in diameter, with BET surface areas between 21 and 54 m2/g and pores ranging from 18 to 120 nm in diameter. The nitrogen sorptometry and mercury porosimetry data of these support particles were modeled to calculate surface fractal dimension, pore accessibility parameters, pore network, and pore geometry.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Impact of Porogens on the Pore Characteristics of Zirconia Particles Made by Polymer-Induced Colloid Aggregation

Pattanayak

Subramanian

2009

International Journal of Applied Ceramic Technology

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“…The dried, free-flowing powder was then subjected to a staged heating process both to remove the polymer and to 1 To whom correspondence should be addressed. 2 Increasing the polymer precursor to zirconia ratio also increases the particle size, but we find it also allows the aggregates to form clusters.…”

Section: Methodsmentioning

confidence: 99%

“…We have previously described a procedure-polymerization-induced colloid aggregation (PICA)-for the controlled aggregation of zirconia colloids into aggregate particles with a narrow particle size distribution (1,2). A polymer formed in the colloidal sol assists the aggregation.…”

Section: Introductionmentioning

confidence: 99%

Synthesis of Porous Zirconia Spheres—Mechanism and Prospects for Multistep Processing

Sathyagal

Carr

McCormick

1999

Journal of Colloid and Interface Science

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“…These particles have large (300 Å), well-connected pores suitable for use as substrates for HPLC stationary phases (13). Table 1 lists various zirconia-based stationary phases we have reported and are currently studying.…”

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confidence: 99%

Peer Reviewed: Zirconia Stationary Phases for Extreme Separations

Dunlap¹,

McNeff²,

Stoll³

et al. 2001

Anal. Chem.

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113

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See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.N O V E M B E R 1 , 2 0 0 1 / A N A LY T I C A L C H E M I S T R Y 5 9 9 A hirty-eight new reversed-phase (RP) columns with various stationary phases were introduced at Pittcon 2001-a stark contrast to the early days of HPLC when, to paraphrase Henry Ford, you could get any kind of column you liked as long as it was an octadecyltrichlorosilane (ODS) modified-silica column (1). Currently, stationary phases for HPLC range from the large family of RPs, including those based on the chemical inertness of zirconia (ZrO 2 ), to highly selective, nearly specific, bioaffinity phases.With an emphasis on RPs, technology is aimed at improving column durability under adverse conditions (especially high pH), column-to-column and batch-to-batch reproducibility, peak tailing toward cationic (basic) analytes, unique selectivities, and speed. Columns are also designed for specific areas, such as LC/MS, and for specific improvements, such as minimal solvent consumption. Recently introduced polar-embedded phases that provide unique selectivity and can be used in highly aqueous media have become particularly popular.Many new phases have emerged from research directed at producing more durable materials, understanding and minimizing silanol-analyte interactions, and addressing the need for more selective separations in all modes of LC (2-5). Another important trend has been the development of spe cifi cally nonporous silica and zirconia particles and shorter and wider column geometries for faster analysis times (6).Most new phase development work focuses on silica-based materials; however, silica's inherent instability at pH > 7-8 and higher dissolution rates at elevated temperatures significantly limit the range of aqueous media conditions. Stabilized silicas, hybrid inorganic-organic particles, and novel support materials-synthetic organic polymers, alumina, and other metal oxides-have been designed to overcome these shortcomings (7-9). Peter W. CarrUniversity of Minnesota Z Zi ir rc co on ni ia a S St ta at ti io on na ar ry y P Ph ha as se es s f fo or r E Ex xt tr re em me e S Se ep pa ar ra at ti io on ns s

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Synthesis of Porous Zirconia Spheres for HPLC by Polymerization-Induced Colloid Aggregation (PICA)

Cited by 60 publications

References 0 publications

Impact of Porogens on the Pore Characteristics of Zirconia Particles Made by Polymer-Induced Colloid Aggregation

Impact of Porogens on the Pore Characteristics of Zirconia Particles Made by Polymer-Induced Colloid Aggregation

Synthesis of Porous Zirconia Spheres—Mechanism and Prospects for Multistep Processing

Peer Reviewed: Zirconia Stationary Phases for Extreme Separations

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