Porous inorganic/organic homogenous copolymeric hybrid materials for chromatographic separation and process for the preparation thereof

a technology of homogenous copolymer hybrid materials and chromatographic separation, which is applied in the direction of chemical/physical processes, inorganic chemistry, component separation, etc., can solve the problems of limited hydrolytic stability, subsequent collapse of chromatographic bed, and loss of analyte retention

Inactive Publication Date: 2005-10-20
WATERS TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, limited hydrolytic stability is a drawback with silica-based columns, because silica may be readily dissolved under alkaline conditions, generally pH>8.0, leading to the subsequent collapse of the chromatographic bed.
Additionally, the bonded phase on a silica surface may be removed from the surface under acidic conditions, generally pH<2.0, and eluted off the column by the mobile phase, causing loss of analyte retention.
However, organic chromatographic materials generally result in columns with low efficiency, leading to inadequate separation performance, particularly with low molecular-weight analytes.
Furthermore, many organic chromatographic materials shrink and swell when the composition of the mobile phase is changed.
In addition, most organic chromatographic materials do not have the mechanical strength of typical chromatographic silica.
These materials, however, were not useful for any liquid based separation application because they are translucent and non-porous.
As a result, these materials lack capacity as a separation material.
Accordingly, it is not possible to make porous monolithic materials that which have a useful capacity as a separation material.
Also, irregularly-shaped particles are generally more difficult to pack than spherical particles.
It is also known that columns packed with irregularly-shaped particles generally exhibit poorer packed bed stability than spherical particles of the same size.
The template agents used in the synthesis of these materials are nonsurfactant optically active compounds, and the use of such compounds limits the range of porogen choices and increases their cost.
The properties of these materials make them undesirable for use as LC packing materials.

Method used

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  • Porous inorganic/organic homogenous copolymeric hybrid materials for chromatographic separation and process for the preparation thereof
  • Porous inorganic/organic homogenous copolymeric hybrid materials for chromatographic separation and process for the preparation thereof
  • Porous inorganic/organic homogenous copolymeric hybrid materials for chromatographic separation and process for the preparation thereof

Examples

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example 1

[0105] One or more organoalkoxysilanes alone or in combination with a one or more alkoxysilanes (all from Gelest Inc., Tullytown, Pa.) were mixed with an alcohol (HPLC grade, J. T. Baker, Phillipsburgh, N.J.) and 0.1 N hydrochloric acid (Aldrich Chemical, Milwaukee, Wis.) in a flask. The resulting solution was agitated and refluxed for 16 hours in an atmosphere of argon or nitrogen. Alcohol was removed from the flask via distillation at atmospheric pressure. Residual alcohol and volatile species were removed by heating at 115-140° C. for 1-2 hours in a sweeping stream of argon or nitrogen or by heating at 125° C. under reduced pressure for 1-2 hours. The resulting polyorganoalkoxysiloxanes were colorless viscous liquids. The chemical formulas are listed in Table 1 for the organotrialkoxysilanes and alkoxysilanes used to make the product polyorganoalkoxysiloxanes (POS). Specific amounts are listed in Table 2 for the starting materials used to prepare these products. Example 1e was ma...

example 2

[0107] A solution of poly(vinyl alcohol) (PVA; 87%-89% hydrolyzed; Ave Mw 13,000-23,000; Aldrich Chemical, Milwaukee, Wis.) in water was prepared by mixing and heating to 80° C. for 0.5 hours. Upon cooling, the PVA solution was combined with a solution comprising divinylbenzene (DVB; 80%; Dow Chemical, Midland, Mich.), a POS selected from Example 1,2,2′-azobisisobutyronitrile (AIBN; 98%, Aldrich Chemical), and or more of the following coporogens: 2-ethylhexanoic acid (2-EHA; Aldrich Chemical), toluene (HPLC grade, J. T. Baker, Phillipsburgh, N.J.), cyclohexanol (CXL; Aldrich Chemical), 1-methyl-2-pyrrolidinone (NMP; Aldrich Chemical). The two solutions were mixed initially using a mechanical stirrer with Teflon paddle and then emulsified by passing the mixture through a static mixer for 10 minutes under an argon flow. With continuous static mixing, the emulsification was heated to 70-80° C. in a period of 30 minutes. Thereafter, the emulsion was agitated mechanically at 70-80° C. fo...

example 3

[0108] A solution of Triton® X-45 (Aq X-45; Fluka, Milwaukee, Wis.), Triton® X-100 (Aq X-100; Fluka, Milwaukee, Wis.), or Methocel E15 (M E15, Dow, Grove City, Ohio; aqueous solution prepared by preheating water to 90° C. before addition of M E15 and cooling to 25° C.) in water and or ethanol was prepared by mixing and heating to 60° C. for 0.5-1.0 hours. In a separate flask, a solution was prepared under a nitrogen purge at ambient temperature by mixing for 0.5 hours divinylbenzene (DVB; 80%; Dow Chemical, Midland, Mich.; washed 3× in 0.1 N NaOH, 3× in water, and then dried MgSO4 from Aldrich Chemical), a POS selected from Example 1, 2,2′-azobisisobutyronitrile (AIBN; 98%, Aldrich Chemical), and one or more of the following reagents: toluene (HPLC grade, J. T. Baker, Phillipsburgh, N.J.), cyclohexanol (CXL; Aldrich, Milwaukee, Wis.), dibutylphthalate (DBP; Sigma; Milwaukee, Wis.), Triton® X-45 (Oil X-45; Fluka, Milwaukee, Wis.). For example 3f, 14 g of Pluronic® F-87 (F-87; BASF; M...

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Abstract

Those skilled in the art will recognize, or be able to ascertain using no more than routine experimentation, numerous equivalents to the specific procedures described herein. Such equivalents were considered to be within the scope of this invention and are covered by the following claims. The contents of all references, issued patents, and published patent applications cited throughout this application are hereby incorporated by reference.

Description

RELATED APPLICATIONS [0001] This application claims benefit of and is a continuation of International Application No. PCT / US03 / 34776, filed Oct. 30, 2003 and designating the United States, which claims benefit of and priority to U.S. Provisional Application No. 60 / 422,580, filed Oct. 30, 2002 . The entire contents of these applications are incorporated herein by reference.BACKGROUND OF THE INVENTION [0002] Packing materials for liquid chromatography (LC) are generally classified into two types: organic materials, e.g., polydivinylbenzene, and inorganic materials, e.g., silica. [0003] As stationary phases for HPLC, silica-based materials result in columns that do not show evidence of shrinking or swelling and are mechanically strong. However, limited hydrolytic stability is a drawback with silica-based columns, because silica may be readily dissolved under alkaline conditions, generally pH>8.0, leading to the subsequent collapse of the chromatographic bed. Additionally, the bonded...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01DB01D15/08B01J20/10B01J20/22B01J20/26B01J20/285B01J20/286B32B5/14C08F20/56C08F230/08C08F265/10C08F283/12C08G77/20C08G77/442C08L53/00G01N30/36
CPCB01J20/26Y10T428/2982B01J20/28019B01J20/28042B01J20/285B01J20/286B01J2220/82C08F230/08C08G77/442C08L53/00C08L53/005B01J20/265C08L2666/02C08F230/085B01J20/10B32B5/14C08F20/56C08F265/10C08F283/12C08G77/20C08J9/35C08J2329/04C08J2383/06
Inventor JIANG, ZHIPINGO'GARA, JOHN E.FISK, RAYMOND P.WYNDHAM, KEVIN D.BROUSMICHE, DARRYL W.
Owner WATERS TECH CORP
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