Patent US4159966A successfully refreshed from Google Patents.
US4159966A
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Chromatographic column packing
Assignee: Dow Chemical Co
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Filing: 1977-12-27
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Granted: 1979-07-03
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Expires: 1997-12-27
Abstract
Abstract A gas or liquid chromatographic column packing material prepared by reacting an activated, i.e., active hydrogen-containing, silica and/or alumina support with a reactive hydrogen-containing partitioning agent. The activated silica and/or alumina support is prepared by reacting a Group III metal hydride (boron, aluminum, gallium or indium hydride) with a hydrated silica and/or alumina (a siliceous or aluminaceous mineral having surface hydroxyl groups or a synthetic siliceous or alumina having surface hydroxyl groups). The support has hydrogen atoms attached to an aluminum, boron, gallium or indium atom which in turn is attached through oxygen to the silica and/or alumina. The hydrogen atoms will react with hydrogen of a hydroxyl, amine, thio, amide, or carbohydrate moieties of organic compounds, as for example, alcohols, polyols, polyglycol ethers, polyglycol amines, polyamines, aliphatic and aromatic amides, alkoxy amides, sugars and the like. The long-chain, high molecular weight compounds of these classes are often used as partitioning agents for chromatographic column packings.
Inventors
- 👤 Charles B. Roberts
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 17:32
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/281; B01J20/286; B01J20/30; B01J20/3085; B01J20/3092; B01J20/32; B01J20/3202; B01J20/3204; B01J20/3214; B01J20/3217; B01J20/3231; B01J20/3242; B01J20/3268; B01J20/3272; B01J2220/00; B01J2220/50; B01J2220/54; B01J2220/58
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
102 words
A chromatographic column packing comprising a chemically bond chromatographic partitioning agent selected from the group consisting of aliphatic alcohols, aliphatic polyols, polyglycol ethers, polyglycol amines, polyamines, aliphatic and aromatic amides thio-compounds and alkoxy amides, having molecular weights of from about 200 to 20,000, and sugars bonded through O, S or N to a Group III metal atom which is bound to a silica and/or alumina support through oxygen said group III metal having been incorporated into the structure as a metal hydride and having any hydrogen atoms not replaced by said partitioning agent replaced with a low molecular weight, below 200, alcohol.
Claim 2
Dependent Claim
102 words
A chromatographic column packing comprising a chemically bond chromatographic partitioning agent selected from the group consisting of aliphatic alcohols, aliphatic polyols, polyglycol ethers, polyglycol amines, polyamines, aliphatic and aromatic amides thio-compounds and alkoxy amides, having molecular weights of from about 200 to 20,000, and sugars bonded through O, S or N to a Group III metal atom which is bound to a silica and/or alumina support through oxygen said group III metal having been incorporated into the structure as a metal hydride and having any hydrogen atoms not replaced by said partitioning agent replaced with a low molecular weight, below 200, alcohol.
Claim 3
Dependent Claim
33 words
The packing of claim 1 wherein the Group III metal is aluminum and the partitioning agent is a liquid polyglycol ether having a molecular weight (MW) of from 200 to about several thousand.
Claim 4
Dependent Claim
14 words
The packing of claim 2 wherein the polyglycol has a MW of about 400.
Claim 5
Dependent Claim
16 words
The packing of claim 2 wherein the polyglycol has a MW of about 20,000 (20 M).
Claim 6
Dependent Claim
31 words
The packing of claim 1 wherein the Group III metal is boron and the partitioning agent is a polyglycol ether liquid having a MW of from 200 to about several thousand.
Claim 7
Dependent Claim
31 words
The packing of claim 1 wherein the Group III metal is gallium and the partitioning agent is a polyglycol ether liquid having a MW of from 200 to about several thousand.
Claim 8
Dependent Claim
31 words
The packing of claim 1 wherein the Group III metal is indium and the partitioning agent is a polyglycol ether liquid having a MW of from 200 to about several thousand.
Claim 9
Independent Claim
160 words
A method for preparing bonded chromatographic column packings comprising reacting by contacting an active hydrogen containing silica, alumina or silica-alumina solid support which has been modified by reaction with a Group III metal hydride selected from the group consisting of aluminum, boron, gallium or indium then reacted with a chromatographic partitioning agent selected from the group consisting of aliphatic alcohols, aliphatic polyols, polyglycol ethers, polyglycol amines, polyamines, aliphatic and aromatic amides and alkoxy amides, having molecular weights of from about 200 to 20,000, and sugars neat or in the presence of an inert solvent at from about room temperature to about 100° C. until the evolution of hydrogen is ceased, said partitioning agent being employed in amounts to react with from a few to all of the activated sites on said activated support, and reacting any unreacted hydrogen atom sites of said Group III metal hydride with a low molecular weight, below 200, compound of the class afore set forth.
Claim 10
Independent Claim
160 words
A method for preparing bonded chromatographic column packings comprising reacting by contacting an active hydrogen containing silica, alumina or silica-alumina solid support which has been modified by reaction with a Group III metal hydride selected from the group consisting of aluminum, boron, gallium or indium then reacted with a chromatographic partitioning agent selected from the group consisting of aliphatic alcohols, aliphatic polyols, polyglycol ethers, polyglycol amines, polyamines, aliphatic and aromatic amides and alkoxy amides, having molecular weights of from about 200 to 20,000, and sugars neat or in the presence of an inert solvent at from about room temperature to about 100° C. until the evolution of hydrogen is ceased, said partitioning agent being employed in amounts to react with from a few to all of the activated sites on said activated support, and reacting any unreacted hydrogen atom sites of said Group III metal hydride with a low molecular weight, below 200, compound of the class afore set forth.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1982-07-02 | 1983-01-01 | 1983-07-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-07-02 | 1987-01-01 | 1987-07-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-07-02 | 1991-01-01 | 1991-07-03 | $7700.00 | Window Closed / Lapsed |