US4016074A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Chromatographic separation
Assignee: Applied Automation Inc
•
Filing: 1975-08-05
•
Granted: 1977-04-05
•
Expires: 1995-08-05
Abstract
Abstract In the liquid chromatographic analysis of a sample containing two or more constituents which are chromatograhically separable using an aqueous ether carrier liquid, an effective amount of water is added to the chromatographic carrier liquid thereby increasing the efficiency of the chromatographic separation and decreasing the incidence of chromatographic column plugging. In a preferred embodiment, addition of a small amount of water to a tetrahydrofuran carrier liquid results in substantial improvement in the analysis of a sulfuric acid alkylation catalyst wherein a sample containing sulfuric acid and other chromatographically separatable organic materials is separated in order to measure the relative proportions of sulfuric acid and hydrocarbon or other materials within the sample.
Inventors
- 👤 Grady T. Porter
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 23:54
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/26; G01N30/28; G01N30/34; B; B01; B01D; B01D15/00; B01D15/08; G01N30/04; G01N30/16; G01N30/20; G01N2030/201
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
78 words
A process comprising: establishing a flow of carrier liquid, comprising a suitable ether solvent and an effective amount of water for preventing column plugging, through a packed chromatographic column suitable for separating hydrocarbon materials from an acid; introducing a liquid sample material comprising an acid and hydrocarbon material into said carrier liquid upstream of said chromatographic column; and passing said carrier liquid containing said sample material through said chromatographic column to separate said acid from said hydrocarbon material.
Claim 2
Dependent Claim
78 words
A process comprising: establishing a flow of carrier liquid, comprising a suitable ether solvent and an effective amount of water for preventing column plugging, through a packed chromatographic column suitable for separating hydrocarbon materials from an acid; introducing a liquid sample material comprising an acid and hydrocarbon material into said carrier liquid upstream of said chromatographic column; and passing said carrier liquid containing said sample material through said chromatographic column to separate said acid from said hydrocarbon material.
Claim 3
Dependent Claim
32 words
A process in accordance with claim 1 wherein said acid comprises sulfuric acid and said solvent material comprises an ether suitable as a liquid chromatographic carrier for both sulfuric acid and hydrocarbons.
Claim 4
Dependent Claim
27 words
A process in accordance with claim 2 wherein said carrier liquid contains up to about 5% by volume, based on the total carrier liquid volume, of water.
Claim 5
Dependent Claim
12 words
A process in accordance with claim 3 wherein said ether comprises tetrahydrofuran.
Claim 6
Dependent Claim
29 words
A process in accordance with claim 4 wherein said sample liquid material comprises at least about 75% by volume, based on the total sample material volume, of sulfuric acid.
Claim 7
Dependent Claim
23 words
A process in accordance with claim 4 wherein said sample liquid material comprises sulfuric acid catalyst material from a sulfuric acid alkylation process.
Claim 8
Dependent Claim
33 words
A process in accordance with claim 6 wherein passing said carrier liquid containing said sample material through said chromatographic column comprises contacting said carrier liquid and sample material with a silica column packing.
Claim 9
Dependent Claim
33 words
A process in accordance with claim 7 wherein said column packing comprises silica having an average pore size of about 150 angstroms and a surface area of about 300 square meters per gram.
Claim 10
Dependent Claim
25 words
A process in accordance with claim 8 wherein said silica has a particle size within the range of from about 15 to about 25 microns.
Claim 11
Dependent Claim
29 words
A process in accordance with claim 9 wherein said sample liquid material comprises at least about 75% by volume, based on the total sample material volume, of sulfuric acid.
Claim 12
Dependent Claim
27 words
A process in accordance with claim 10 wherein said carrier liquid consists essentially of about 97% by volume of tetrahydrofuran and about 3% by volume of water.
Claim 13
Dependent Claim
29 words
A process in accordance with claim 1 wherein said sample liquid material comprises at least about 75% by volume, based on the total sample material volume, of sulfuric acid.
Claim 14
Dependent Claim
26 words
A process in accordance with claim 12 wherein said solvent material comprises an ether suitable as a liquid chromatographic carrier for both sulfuric acid and hydrocarbons.
Claim 15
Dependent Claim
34 words
A process in accordance with claim 13 wherein passing said carrier liquid containing said sample material through said chromatographic column comprises contacting said carrier liquid and sample material with a silica gel column packing.
Claim 16
Dependent Claim
27 words
A process in accordance with claim 14 wherein said carrier liquid contains up to about 5% by volume, based on the total carrier liquid volume, of water.
Claim 17
Dependent Claim
23 words
A process in accordance with claim 14 wherein said sample liquid material comprises sulfuric acid catalyst material from a sulfuric acid alkylation process.
Claim 18
Dependent Claim
84 words
A process comprising: establishing a flow of carrier liquid, comprising a suitable ether and an amount of water effective to prevent column plugging, through a packed chromatographic column packed with a solid chromatographic separation material suitable for separating hydrocarbon materials from an acid; introducing a liquid sample material comprising an acid and hydrocarbon material into said carrier liquid upstream of said chromatographic column; and passing said carrier liquid containing said sample material through said chromatographic column to separate said acid from said hydrocarbon material.
Claim 19
Dependent Claim
84 words
A process comprising: establishing a flow of carrier liquid, comprising a suitable ether and an amount of water effective to prevent column plugging, through a packed chromatographic column packed with a solid chromatographic separation material suitable for separating hydrocarbon materials from an acid; introducing a liquid sample material comprising an acid and hydrocarbon material into said carrier liquid upstream of said chromatographic column; and passing said carrier liquid containing said sample material through said chromatographic column to separate said acid from said hydrocarbon material.
Claim 20
Dependent Claim
31 words
A process in accordance with claim 17 wherein establishing said flow of carrier liquid through said packed chromatographic column comprises establishing said flow through a column packed with a silica material.
Claim 21
Dependent Claim
27 words
A process in accordance with claim 18 wherein said carrier liquid contains up to about 5% by volume, based on the total carrier liquid volume, of water.
Claim 22
Dependent Claim
20 words
A process in accordance with claim 19 wherein said chromatographic separation column is packed with a silica gel packing material.
Claim 23
Dependent Claim
33 words
A process in accordance with claim 20 wherein said column packing comprises silica having an average pore size of about 150 angstroms and a surface area of about 300 square meters per gram.
Claim 24
Dependent Claim
25 words
A process in accordance with claim 21 wherein said silica has a particle size within the range of from about 15 to about 25 microns.
Claim 25
Dependent Claim
12 words
A process in accordance with claim 22 wherein said ether comprises tetrahydrofuran.
Claim 26
Dependent Claim
23 words
A process in accordance with claim 23 wherein said sample liquid material comprises sulfuric acid catalyst material from a fulfuric acid alkylation process.
References Cited (Backward Citations)
US2287732A
Cited
US2430673A
Cited
US3246047A
Cited
US3352643A
Cited
US3522725A
Cited
US3846297A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-04-04 | 1980-10-04 | 1981-04-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-04-04 | 1984-10-04 | 1985-04-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-04-04 | 1988-10-04 | 1989-04-05 | $7700.00 | Window Closed / Lapsed |