US4042499A
Expired / Lapsed
US
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Liquid adsorption chromatographic apparatus and method
Assignee: Dow Chemical Co
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Filing: 1976-08-02
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Granted: 1977-08-16
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Expires: 1996-08-02
Abstract
Abstract Apparatus and method for the repetitive use of a single packed chromatographic column for the separation of a first solute from at least one second solute of differing polarity, said solutes being commingled in a sample solution. The sample solution is introduced into the inlet end of a single re-usable chromatographic column packed with a charge of porous adsorbent material suited to preferentially adsorb the first solute. A series of different eluants are then passed through the stationary phase to selectively stepwise elute the second solute, and the first adsorbed solute, and to regenerate the stationary phase before introduction of a subsequent sample solution into the column. A control means coordinates the respective sequential processing of each of a plurality of sample solutions through the same charge of porous adsorbent material in the column.
Inventors
- 👤 Tore Ramstad
- 👤 Nels H. Mahle
- 👤 Ralph Matalon
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 11:56
CPC Classifications
B; B01; B01D; B01D15/00; B01D15/08; B01D15/10; B01D15/20; B01D15/203; B01D15/18; G; G01; G01N; G01N30/00; G01N30/02; G01N30/26; G01N30/38; G01N30/40
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
192 words
In a liquid adsorption chromatographic process for the separation of a first solute from at least one second solute of differing polarity said solutes being commingled in a sample solution, by the preferential adsorption of the first solute on a chromatographic column with a solid particulate stationary phase consisting essentially of a charge of porous adsorbent material selected from the group consisting of silica gel, alumina and magnesium silicates, the improvement comprising sequentially: a. passing a first eluant through the stationary phase at a rate sufficient to selectively elute the second solute from the stationary phase; b. passing a second eluant through the stationary phase in a direction countercurrent to the direction of the first eluant to selectively elute the first adsorbed solute from the stationary phase; c. passing a stripping fluid through the stationary phase in a direction cocurrent to the direction of the second eluant to remove second eluant retained on the stationary phase; and d. passing additional first eluant through the stationary phase in a direction cocurrent to the direction of the stripping fluid to re-equilibrate the stationary phase for introduction of a subsequent sample solution into the column.
Claim 2
Dependent Claim
192 words
In a liquid adsorption chromatographic process for the separation of a first solute from at least one second solute of differing polarity said solutes being commingled in a sample solution, by the preferential adsorption of the first solute on a chromatographic column with a solid particulate stationary phase consisting essentially of a charge of porous adsorbent material selected from the group consisting of silica gel, alumina and magnesium silicates, the improvement comprising sequentially: a. passing a first eluant through the stationary phase at a rate sufficient to selectively elute the second solute from the stationary phase; b. passing a second eluant through the stationary phase in a direction countercurrent to the direction of the first eluant to selectively elute the first adsorbed solute from the stationary phase; c. passing a stripping fluid through the stationary phase in a direction cocurrent to the direction of the second eluant to remove second eluant retained on the stationary phase; and d. passing additional first eluant through the stationary phase in a direction cocurrent to the direction of the stripping fluid to re-equilibrate the stationary phase for introduction of a subsequent sample solution into the column.
Claim 3
Dependent Claim
24 words
The method of claim 1 wherein the first solute is an ester of 2,4,5 trichlorophenoxyacetic acid and the second solute is a halogenated dioxin.
Claim 4
Dependent Claim
11 words
The method of claim 2 wherein the halogenated dioxin is 2,3,7,8-tetrachlorodibenzo-p-dioxin.
Claim 5
Dependent Claim
16 words
The method of claim 1 wherein the first eluant is more polar than the second solute.
Claim 6
Dependent Claim
16 words
The method of claim 1 wherein the first solute is more polar than the second solute.
Claim 7
Dependent Claim
26 words
The method of claim 1 including repeating at least once steps (a) through (d) utilizing substantially the same charge of porous adsorbent material in the column.
Claim 8
Dependent Claim
27 words
The method of claim 1 including repeating at least 400 times steps (a) through (d) utilizing substantially the same charge of porous adsorbent material in the column.
Claim 9
Dependent Claim
194 words
A liquid adsorption chromatographic apparatus for the repetitive use of a single packed chromatographic column for the separation of a first solute from at least one second solute of differing polarity, said solutes being commingled in a sample solution, which apparatus comprises: a. a chromatographic column with an inlet end and an outlet end; b. sample supply means, in fluid communication with the inlet end, for passing sample solution into the column; c. respective reservoirs for a first and second eluant and a stripping fluid; d. first eluant supply means, communicating with both the inlet end of the column and the reservoir for the first eluant, for passing the first eluant into the column at the input end of the column; e. second eluant supply means for selectively passing each of the first eluant, the second eluant and the stripping fluid into the column at the output end, said means communicating with each respective reservoir and the outlet end of the column; f. discharging means, communicating with the column, for removing effluent from the column; and g. control means for coordinating the sequential operation of the means of steps (b), (d), (e) and (f).
Claim 10
Dependent Claim
194 words
A liquid adsorption chromatographic apparatus for the repetitive use of a single packed chromatographic column for the separation of a first solute from at least one second solute of differing polarity, said solutes being commingled in a sample solution, which apparatus comprises: a. a chromatographic column with an inlet end and an outlet end; b. sample supply means, in fluid communication with the inlet end, for passing sample solution into the column; c. respective reservoirs for a first and second eluant and a stripping fluid; d. first eluant supply means, communicating with both the inlet end of the column and the reservoir for the first eluant, for passing the first eluant into the column at the input end of the column; e. second eluant supply means for selectively passing each of the first eluant, the second eluant and the stripping fluid into the column at the output end, said means communicating with each respective reservoir and the outlet end of the column; f. discharging means, communicating with the column, for removing effluent from the column; and g. control means for coordinating the sequential operation of the means of steps (b), (d), (e) and (f).
Claim 11
Dependent Claim
24 words
The apparatus of claim 8 wherein the column is packed with a particulate stationary phase consisting essentially of a charge of porous adsorbent material.
Claim 12
Dependent Claim
41 words
The apparatus of claim 8 wherein the column is packed with a particulate stationary phase consisting essentially of a charge of porous adsorbent material containing at least one member selected from the group consisting of silica gel, alumina, and magnesium silicates.
Claim 13
Dependent Claim
23 words
The apparatus of claim 8 wherein the column is packed with a particulate stationary phase consisting essentially of a charge of silica gel.
Claim 14
Dependent Claim
114 words
The apparatus of claim 8 wherein the sample supply means comprises: a. at least one sample reservoir; b. a sampling valve, in fluid communication with the input end of the column, for selectively passing a predetermined amount of the sample solution into the column; c. a sample conduit with an inlet end and an outlet end, the inlet end of the sample conduit communicating with the sample reservoir and the outlet end communicating with the sampling valve; and d. a pump, interposed in the sample conduit, between the sample reservoir and the sampling valve, for inducing the flow of sample solution through the sample conduit and into the sampling valve at a predetermined rate.
Claim 15
Dependent Claim
38 words
The apparatus of claim 12 having a conveying means for supporting and intermittently moving at respective times each of a series of sample reservoirs into a predetermined position for withdrawal of a sample solution into the sample conduit.
Claim 16
Dependent Claim
34 words
The apparatus of claim 12 including a plunger assembly fitted with a hypodermic needle, said plunger being operatively connected to the input end of the sample conduit, for introducing sample solution into the conduit.
Claim 17
Dependent Claim
110 words
The apparatus of claim 8 wherein the first eluant supply means comprises: a. a sampling valve, in fluid communication with the input end of the column, for selectively passing the first eluant into the column; b. a first eluant conduit with a inlet end and an outlet end, the inlet end communicating with the reservoir for the first eluant and the outlet end communicating with the sampling valve; and c. a pump, interposed in the first eluant conduit between the reservoir for the first eluant and the sampling valve, for inducing the flow of first eluant through the first eluant conduit and into the sampling valve at a predetermined rate.
Claim 18
Dependent Claim
37 words
The apparatus of claim 15 including a flow control means, interposed in the first eluant conduit between the sampling valve and the pump, for selecting a fluid passageway between the first eluant conduit and the sampling valve.
Claim 19
Dependent Claim
143 words
The apparatus of claim 8 wherein the second eluant supply means comprises: a. a second eluant conduit with a plurality of inlet ends and an outlet end, with at least one of the inlet ends communicating with one each of the reservoirs for the first eluant, the second eluant and the stripping fluid, and the outlet end communicating with the outlet end of the column; b. a pump, interposed in the second eluant conduit between the reservoirs and the outlet end of the second eluant conduit, for moving the first eluant, the second eluant and the stripping fluid through the second eluant conduit at a predetermined rate; and c. a plurality of control valves interrupting the second eluant conduit between the pump and each reservoir for selectively passing a first eluant, a second eluant and a stripping fluid into the second eluant conduit.
Claim 20
Dependent Claim
35 words
The apparatus of claim 8 including a flow control means, interposed in the second eluant conduit between the column and the pump, for selecting a fluid passageway between the second eluant conduit and the column.
Claim 21
Dependent Claim
14 words
The apparatus of claim 8 wherein the control means includes a multichannel, mechanically-programmable timer.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-08-15 | 1981-02-14 | 1981-08-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-08-15 | 1985-02-14 | 1985-08-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-08-15 | 1989-02-14 | 1989-08-16 | $7700.00 | Window Closed / Lapsed |