Patent US4175037A successfully refreshed from Google Patents.
US4175037A
Expired / Lapsed
US
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Process for packing chromatographic columns
Assignee: Global Life Sciences Solutions USA LLC
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Filing: 1978-04-10
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Granted: 1979-11-20
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Expires: 1998-04-10
Abstract
Abstract Methods for packing chromatographic columns are disclosed, including introducing a packing material into a chromatographic column under the influence of a first pressure differential until the column is filled to a desired extent with the packing material, and subsequently establishing a substantially regular periodic vibration along the length of the column and subjecting the packing material to a second pressure differential, which is preferably greater than the first pressure differential. The substantially regular periodic vibration can comprise ultrasonic vibration, which is preferably applied to the column by immersing it in a liquid bath and subjecting the liquid bath to ultrasonic vibrations.
Inventors
- 👤 Charles H. Benney
- 👤 Thomas J. Filipi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 10:35
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/50; G01N30/56; B; B01; B01D; B01D15/00; B01D15/08; B01D15/10; B01D15/20; B01D15/206; G01N2030/562
Claims Analysis
Total Claims: 36
Claim 1
Independent Claim
104 words
A method of packing a chromatographic column which comprises introducing a packing material into a chromatographic column in a predetermined direction under the influence of a first pressure differential and in the substantial absence of substantially regular periodic vibration until said chromatographic column is filled to a desired extent with said packing material, and subsequently establishing a substantially regular periodic vibration along the length of said column and subjecting said packing material to a second pressure differential therein, said first and second pressure differentials being applied in said predetermined direction so as to aid in filling and packing said column with said packing material.
Claim 2
Independent Claim
104 words
A method of packing a chromatographic column which comprises introducing a packing material into a chromatographic column in a predetermined direction under the influence of a first pressure differential and in the substantial absence of substantially regular periodic vibration until said chromatographic column is filled to a desired extent with said packing material, and subsequently establishing a substantially regular periodic vibration along the length of said column and subjecting said packing material to a second pressure differential therein, said first and second pressure differentials being applied in said predetermined direction so as to aid in filling and packing said column with said packing material.
Claim 3
Dependent Claim
17 words
The method of claim 1 wherein said second pressure differential is greater than said first pressure differential.
Claim 4
Dependent Claim
16 words
The method of claim 1 wherein said subsequently established substantially regular periodic vibration comprises ultrasonic vibration.
Claim 5
Dependent Claim
29 words
The method of claim 3 wherein said ultrasonic vibration is produced by immersing said column in a liquid-containing bath and subjecting said liquid in said bath to ultrasonic vibration.
Claim 6
Dependent Claim
19 words
The method of claim 4 wherein said ultrasonic vibration has a frequency greater than about 15 kilocycles per second.
Claim 7
Dependent Claim
30 words
The method of claim 1 wherein said first and second pressure differentials are produced at least in part by introducing a fluid stream into said column in said predetermined direction.
Claim 8
Dependent Claim
12 words
The method of claim 6 wherein said fluid comprises an inert gas.
Claim 9
Dependent Claim
23 words
The method of claim 7 wherein said inert gas is contacted with a source of radiation prior to its entry into said column.
Claim 10
Dependent Claim
26 words
The method of claim 6 including substantially abating said first pressure differential prior to establishing said substantially regular periodic vibration along the length of said column.
Claim 11
Dependent Claim
32 words
The method of claim 9 wherein said column is subjected to said second pressure differential immediately subsequent to the establishment of said substantially regular periodic vibration along the length of said column.
Claim 12
Dependent Claim
14 words
The method of claim 10 wherein said second pressure differential is established substantially instantaneously.
Claim 13
Dependent Claim
28 words
The method of claim 1 including applying an irregular vibration to said column during the introduction of said packing material under the influence of said first pressure differential.
Claim 14
Dependent Claim
17 words
The method of claim 12 wherein said irregular vibration is produced by tapping intermittently on said column.
Claim 15
Dependent Claim
22 words
The method of claim 6 including reducing the residual pressure in said column after the termination of said second pressure differential therein.
Claim 16
Dependent Claim
28 words
The method of claim 1 wherein said first and second pressure differentials are produced at least in part by applying a vacuum to one end of said column.
Claim 17
Dependent Claim
52 words
The method of claim 2 wherein said column has an inner diameter of between about 0.7 and 1.2 millimeters, said first pressure differential ranges between about 5 and 50 psid per yard of column length and said second pressure differential ranges between about 50 and 500 psid per yard of column length.
Claim 18
Dependent Claim
51 words
The method of claim 2 wherein said column has an inner diameter of greater than about 1.2 millimeters, said first pressure differential ranges between about 5 and 25 psid per yard of column length and said second pressure differential ranges between about 25 to 250 psid per yard of column length.
Claim 19
Dependent Claim
20 words
The method of claim 16 wherein said packing material has an average particle size of between about 5 and 200.
Claim 20
Dependent Claim
33 words
The method of claim 18 wherein said packing material is selected from a group consisting of diatomaceous earth, alumina, glass beads, Teflon beads, graphitized carbon black, molecular sieves, silica gel, and mixtures thereof.
Claim 21
Dependent Claim
38 words
The method of claim 1 wherein said packing material has an average particle size of between about 5 and 75 microns, and further wherein said chromatographic column has an inner diameter of between about 0.7 and 1.2 millimeters.
Claim 22
Dependent Claim
36 words
The method of claim 1 wherein said packing material has an average particle size of between about 50 and 200 microns and wherein said chromatographic column has an inner diameter of greater than about 1.2 millimeters.
Claim 23
Dependent Claim
45 words
The method of claim 1 wherein the introduction of said packing material into said column under the influence of said first pressure differential comprises a plurality of steps, with a portion of said packing material being introduced into said column in each of said steps.
Claim 24
Dependent Claim
20 words
The method of claim 22 including applying an irregular vibration to said column during each of said plurality of steps.
Claim 25
Dependent Claim
33 words
The method of claim 1 wherein said substantially regular periodic vibration is maintained for a period of from about 5 to 30 minutes while subjecting said packing material to said second pressure differential.
Claim 26
Independent Claim
126 words
A method of packing a chromatographic column comprising: (i) introducing a packing material, in the substantial absence of regular periodic vibration, into a chromatographic column under the influence of a first pressure differential ranging from about 5 to 50 psid per yard of column length until said column is filled with the packing material; (ii) subjecting said filled column, while under the influence of said first pressure differential, to ultrasonic vibration; (iii) increasing said pressure differential, while maintaining said ultrasonic vibration to a second pressure differential greater than said first pressure differential and ranging from about 50 to 500 psid per yard of column length for a period of from about 5 minutes to 10 hours; and thereafter (iv) terminating the ultrasonic vibration and pressure differential.
Claim 27
Independent Claim
126 words
A method of packing a chromatographic column comprising: (i) introducing a packing material, in the substantial absence of regular periodic vibration, into a chromatographic column under the influence of a first pressure differential ranging from about 5 to 50 psid per yard of column length until said column is filled with the packing material; (ii) subjecting said filled column, while under the influence of said first pressure differential, to ultrasonic vibration; (iii) increasing said pressure differential, while maintaining said ultrasonic vibration to a second pressure differential greater than said first pressure differential and ranging from about 50 to 500 psid per yard of column length for a period of from about 5 minutes to 10 hours; and thereafter (iv) terminating the ultrasonic vibration and pressure differential.
Claim 28
Dependent Claim
30 words
A method of packing a chromatographic column as defined in claim 25 wherein the first and/or second pressure differentials are maintained by introducing an inert gas stream into said column.
Claim 29
Dependent Claim
30 words
The method of packing a chromatographic column as defined in claim 26 wherein said gas stream is passed into contact with a radiation source prior to entry into said column.
Claim 30
Dependent Claim
48 words
A method of packing a chromatographic column as defined in claim 25 wherein said ultrasonic vibration is imparted to the packing material in said column by immersing said column in a water bath and subjecting said water to ultrasonic vibrations having a frequency greater than about 15 kilohertz.
Claim 31
Dependent Claim
25 words
A method of packing a chromatographic column as defined in claim 25 wherein the passageway through the chromatographic column is coated with a non-reactive metal.
Claim 32
Dependent Claim
18 words
A method of packing a chromatographic column as defined in claim 29 wherein the non-reactive metal is gold.
Claim 33
Independent Claim
82 words
A method of packing a chromatographic column which comprises introducing a packing material into a chromatographic column under the influence of a first pressure differential and in the substantial absence of substantially regular periodic vibration until said chromatographic column is filled to a desired extent with said packing material, and subsequently establishing a substantially regular periodic vibration along the length of said column and subjecting said packing material to a second pressure differential therein, said substantially regular periodic vibration comprising ultrasonic vibration.
Claim 34
Independent Claim
82 words
A method of packing a chromatographic column which comprises introducing a packing material into a chromatographic column under the influence of a first pressure differential and in the substantial absence of substantially regular periodic vibration until said chromatographic column is filled to a desired extent with said packing material, and subsequently establishing a substantially regular periodic vibration along the length of said column and subjecting said packing material to a second pressure differential therein, said substantially regular periodic vibration comprising ultrasonic vibration.
Claim 35
Dependent Claim
30 words
The method of claim 31 wherein said ultrasonic vibration is produced by immersing said column in a liquid containing bath and subjecting said liquid in said bath to ultrasonic vibration.
Claim 36
Dependent Claim
19 words
The method of claim 32 wherein said ultrasonic vibration has a frequency greater than about 15 kilocycles per second.
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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) | 1982-11-19 | 1983-05-21 | 1983-11-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-11-19 | 1987-05-21 | 1987-11-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-11-19 | 1991-05-21 | 1991-11-20 | $7700.00 | Window Closed / Lapsed |