US4160728A
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US
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Bimodal chromatographic resolving zone
Assignee: BIO-TECHNICAL RESOURCES LP
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Filing: 1977-08-22
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Granted: 1979-07-10
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Expires: 1997-08-22
Abstract
Abstract Disclosed herein is a resolving zone for a chromatograph comprising a plurality of porous, silica macroparticles chosen to provide the resolving zone with a bimodal pore distribution, the average pore size for each mode being such that the linear portions of the molecular weight calibration curve for each pore size in the bimodal distribution are nonoverlapping and the pore volume of each mode being such that the aforesaid linear portions are substantially parallel. The macroparticles can be either totally or superficially porous. The resolving zone can be composed of either a plurality of macroparticles each having a bimodal pore distribution or a plurality of macroparticles having one pore size distribution and a plurality of macroparticles having another pore distribution.
Inventors
- 👤 Joseph J. Kirkland
- 👤 Wallace W. Yau
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 03:19
CPC Classifications
B; B01; B01D; B01D15/00; B01D15/08; B01D15/26; B01D15/34; B01J; B01J20/00; B01J20/28; B01J20/28002; B01J20/28004; B01J20/28014; B01J20/28016; B01J20/28054; B01J20/28088; B01J20/28092; B01J20/281; B01J20/282; B01J20/286; B01J20/30; B01J20/32; B01J20/3231; B01J20/3289; B01J20/3291; B01J20/3295; B01J2220/00; B01J2220/50; B01J2220/54; G; G01; G01N; G01N30/00; G01N30/02; G01N30/50; G01N30/52; G01N2030/524; G01N2030/525
Claims Analysis
Total Claims: 43
Claim 1
Independent Claim
131 words
A resolving zone for a chromatograph comprising a plurality of macroparticles, said macroparticles being chosen to provide said resolving zone with a bimodal pore size distribution, the average pore size for each mode being such that the linear portions of the molecular weight calibration curve for each pore size in the bimodal distribution are substantially nonoverlapping and the pore volume of each mode being such that said linear portions are substantially parallel, wherein the component of the bimodal pore size distribution having a smaller average pore size provides from about 30 to 60% of the total pore volume and the component of the bimodal pore size distribution having a larger average pore size provides from about 70 to 40% of the total pore volume of the macroparticles in the resolving zone.
Claim 2
Dependent Claim
131 words
A resolving zone for a chromatograph comprising a plurality of macroparticles, said macroparticles being chosen to provide said resolving zone with a bimodal pore size distribution, the average pore size for each mode being such that the linear portions of the molecular weight calibration curve for each pore size in the bimodal distribution are substantially nonoverlapping and the pore volume of each mode being such that said linear portions are substantially parallel, wherein the component of the bimodal pore size distribution having a smaller average pore size provides from about 30 to 60% of the total pore volume and the component of the bimodal pore size distribution having a larger average pore size provides from about 70 to 40% of the total pore volume of the macroparticles in the resolving zone.
Claim 3
Dependent Claim
54 words
The resolving zone of claim 1 wherein each component of the bimodal pore size distribution provides about 40 to 60% of the total pore volume of the macroparticles in the resolving zone and wherein the average pore sizes of the components of the bimodal pore size distribution are about one order of magnitude apart.
Claim 4
Dependent Claim
63 words
The resolving zone of claim 2 wherein the component of the bimodal pore size distribution having the smaller average pore size provides about 40 to 55% of the total pore volume and the component of the bimodal pore size distribution having the larger average pore size provides about 45 to 60% of the total pore volume of the macroparticles in the resolving zone.
Claim 5
Dependent Claim
30 words
The resolving zone of claim 3 wherein each component of the bimodal pore size distribution provides about 45-55% of the total pore volume of the macroparticles in the resolving zone.
Claim 6
Dependent Claim
47 words
The resolving zone of claim 3 wherein the macroparticles have an average diameter of about 0.5 to 500 microns and are composed of a plurality of microparticles having a diameter of about 0.005 to about 1.0 micron and wherein each macroparticle has a bimodal pore size distribution.
Claim 7
Dependent Claim
82 words
The resolving zone of claim 3 wherein the macroparticles have an average diameter of about 0.5 to 500 microns and are composed of a plurality of microparticles having a diameter of about 0.005 to about 1.0 micron, the bimodal pore size distribution in the zone being provided by a plurality of macroparticles having an average pore size within one mode of the bimodal distribution and a plurality of macroparticles having an average pore size within the other mode of the bimodal distribution.
Claim 8
Dependent Claim
40 words
The resolving zone of claim 5 wherein said macroparticles are totally porous macroparticles having an average diameter of about 0.5 to 50 microns and are composed of a plurality of microparticles having an average diameter of 0.005 to 0.5 micron.
Claim 9
Dependent Claim
11 words
The resolving zone of claim 7 wherein the macroparticles are silica.
Claim 10
Dependent Claim
39 words
The resolving zone of claim 5 wherein the macroparticles are superficially porous having an average diameter of about 5 to 50 microns and are composed of a macrocore surrounded by microparticles having a diameter of 0.1 to 0.5 micron.
Claim 11
Dependent Claim
14 words
The resolving zone of claim 9 wherein the macroparticles are composed primarily of silica.
Claim 12
Dependent Claim
41 words
The resolving zone of claim 6 wherein the macroparticles are totally porous macroparticles having an average diameter of about 0.5 to 50 microns and are composed of a plurality of microparticles having an average diameter of about 0.005 to 0.5 micron.
Claim 13
Dependent Claim
11 words
The resolving zone of claim 11 wherein the macroparticles are silica.
Claim 14
Dependent Claim
40 words
The resolving zone of claim 6 wherein the macroparticles are superficially porous having an average diameter of about 5 to 50 microns and are composed of a macrocore surrounded by microparticles having a diameter of about 0.1 to 0.5 micron.
Claim 15
Dependent Claim
14 words
The resolving zone of claim 13 wherein the macroparticles are composed primarily of silica.
Claim 16
Dependent Claim
115 words
In a process for chromatographic separation comprising the steps (a) placing the material to be separated in a carrier fluid; (b) contacting the carrier fluid with a resolving zone; and (c) determining the extent of retention of said material in the zone, the improvement comprising using a resolving zone comprising a plurality of macroparticles, said macroparticles being chosen to provide said resolving zone with a bimodal pore size distribution, the average pore size for each mode being such that the linear portions of the molecular weight calibration curve for each pore size in the bimodal distribution are substantially nonoverlapping and the pore volume of each mode being such that said linear portions are substantially parallel.
Claim 17
Dependent Claim
115 words
In a process for chromatographic separation comprising the steps (a) placing the material to be separated in a carrier fluid; (b) contacting the carrier fluid with a resolving zone; and (c) determining the extent of retention of said material in the zone, the improvement comprising using a resolving zone comprising a plurality of macroparticles, said macroparticles being chosen to provide said resolving zone with a bimodal pore size distribution, the average pore size for each mode being such that the linear portions of the molecular weight calibration curve for each pore size in the bimodal distribution are substantially nonoverlapping and the pore volume of each mode being such that said linear portions are substantially parallel.
Claim 18
Dependent Claim
64 words
The process of claim 15 wherein the component of the bimodal pore size distribution having a smaller average pore size provides from about 30 to 60% of the total pore volume and the component of the bimodal pore size distribution having a larger average pore size provides from about 70 to 40% of the total pore volume of the macroparticles in the resolving zone.
Claim 19
Dependent Claim
52 words
The process of claim 16 wherein each component of the bimodal pore size distribution provides about 40 to 60% of the total pore volume of the macroparticles in the resolving zone and wherein the average pore sizes of the components of the bimodal pore distribution are about one order of magnitude apart.
Claim 20
Dependent Claim
62 words
The process of claim 17 wherein the component of the bimodal pore size distribution having the smaller average pore size provides about 40 to 55% of the total pore volume and the component of the bimodal pore size distribution having the larger average pore size provides about 45 to 60% of the total pore volume of the macroparticles in the resolving zone.
Claim 21
Dependent Claim
29 words
The process of claim 18 wherein each component of the bimodal pore size distribution provides about 45-55% of the total pore volume of the macroparticles in the resolving zone.
Claim 22
Dependent Claim
46 words
The process of claim 18 wherein the macroparticles have an average diameter of about 0.5 to 500 microns and are composed of a plurality of microparticles having a diameter of about 0.005 to about 1.0 micron and wherein each macroparticle has a bimodal pore size distribution.
Claim 23
Dependent Claim
81 words
The process of claim 18 wherein the macroparticles have an average diameter of about 0.5 to 500 microns and are composed of a plurality of microparticles having a diameter of about 0.005 to about 1.0 micron, the bimodal pore size distribution in the zone being provided by a plurality of macroparticles having an average pore size within one mode of the bimodal distribution and a plurality of macroparticles having an average pore size within the other mode of the bimodal distribution.
Claim 24
Dependent Claim
39 words
The process of claim 20 wherein said macroparticles are totally porous macroparticles having an average diameter of about 0.5 to 50 microns and are composed of a plurality of macroparticles having an average diameter of 0.005 to 0.5 micron.
Claim 25
Dependent Claim
38 words
The process of claim 20 wherein the macroparticles are superficially porous having an average diameter of about 5 to 50 microns and are composed of a macrocore surrounded by microparticles having a diameter of 0.1 to 0.5 micron.
Claim 26
Dependent Claim
40 words
The process of claim 21 wherein the macroparticles are totally porous macroparticles having an average diameter of about 0.5 to 50 microns and are composed of a plurality of microparticles having an average diameter of about 0.005 to 0.5 micron.
Claim 27
Dependent Claim
39 words
The process of claim 21 wherein the macroparticles are superficially porous having an average diameter of about 5 to 50 microns and are composed of a macrocore surrounded by microparticles having a diameter of about 0.1 to 0.5 micron.
Claim 28
Dependent Claim
99 words
A powder for chromatographic separations consisting essentially of a plurality of discrete porous macroparticles, each macroparticle having an average diameter of about 0.5 to about 500 microns and a bimodal pore size distribution, the average pore sizes of the components of the bimodal distribution being about one order of magnitude apart and the component of the bimodal distribution having the smaller average pore size provides from about 30 to 60% of the total pore volume and the component of the bimodal distribution having the larger average pore size provides from about 70 to 40% of the total pore volume.
Claim 29
Dependent Claim
99 words
A powder for chromatographic separations consisting essentially of a plurality of discrete porous macroparticles, each macroparticle having an average diameter of about 0.5 to about 500 microns and a bimodal pore size distribution, the average pore sizes of the components of the bimodal distribution being about one order of magnitude apart and the component of the bimodal distribution having the smaller average pore size provides from about 30 to 60% of the total pore volume and the component of the bimodal distribution having the larger average pore size provides from about 70 to 40% of the total pore volume.
Claim 30
Dependent Claim
56 words
The powder of claim 26 wherein the component of the bimodal pore size distribution having the smaller average pore size provides about 40 to 55% of the total pore volume and the component of the bimodal pore size distribution having the larger average pore size provides from about 60 to 45% of the total pore volume.
Claim 31
Dependent Claim
26 words
The powder of claim 27 wherein each component of the bimodal pore size distribution provides from about 45 to about 55% of the total pore volume.
Claim 32
Dependent Claim
61 words
The powder of claim 26 wherein said macroparticles are superficially porous macroparticles having an impervious core and a coating of a multiplicity of like monolayers of colloidal microparticles joined to and surrounding the core, the microparticles having a diameter of about 0.005 to about 1.0 micron and comprising from about 0.2 to about 25% of the total volume of the macroparticle.
Claim 33
Dependent Claim
28 words
The powder of claim 29 wherein the microparticles have a diameter of about 0.1 to 0.5 micron and the macroparticles have a diameter of 5 to 50 microns.
Claim 34
Dependent Claim
65 words
The powder of claim 30 wherein the macroparticles are composed principally of silica and wherein the component of the bimodal pore size distribution having the smaller average pore size provides about 40 to about 55% of the total pore volume and the component of the bimodal pore size distribution having the larger average pore size provides about 60 to 45% of the total pore volume.
Claim 35
Dependent Claim
24 words
The powder of claim 31 wherein each component of the bimodal pore size distribution provides about 45 to 55% of the total pore volume.
Claim 36
Dependent Claim
30 words
A powder of claim 26 wherein said macroparticles are totally porous, each being composed of a plurality of microparticles, the microparticles having a diameter of about 0.005 to 1.0 micron.
Claim 37
Dependent Claim
29 words
A powder of claim 32 wherein the macroparticles have a diameter of from about 5 to 50 microns and the microparticles have a diameter of 0.005 to 0.5 micron.
Claim 38
Dependent Claim
65 words
The powder of claim 34 wherein the macroparticles are composed principally of silica and wherein the component of the bimodal pore size distribution having the smaller average pore size provides about 40 to about 55% of the total pore volume and the component of the bimodal pore size distribution having the larger average pore size provides about 60 to 45% of the total pore volume.
Claim 39
Dependent Claim
24 words
The powder of claim 35 wherein each component of the bimodal pore size distribution provides about 45 to 55% of the total pore volume.
Claim 40
Dependent Claim
41 words
The powder of claim 26 wherein the macroparticles are totally porous having a core of a plurality of ultramicroparticles about 1 to 30 nanometers in diameter and a skin of a plurality of microparticles about 0.1 to 1.0 micron in diameter.
Claim 41
Dependent Claim
25 words
The powder of claim 37 wherein the macroparticles are 5 to 50 microns in diameter and the microparticles are 0.1 to 0.5 micron in diameter.
Claim 42
Dependent Claim
56 words
The powder of claim 38 wherein the macroparticles are silica and wherein the component of the bimodal distribution having the smaller average pore size provides about 40 to 55% of the total pore volume and the component of the bimodal distribution having the larger pore size provides about 60 to 45% of the total pore volume.
Claim 43
Dependent Claim
24 words
The powder of claim 39 wherein each component of the bimodal pore size distribution provides about 45 to 55% of the total pore volume.
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) | 1982-07-09 | 1983-01-08 | 1983-07-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-07-09 | 1987-01-08 | 1987-07-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-07-09 | 1991-01-08 | 1991-07-10 | $7700.00 | Window Closed / Lapsed |