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US4250035A Expired / Lapsed US ⏱️ 0.0 years remaining

Radial compression of packed beds

Assignee: Waters Technologies Corp
•
Filing: 1978-11-13
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Granted: 1981-02-10
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Expires: 1998-11-13
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Abstract

Abstract Improved liquid chromatographic apparatus and an improved process for making and utilizing a chromatographic column. By providing means to exert radial pressure on the column packing, the packing efficiency of the column is increased and is more reproducible, and greater uniformity can be achieved in column performance both among packed columns of the same kind and during the useful life of a given packed column.

Inventors

  • 👤 Patrick D. McDonald
  • 👤 Carl W. Rausch

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 05:28
CPC Classifications
B; B01; B01D; B01D53/00; B01D53/02; B01D53/025; B01D15/00; B01D15/08; G; G01; G01N; G01N30/00; G01N30/02; G01N30/50; G01N30/52; G01N30/56; G01N30/60; G01N30/6052; G01N2030/522; G01N2030/562; G01N2030/565; G01N30/6065; G01N30/6086

Claims Analysis

Total Claims: 44
Claim 1
Independent Claim 87 words
In a package of the type defining an elongate chamber holding, and substantially filled by, a porous mass of a stationary-phase, liquid chromatographic, packing material forming means to intimately contact a liquid as it passes through said chamber, and retaining means, at an inlet to and outlet from said chamber for holding said porous mass in said chamber, the improvement wherein said chamber has a flexible wall forming a movable diaphragm means to radially compress said porous mass of packing throughout the cross section of said bed.
Claim 2
Dependent Claim 87 words
In a package of the type defining an elongate chamber holding, and substantially filled by, a porous mass of a stationary-phase, liquid chromatographic, packing material forming means to intimately contact a liquid as it passes through said chamber, and retaining means, at an inlet to and outlet from said chamber for holding said porous mass in said chamber, the improvement wherein said chamber has a flexible wall forming a movable diaphragm means to radially compress said porous mass of packing throughout the cross section of said bed.
Claim 3
Dependent Claim 44 words
A package as defined in claim 1 wherein said diaphragm is in a sufficiently snug radially compressing relationship with said porous mass to deform and reduce the void volume between said diaphragm and said mass without further application of external pressure to said diaphragm.
Claim 4
Dependent Claim 17 words
A package as defined in claim 1 wherein said mass comprises a stationary-phase, particulate liquid-chromatography packing material.
Claim 5
Dependent Claim 56 words
A package as defined in claim 3 wherein said diaphragm comprises an interior wall formed of a distensible organic polymer material said polymer material forming means to press radially against said mass and to conform to the surface of said mass and reduce void volume at the interface of said mass of particles with said diaphragm.
Claim 6
Dependent Claim 16 words
A package as defined in claim 4 wherein said diaphragm wall is formed of poly (tetrafluoroethylene).
Claim 7
Dependent Claim 15 words
A package as defined in claim 4 wherein said diaphragm wall is formed of polyethylene.
Claim 8
Dependent Claim 43 words
A package as defined in claim 1 wherein said diaphragm is so constructed that it forms means to radially compress said mass when an external pressure of about 10 to 1000 psi above the pressure within the chamber is applied to said diaphragm.
Claim 9
Dependent Claim 23 words
A package as defined in claim 4 wherein said diaphragm is formed of a polymer of from 0.001 to 0.100 inches in thickness.
Claim 10
Dependent Claim 60 words
A package as defined in claim 1 wherein said diaphragm is formed of an organic plastic having sufficiently high memory to be able to at least partially recover its surface shape after pressurization is relieved and forming means to assume a newly-shaped interface, on each pressurization of said diaphragm against said packing, minimizing liquid flow between said diaphragm and packing.
Claim 11
Dependent Claim 16 words
A package as defined in claim 8 wherein said diaphragm is formed of polyethylene or polytetrafluoroethylene.
Claim 12
Dependent Claim 17 words
A package as defined in claim 9 wherein said mass comprises a stationary-phase, particulate liquid chromatography material.
Claim 13
Dependent Claim 16 words
A package as defined in claim 8 wherein said mass comprises a stationary-phase, liquid chromatography material.
Claim 14
Dependent Claim 17 words
A package as defined in claim 2 wherein said mass comprises a stationary-phase, particulate liquid chromatography material.
Claim 15
Dependent Claim 16 words
A package as defined in claim 10 wherein said mass comprises a stationary-phase, liquid chromatography material.
Claim 16
Dependent Claim 17 words
A package as defined in claim 1 wherein said diaphragm comprises a thin layer of metallic foil.
Claim 17
Dependent Claim 43 words
A package as defined in claim 15 wherein said diaphragm is so constructed that it forms means to radially compress said mass when an external pressure of about 10 to 1000 psi above the pressure in the chamber, is applied to said diaphragm.
Claim 18
Dependent Claim 16 words
A package as defined in claim 15 wherein said mass comprises a stationary-phase, liquid chromatography material.
Claim 19
Dependent Claim 19 words
A package as defined in claim 8 wherein said package has a diameter of less than about six inches.
Claim 20
Dependent Claim 14 words
A package as defined in claim 3 wherein the chamber is helical in shape.
Claim 21
Dependent Claim 30 words
A package as defined in claim 8 wherein the chamber is continuous and comprises at least two segments arranged at angles of substantially less than 180°, one to the other.
Claim 22
Dependent Claim 106 words
In an apparatus of the type comprising an elongate chamber having an inlet adapted to receive fluid at one end thereof and a port adapted to discharge fluid at the other end thereof, and further comprising a porous mass a stationary phase of liquid chromatographic packing material substantially filling said chamber, said porous mass forming means to intimately contact said fluid as it passes through the chamber, the improvement wherein said chamber wall is a pre-stressed diaphragm forming means to radially compress said porous mass and maintain said mass in a substantially uniform state of compression of packing material throughout said chamber during shipment or use.
Claim 23
Dependent Claim 106 words
In an apparatus of the type comprising an elongate chamber having an inlet adapted to receive fluid at one end thereof and a port adapted to discharge fluid at the other end thereof, and further comprising a porous mass a stationary phase of liquid chromatographic packing material substantially filling said chamber, said porous mass forming means to intimately contact said fluid as it passes through the chamber, the improvement wherein said chamber wall is a pre-stressed diaphragm forming means to radially compress said porous mass and maintain said mass in a substantially uniform state of compression of packing material throughout said chamber during shipment or use.
Claim 24
Dependent Claim 24 words
Apparatus as defined in claim 21 wherein said porous mass is particulate and comprises the immobile phase component of a liquid chromatography packing material.
Claim 25
Dependent Claim 15 words
Apparatus as defined in claim 22 wherein said chamber wall is formed of stainless steel.
Claim 26
Dependent Claim 63 words
Apparatus as defined in claim 22 wherein said chamber is formed of a metallic material and the wall of said chamber comprises, in contact with said particulate material, a coating of a distensible organic material forming means to conform to the surface of said mass of particles and reduce viod volume at the interface of said mass of particles with said chamber wall.
Claim 27
Dependent Claim 14 words
Apparatus as defined in claim 24 wherein said organic material is formed of polytetrafluoroethylene.
Claim 28
Dependent Claim 14 words
Apparatus as defined in claim 24 wherein said organic material is formed of polyethylene.
Claim 29
Dependent Claim 18 words
Apparatus as defined in claim 2 wherein said package has a diameter of less than about six inches.
Claim 30
Dependent Claim 113 words
In a liquid chromatography apparatus of the type comprising a chamber having an inlet adapted to receive liquid at one end thereof and a port adapted to discharge fluid at the other end thereof, and further comprising a porous mass substantially filling said chamber, said mass comprising an immobile phase material forming means to differentially retard the passage of chemical compounds through said chamber the improvement wherein, (a) said apparatus comprises means to radially compress said particulate mass throughout said chamber, to decrease the cross section thereof with substantial uniformity along the length of said chamber and (b) means to take up any decrease in volume of said mass caused by said compression.
Claim 31
Dependent Claim 113 words
In a liquid chromatography apparatus of the type comprising a chamber having an inlet adapted to receive liquid at one end thereof and a port adapted to discharge fluid at the other end thereof, and further comprising a porous mass substantially filling said chamber, said mass comprising an immobile phase material forming means to differentially retard the passage of chemical compounds through said chamber the improvement wherein, (a) said apparatus comprises means to radially compress said particulate mass throughout said chamber, to decrease the cross section thereof with substantial uniformity along the length of said chamber and (b) means to take up any decrease in volume of said mass caused by said compression.
Claim 32
Dependent Claim 51 words
In apparatus as defined in claim 28 wherein, (a) said chamber wall is a diaphragm means which, upon application of an external pressure thereto, forms means to radially compress said mass, and wherein said apparatus comprises (b) means to reduce the cross-sectional area of said chamber, and radially compress said mass.
Claim 33
Dependent Claim 47 words
Apparatus as defined in claim 29 wherein said mass is particulate and said diaphragm wall is formed of a distensible organic material forming means to conform to the surface of said particulate mass and to reduce void volume at the interface of said mass with said diaphragm.
Claim 34
Dependent Claim 14 words
Apparatus as defined in claim 30 wherein said chamber wall is formed of polyethylene.
Claim 35
Dependent Claim 14 words
Apparatus as defined in claim 30 wherein said chamber wall is formed of polytetrafluoroethylene.
Claim 36
Dependent Claim 18 words
Apparatus as defined in claim 28 wherein said chamber has a diameter of less than about six inches.
Claim 37
Dependent Claim 18 words
Apparatus as defined in claim 30 wherein said chamber has a diameter of less than about six inches.
Claim 38
Dependent Claim 27 words
Apparatus as defined in claim 28 wherein, at said inlet port, there is means to distribute liquid entering said chamber evenly across the top of said chamber.
Claim 39
Dependent Claim 27 words
Apparatus as defined in claim 30 wherein at said inlet port, there is means to distribute liquid entering said chamber evenly across the top of said chamber.
Claim 40
Dependent Claim 15 words
A package as defined in claim 1 wherein said diaphragm means if formed of polyethylene.
Claim 41
Dependent Claim 19 words
A package as defined in claim 3 wherein said package has a diameter of less than about six inches.
Claim 42
Dependent Claim 19 words
A package as defined in claim 13 wherein said package has a diameter of less than about six inches.
Claim 43
Dependent Claim 28 words
Apparatus as defined in claim 3 wherein said movable diaphragm is a means to improve bridging stability of said particles and to increase stability of the particulate mass.
Claim 44
Dependent Claim 26 words
Apparatus as defined in claim 34 wherein said diaphragm forms means to improve bridging stability of said particles and to increase the stability of said mass.

References Cited (Backward Citations)

US3017996A Cited
US3180825A Cited
US3266628A Cited
US3349920A Cited
US3487938A Cited
US3791522A Cited
US3966609A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-02-10 1984-08-11 1985-02-10 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-02-10 1988-08-11 1989-02-10 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-02-10 1992-08-11 1993-02-10 $7700.00 Window Closed / Lapsed

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