DEVICE, APPARATUS AND METHOD FOR PERFORMING SEPARATIONS

Abstract

Embodiment of the present invention feature a device having a body, a separation media and a frit element. The exterior surface of the body has a first attachment means positioned radially about at least one of the media chamber and the frit section to form a compact assembly.

Claims

1-33. (canceled)

34. A separation device comprising: a body having a media chamber configured to hold a media, a connection section configured to place the media chamber in fluid communication with a source of fluid, and at least one frit section in fluid communication with the media chamber; a frit element held in the at least one frit section; and a separation media disposed within the media chamber, wherein the separation media is held within the media chamber by the frit element.

35. The separation device of claim 34, wherein the at least one frit section is disposed at a first end of the media chamber.

36. The separation device of claim 35, further comprising a second frit element disposed at a second end of the media chamber.

37. The separation device of claim 34, further comprising a rod assembly and a compression fitting, the compression fitting configured to couple the rod assembly to the body.

38. The separation device of claim 37, wherein the rod assembly includes a tube section and a compression plate section, wherein the compression fitting engages the compression plate to couple the rod assembly to the body.

39. The separation device of claim 37, wherein the compression fitting has an interior surface defining a tube channel, the tube channel configured to receive the tube section of the rod assembly therethrough.

40. The separation device of claim 37, wherein an exterior surface of the compression fitting comprises turning surfaces.

41. The separation device of claim 40, wherein the turning surfaces are recessed.

42. The separation device of claim 40, further comprising a tube compression assembly.

43. The separation device of claim 42, wherein the tube compression assembly comprises a ferrule and a ferrule fitting.

44. The separation device of claim 43, wherein the ferrule fitting is received on the tube section extending from the compression fitting.

45. The separation device of claim 42, wherein the tube compression assembly conceals the turning surfaces.

46. The separation device of claim 34, further comprising a wiper, wherein the media chamber further comprises a wiper recess configured to receive the wiper, the wiper comprising a resilient ring.

47. The separation device of claim 34, further comprising a compression element, the compression element compelled into the separation media disposed within the media chamber to occupy a volume in the range of about 0.1% to about 5% of a total volume occupied by uncompressed particles of the separation media.

48. The separation device of claim 47, wherein the compression element is compelled into the particles to occupy a volume of about 2% of the total volume occupied by uncompressed particles of the separation media.

49. The separation device of claim 47, wherein the compression element is compelled into the particles to form an interstitial volume fraction in the range of about 0.38 to about 0.35.

50. The separation device of claim 49, wherein the interstitial volume fraction is in the range of about 0.365 to about 0.375.

51. The separation device of claim 49, wherein the compression element compelled into the particles to effect a reduction of an at-rest interstitial volume fraction in the range of about 5% to about 15%.

52. The separation device of claim 51, wherein the reduction is in the range of about 8% to about 12%.

53. A method of separating compounds in a solution from each other or undesired components of the solution, comprising: providing a separation device having a body, a separation media, and a frit element; the body having a media chamber configured to hold a media, a connection section configured to place the media chamber in fluid communication with a source of fluid, and at least one frit section in fluid communication with the media chamber, the frit element held in the at least one frit section, and the separation media disposed within the media chamber for effecting separations of compounds in solutions flowing therethrough; and flowing a fluid through the device to separate one or more compounds.

54. The separation device of claim 53, further comprising a rod assembly and a compression fitting, the compression fitting configured to couple the rod assembly to the body.

55. The separation device of claim 55, wherein an exterior surface of the compression fitting comprises turning surfaces.

56. The separation device of claim 55, further comprising a tube compression assembly.

57. The separation device of claim 56, wherein the tube compression assembly conceals the turning surfaces.

58. A method of making a separation device comprising: providing a body, a separation media, at least one frit element, and at least one compression element; the body having a media chamber configured to hold a media, a connection section configured to place the media chamber in fluid communication with a source of fluid, and at least one frit section in fluid communication with the media chamber; placing the at least one frit element in the at least one frit section for retaining the separation media; placing the separation media within the media chamber for effecting separations of compounds in solutions flowing therethrough; and placing the compression element in the body to compress the separation media to form a stable separation media.

59. The method of claim 58, wherein the compression element comprises a second frit element.

60. The method of claim 58, wherein the compression element is compelled into the separation media to occupy a volume in the range of about 0.1% to about 5% of a total volume occupied by uncompressed particles of the separation media.

61. The method of claim 58, wherein the compression element is compelled into the separation media to occupy a volume of about 2% of the total volume occupied by uncompressed particles of the separation media.

62. The method of claim 58, wherein the compression element is compelled into the particles to form an interstitial volume fraction in the range of about 0.38 to about 0.35.

63. The separation device of claim 58, wherein the interstitial volume fraction is in the range of about 0.365 to about 0.375.

64. The separation device of claim 58, wherein the compression element is compelled into the particles to elect a reduction of an at-rest interstitial volume fraction in the range of about 5% to about 15%.

65. The separation device of claim 64, wherein the reduction is in the range of about 8% to about 12%.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0029] FIG. 1 depicts a cross-sectional view of a device embodying features of the present invention;

[0030] FIG. 2 depicts a cross-sectional view of a device embodying features of the present invention;

[0031] FIG. 3a depicts an exploded view of the device in FIG. 2;

[0032] FIG. 3b depicts an exploded view of the device in FIG. 1 with a wiper and projecting frit;

[0033] FIG. 3c depicts an detailed view of the device in FIG. 3b;

[0034] FIG. 4 depicts an exploded view of the device of FIG. 1; and,

[0035] FIG. 5 depicts a view of the device of FIG. 1 in partial cross-section with a further column, conduit, or instrument.

DETAILED DESCRIPTION OF THE INVENTION

[0036] Embodiments of the present invention will be described with respect to a column used to protect a analytical column, commonly referred to as a guard column with the understanding that such column can be used for performing chromatography without an analytical column. Indeed, such column can be used directly with analytical, diagnostic instruments, detectors and the like. The description that follows describes a preferred embodiment of the device, methods and apparatus of the present invention. Those skilled in the art will readily recognize that the present invention can be modified and altered to address specific needs without departing from the present teaching.

[0037] Turning now to FIG. 1, a device, generally designated by the numeral 11 is depicted in cross-section. The device is for separating one or more compounds of interest from each other or from undesired compounds or particulates. The device 11 has the following major components: a body 13, a separation media 15 and frit element 17a and 17b.

[0038] As best seen in FIG. 2, the body 13 has an interior body surface 21, an exterior body surface 23, a first body opening 25 at a first body end 27 and a second body opening 31 at a second body end 33. The first body opening 25 and the second body opening 31 define a boundary between the interior body surface 21 and the exterior body surface 23. The interior body surface 21 has at least one wall 35 creating a passage 37 in the body 13. The body 13, and all components of the device 11, unless otherwise indicated, is made of a substantially rigid material such as plastic and metal. A preferred metal is titanium, brass, and stainless steel. The body 13, for extreme high pressure applications is approximately 2.1 millimeters in diameter and 5 millimeters in length. The passage 37 is about 0.050 to 0.0005 inches in diameter at its narrowest.

[0039] The passage 37 has at least one frit section 39a and a media chamber 39b proximal to the first opening 25. And, the passage 37 has a manifold section 39c in fluid communication with the frit section 39a and a connection section 39d more proximal to the second opening 31.

[0040] The frit section 39a is for holding first frit element 17a. The media chamber 39b is for holding the separation media 15, which comprises a porous monolith, packed bed of particles, beads or other solid forms or fibers [not shown], known in the art. The separation media 15 is held within the media chamber 39b for effecting separations of compounds in solutions flowing therethrough. For guard column applications at extreme pressures, chamber 39a has a volume of 17 to 19 cubic mm. When packed with a bed of particles, the preferred particles are packed at similar extreme pressures. A preferred particle bed has particles having a mean diameter of 1.7 microns.

[0041] A first frit 17a is held in the frit section 39a for holding the packed bed of particles in the media chamber 39b. First frit 17a is porous filter disc made of a material such as titanium, plastic or stainless steel in a manner known in the art.

[0042] The manifold section 39c is for receiving from or discharging to the frit section 39a. The connection section 39d is constructed and arranged as a union means for receiving a fitting [not shown] to place the manifold section in fluid communication with a further conduit, instrument, or detector. Those skilled in the art will readily recognize that such union means can be formed as part of the exterior surface 23.

[0043] A second frit element comprising a second frit 17b and a frit sealing ring 43a is received at or about the first body end 27 in a second frit section of the passage [not shown] in the manner of the first frit 17a, or, as shown in FIGS. 2 and 3a, outside the first body 13 end surface 27, or a combination of a second frit section of the passage and projecting outside the passage surface 27 as shown in FIGS. 3b and 3c to be discussed in greater detail below.

[0044] Returning now to FIGS. 2 ands 3a, second frit 17b, like first frit 17a, is a porous filter disc made of a material such as titanium, plastic or stainless steel. Second frit 17b is held in frit sealing ring opening 63 of frit sealing ring 43a.

[0045] Exterior surface 23 has a rim 41 extending around the first body opening 25. Rim 41 has a planar rim surface for receiving frit sealing ring 43a. Turning now to FIG. 2a, frit sealing ring 43a has a flat surface that mates with the flat surface of rim 41. At least one of the flat surface of rim 41 and the flat surface of frit sealing ring 43a has ridge. As depicted, in FIG. 2, the rim surface 41 has a ridge 45 surrounding the first opening 25. The frit sealing ring 43a receives the ridge 45 against the ring flat surface. The ridge 45 seals the frit sealing ring 43a upon compression against said rim 41.

[0046] Turning now to FIGS. 3b and 3c, such figures depict an embodiment in which the second frit 17b, is placed into the chamber 39b which would be occupied by particles of other separation media. Preferably, a compression element, such as a sleeve [not shown], frit sealing ring 43a, a wiper element 161, to be discussed in greater detail later, or, as described herein, second frit 17b is compelled into the media held in chamber 39b to occupy approximately 0.1 to 5% of the total area occupied by particles not under pressure. More preferably, the compression element such as second frit 17b is forced into the at-rest particles to occupy approximately 2% of the volume. Compression presses the particles to form an interstitial volume fraction of approximately 0.38 to 0.35. And, preferably, compression presses the particles to form an interstitial volume fraction of approximately 0.365 to 0.375. These interstitial volume fractions represent a reduction of at-rest interstitial volume fraction of approximately 5 to 15%, and preferably of about 8 to 12%. The compressed particles have an optimal bed density to promote stability of the bed and avoid the formation of voids.

[0047] Thus, frit sealing ring 43a and second frit 17b are sized to allow second frit 17b to project outside the frit seal ring opening 63. The amount of projection can be changed by changing the thickness of the second frit 17b or the frit sealing ring 43a. The portion of the second frit 17b projecting outside the opening 63, as best seen in FIG. 3c, occupies a space of 2% of the volume of the particles that would occupy chamber 39b. For a chamber of approximately 18 cubic milimeters in volume and 2.1 mm in diameter, the amount of projection is approximately 0.051 to 0.330 mm.

[0048] Again referring to FIGS. 3b and 3c, a wiper 161 is received in a recess 163 in the passage 37 forming chamber 39b. The wiper 161 is a ring of resilient material such as plastic to provide radial compression of the packed material forming the bed and to facilitate the compression of the bed upon the pressing the second frit 17b into the chamber 39b. A preferred plastic is a fluoropolymer sold under the mark TEFLON (Dupont). The second frit 17b is normally fitted to the first body 13 after the particles are loaded. The remainder of the structures of FIGS. 3b and 3c are as described with respect to FIG. 3a.

[0049] Turning now to FIG. 2, the body 13 is fitted to conduits, instruments and detectors by first union means comprising cooperating fittings, conduits or structures associated with instruments and detectors. First union means, as depicted, comprises the exterior body surface 23 and attachment surfaces 51 positioned radially about at least one of the media chamber 39b and the frit section 39a. Attachment surfaces comprise pins, cams and locking fittings known in the art, and as illustrated, a threaded section of the body 13.

[0050] Turning now to FIGS. 2 and 3, one first union means comprises a rod assembly 55 and compression fitting 57. The rod assembly is preferably made of rigid plastic, and metals such as brass, titanium and stainless steel. The rod assembly 55 has a tube section 59 and a compression plate section 61. The tube section 59 is in fluid communication via port 67 with the frit center opening 63 of second frit 17b.

[0051] The compression plate section 61 has a first plate surface 65a for pressing in sealing relationship against the corresponding planar surface of frit sealing ring 43a. Preferably, at least one of the plate surface 65a and the planar surface of the frit sealing ring 43a has a ridge for effecting a seal. As depicted in FIG. 3a, first plate surface 65a has a ridge 71 extending around the port 67. Upon compression the ridge 71 presses into and seals the frit sealing ring 43a against the plate section 61. The compression plate section 61 has a second plate surface 65b for receiving a compression surface 73 of compression fitting 57.

[0052] Compression fitting 57 has a fitting interior surface 81 and a fitting exterior surface 83, a first fitting opening 85 and a second fitting opening 87. As best seen in FIG. 2, the fitting interior surface 81 defines a tube channel 91 between the first fitting opening 85 and the second fitting opening 87.

[0053] Tube channel 91 has a narrow section 93a, an expanded section 93b and compression surface 73. The compression surface 73 is interposed between the narrow section 93a and the expanded section 93b. The expanded section 93b and the attachment surfaces 51 of the body 13 have cooperating threads to allow the compression surface 73 to compress the compression plate section 61 and frit sealing ring 43a on the rim 41 of the body 13. The tube section 59 is received in and extends from the tube channel 91.

[0054] Rotation of the compression fitting 57 with respect to the body 13 in one direction compresses the compression plate section 61, the frit sealing ring 43a and the rim 41 of the body 13 in sealing engagement. Rotation of the compression fitting 57 in the opposite direction causes decompression and loss of the sealing engagement. Preferably, at least one of, and even more preferably, both the body 13 and the compression fitting 57 have exterior surfaces that facilitate rotation such as knurled surfaces, wrench receiving notches and other turning surfaces. Such turning surfaces facilitate manufacture of the device 11.

[0055] However, it is desirable to maintain the sealing relationship of the compression plate section 61, the frit sealing ring 43a and the rim 41 of the body 13 after the device is packed with separation media 15. Disruption of the sealing relationship disturbs the separation media 15 making such media less effective. It is desirable in this regard to not allow or discourage rotation of the compression fitting 57 and the body 13 after the device 11 is made. As best seen in FIGS. 3 and 4, compression fitting 57 has an exterior surface 83 having turning surfaces 95 in the form of notches for receiving a wrench or similar tool [not shown]. The turning surfaces 95 are recessed and are proximal to the second opening 87.

[0056] The turning surfaces 95 are preferably concealed by a tube compression assembly 101. The tube compression assembly 101 is received on the tube section 59 of the rod assembly 55. As best seen in FIG. 5, the tube compression assembly 101 facilitates placing the tube section 59 in fluid communication with a fitting, detector, column or conduit, generally designated by the numeral 103. The tube compression assembly 101 is made of rigid materials, such as plastic and metals.

[0057] Tube compression assembly 101 comprises a ferrule 103 and a ferrule fitting 105. The ferrule fitting 105 is rotatably slidably received on the tube section 59 extending from the compression fitting 57 to allow movement. The ferrule fitting 105 moves axially along the tube section 59 as the ferrule fitting 105 is tightened against the ferrule 103. As best seen in FIG. 5, the fitting, detector, column or conduit, generally designated by the numeral 133, has ferrule fitting receiving surfaces 109a which cooperate with threaded surfaces 109b on the ferrule fitting 105, to allow the ferrule fitting 105 to be tightened. Ferrule 103 is slidably received on tube section 59 to allow ferrule 103 to compress against a ferrule receiving surface 107 fitting, detector, column or conduit, generally designated by the numeral 133. As the ferrule fitting 105 is tightened, the ferrule 103 is sealed under compression against the tube section 59 and the ferrule receiving surface 107.

[0058] Turning now to FIGS. 1 and 4, when the device 11 is not fitted to a fitting, detector, column or conduit, generally designated by the numeral 133, an O ring 111 is fitted to the tube section 59 to retain the ferrule fitting 101 and the ferrule 103 in place. In use, the O ring 111 is removed.

[0059] The ferrule fitting 105 has a ferrule fitting interior surface 113, a ferrule fitting exterior surface 115, a ferrule fitting first opening 117 and a ferrule fitting second opening 119. The ferrule fitting interior surface 113 defines a ferrule fitting tube channel 121, as best seen in FIG. 1, between the ferrule fitting first opening 117 and the ferrule fitting second opening 119. The ferrule fitting tube channel 121 has a ferrule fitting narrow section 123a and a ferrule fitting expanded section 123b. The ferrule fitting narrow section 123a receives the tube section 59.

[0060] As best seen in FIG. 1, the ferrule fitting expanded section 123b receives and conceals the compression fitting turning surfaces 95. Thus, the user is discouraged from separating the body 13 from the compression fitting 57.

[0061] The ferrule fitting 105 has a male end 125 at the ferrule fitting second opening 119. The ferrule fitting 105 has a ferrule fitting rim 127 for receiving the ferrule 103.

[0062] Turning now to FIG. 5, the second body end 33, the body 13 has second end attachment means for affixing, in fluid communication to an analytical column, fitting, detector or a conduit, generally designated by the numeral 131. Those skilled in the art will recognize that the device 11 may accommodate flow in either direction and the use of the terms analytical column, fitting, detector or a conduit is intended to encompass the use of the device 11 with a flow in either direction.

[0063] Turning again to FIG. 1, second end attachment means comprise connection section 39d of passage 37. Connection section 39d has threads 141 for receiving cooperating threads of a column, or a detector or conduit, or a further fitting, generally designated by the numeral 131. Such cooperating threads are common in ferrule compression fittings and the like. For guard column applications, the total volume, from the narrows of passage 21 at end 31 to the end of tube 59 is approximately 20 to 22 microliters of which 9 to 10 microliters are occupied by a particulate bed 15 for a total device volume of approximately 10 to 12 microliters.

[0064] A further embodiment of the present invention comprises a method of separating compounds in a solution from each other or undesired components of the solution. The method comprises the step of providing a device 11 having a body 13, a separation media 15, and at least one frit element 17a or 17b as previously described. The method comprises the further step of flowing solutions through the device 11 to separate compounds from each other or from particulates.

[0065] Referring now to FIG. 5, a further embodiment of the present invention comprises an apparatus, generally designated by the numeral 151. The apparatus 151 comprises a device 11 as previously described and one or more instruments selected from the group comprising a high performance chromatography pump, detector and column, generally designated by the numerals 103 or 131.

[0066] Thus, embodiments of the present invention have been describe with respect to preferred configurations and steps with the understanding that the invention can be modified and altered without departing from the teaching herein. Thus, the present invention should not be limited to the precise details herein but should encompass the subject matter of the claims that follow and their equivalents.