CN101495206A - Graded external prefilter element for continuous-flow systems - Google Patents
Graded external prefilter element for continuous-flow systems Download PDFInfo
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- CN101495206A CN101495206A CNA2007800286952A CN200780028695A CN101495206A CN 101495206 A CN101495206 A CN 101495206A CN A2007800286952 A CNA2007800286952 A CN A2007800286952A CN 200780028695 A CN200780028695 A CN 200780028695A CN 101495206 A CN101495206 A CN 101495206A
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- prefilter
- filter element
- gradient
- gradient filter
- multihole device
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Abstract
A prefilter element for continuous flow systems as illustrated by a high-performance liquid chromatography cartridge or column is constructed with a gradient filter that has a gradient in average pore size over its thickness, the pore size decreasing in the direction of flow. This prefilter element is retained in a housing separate from any functional components of the continuous-flow system other than the prefilter element itself, the prefilter element being separable from the other functional components to allow the prefilter to be replaced without disturbing any other functional components.
Description
The cross reference of related application
The application requires the priority of No. the 60/820th, 245, U.S. Provisional Patent Application that on July 25th, 2006 was submitted to, and this paper is to be incorporated into this referring to mode with its full content.
Background of the present invention
1. technical field
The present invention relates to the system of continuous-flow, comprise column chromatography, relate in particular to design and be used for the chromatographic column of the various compositions of sample separation mixture, mixture also comprises solid or is tending towards forming sediment, these sediments reside in the splitter or pre-filter media in, or otherwise disturb solute freely to flow through post, or cause the post back pressure to rise at the limited number of time after separating.
Background technology
The analysis that the system that comprises the high efficiency liquid chromatography (HPLC) and the continuous-flow of other form chromatogram is widely used in various chemical species mixtures with preparation with separating.For instance, typical HPLC post can be used multiple times, in the automation chromatographic system.Reuse single post and allow the direct comparison of sample, not by cleaning separating medium between twice injection or by being replaced by the error of introducing with the fresh post of sample ingredient with the post of crossing to sample.Yet, in any single separates, solid debris, no matter be exist in the sample or sampling or analytical equipment produce, these chips are all carried secretly away by sample or carrier fluid.For example, in the whole blood sample of dissolving, chip can be made up of cell wall fragments, insoluble protein and the soluble protein of agglomeration or precipitation.If the hermetically-sealed construction of valve and pump is broken particulate matter is discharged in the carrier fluid, or when fragment dropped out from specimen tube or barrier film when puncturing specimen tube or barrier film with the sampling pricker, then chip also can originate from chromatograph itself.The chip of carrying secretly usually enters post and accumulates in the post, hinders fluid and freely flows through post, and back pressure rises in the post thereby cause.
The resin that is used as separating medium in the HPLC post is fixing on the throne with frit usually, and this frit also is used as the filter that filters solid debris.Yet frit itself can be stopped up by chip, and special interface between frit and resin can cause the post back pressure to raise equally.Obstruction in the interface region also can be blocked the passing through of material of very little protein, thus, when these protein belong to want to discern and/or quantitative component in the time, with regard to carrying out that thus can interference separation.
Debris accumulation is the greatest problem of continuous-flow system with the formation of the back pressure that is produced.In these systems, in the sample injected system before, some chip can filtration or centrifugation by sample come off-line to remove.Yet filtration and centrifugation are time-consuming step, and can increase the mistake that the operator brings.Also can not utilize and implement on-line filtration with guard column and prefilter that resin directly contacts.An example that is designed for the prefilter of whole blood sample is the stainless steel prefilter of sintering, its hole size is 0.5 micron, thickness is 1.9mm, can be from (the Bio-Rad Laboratories of joint-stock company of biological SSRL in California, USA Heracles city (Hercules), Inc.) buy, catalogue is No. 2700270.Regrettably, by the same token, prefilter itself is easy to stop up and form back pressure.When adopting guard column, the back pressure of rising causes will changing guard column according to applicable cases after 50 to 200 injections usually.When adopting prefilter as when separating the protection with resin, resin often can be kept the long period between twice replacing, but before needs are changed, and resin is usually durable to be no more than 500 injections.
The United States Patent (USP) of authorizing Dewaele the 5th that November 16 in 1999 submitted to, 985, No. 140, be entitled as " utilizing graded filter medium to reduce the formation (Reduction in Back PressureBuildup in Chromatography by Use of Graded Filter Media) of back pressure in the chromatography ", described one and solved the disclosed method early that back pressure forms problem.Yet, patent the 5th, 985, the stage filter (graded filter) in No. 140 directly contacts with the resin in the shared pipe, and changes filter and need dismantle pitch tube, often changes resin and filter.
Summary of the invention
Have found that when graded filter medium is configured to the outer protector of system, rather than during with being connected such as other such functional parts of separation resin of system, graded filter medium can be protected chromatographic column, analyze any parts of box or continuous-flow system.So-called " functional parts " is meant execution except simply the position of liquid from system being transferred to the parts of the function another position.As outer protector; when back pressure begins to rise; graded filter medium can be removed and change; can not disturb resin or other parts of continuous-flow system; and; utilize the mechanical fasteners method this graded filter medium can be fixed firmly on its shell, the danger that does not damage resin or cause resin particle to penetrate filter medium and mix with it.Therefore filter medium itself will not need to change so continually, and when needs are changed, can change more easily.In addition, during by the short non-graded filter medium supporting of the length that is used as structure support, then can realize more benefits at upstream extremity, downstream or upstream and downstream two ends when graded filter medium.In some cases, when graded filter medium is divided into two length of being separated by the non-graded filter medium or thickness, also can realize more benefit.No matter in any situation, also can provide additional filtration when the non-graded filter medium exists except supporting functions, filtration that is provided by graded filter medium is provided for it.In any of these configuration; placing graded filter medium outside the system or in the shell outside the parts that the filter design is used for protecting; can from the sample that flows through system, remove any chip; and compare to the filter of prior art, also can on much more sample, reuse continuously and need not to insert cleaning.
Description of drawings
Fig. 1 is the exploded perspective view as the prefilter of an example of embodiment of the present invention.
Fig. 2 is the exploded perspective view as second prefilter of another example of embodiment of the present invention.
Fig. 3 is the exploded perspective view as the 3rd prefilter that also has another example of embodiment of the present invention.
The specific embodiment
As mentioned above, gradient in the prefilter of the present invention is filtered (gradient filter) medium and is arranged like this: make sample fluid and any other liquid enter medium by the side with big void space, then, pass medium and leave medium by a side with less void space.When having two layers of gradient media, two layer medium can be arranged to allow liquid enter by the side with big void space, and go out by the effluent with less void space, or alternately, two gradient layers can be arranged to make its gradient to arrange symmetrically in opposite direction, so that prefilter can be installed on arbitrary orientation with respect to flow direction.Yet in all scenario of two or more gradient media layers was arranged, the upstream gradient dielectric layer had the hole dimension that streamwise reduces.Same in some such embodiment, prefilter contains the element of one or more porous, except their porous is evenly basically, that is, does not have outside the gradient, and they are similar to gradient filter medium.The multihole device of these non-gradients is with the structure support of doing gradient media, and can be present in gradient media upstream side, downstream or upstream and downstream side both, or between two gradient media layers.Non-gradient porous element also can be present on all three positions.
Although the degree and the spatial distribution rate of the pore size gradation in the gradient media within the scope of the present invention can change, just as hole dimension itself changes, but the hole dimension of any non-gradient porous element that the hole dimension in the gradient media generally is equal to or greater than gradient media to be contacted.In a preferred embodiment, the ratio of the average pore diameter in the average pore diameter at the minimum diameter end place of each gradient media layers and the non-gradient component is from about 1: 1 to about 20: 1, more preferably from about 1: 1 to about 12: 1, best from about 1: 1 to about 10: 1.When gradient layer or each gradient layer when two or more layers exist have a kind of like this gradual change of hole dimension, it is reduced to the enough narrow diameter that retains is 10 microns particle, preferably retain diameter and be 5 microns particle, retaining diameter best is the final size of 1 to 3 micron particle, but also can use the gradient layer that can retain 0.5 micron dimension particle.No matter explain whether clearly, refer to the average pore diameter on given thickness or zone when referring to bore dia here, and to an element be described as having uniformly or basically uniformly hole dimension be meant that being distributed on distance, volume or the area of hole dimension is consistent basically or uniformly, thus, described bore dia is an average pore diameter.Therefore, the gradient of bore dia or void space is meant the gradient of average bore dia or average void space.
The factor that other of the classification of prefilter or non-graded elements is relevant is the thickness and the permeability factor of element, and the two can change as hole dimension.When having one or more non-graded elements, their thickness can be than the thickness big (size that refers to the full-page proof flow direction) of the gradient layer that they contacted.Preferable thickness range is extremely about 6.0mm of about 0.5mm, and best thickness range is that about 1.0mm is to about 3.0mm.Each gradient layer has the preferred thickness range from about 0.1mm to about 1.0mm, preferably from about 0.2mm to about 0.6mm, best from about 0.3mm to about 0.6mm.The ratio of each non-graded porous layer and the thickness of each gradient layer is preferably from about 1: 1 to 30: 1, more preferably from about 1: 1 to about 15: 1, best from about 1: 1 to about 10: 1.Permeability factor k defines according to Darcy's law:
Wherein, Δ P is pressure drop, and L is a filter thickness, and μ is a fluid viscosity, and V is a superficial velocity.The permeability factor of each gradient layer is preferably about 4 * 10
-13To about 1 * 10
-10In the scope, more preferably about 4 * 10
-13To 1 * 10
-11In the scope, best about 4 * 10
-13To about 4 * 10
-12In the scope.The preferred range of the permeability factor of non-graded multihole device is about 1 * 10
-12To about 1 * 10
-6, more preferably be about 1 * 10
-10To about 1 * 10
-8
Gradual change in each gradient layer can be step or continuous, can change widely to the variation than aperture one side than macropore one side.The difference of hole dimension (that is, between maximal pore size and the smallest cell dimension poor) therefore can about 1 micron to about 50 micrometer ranges, or preferably from about 2 microns to about 20 microns.When gradual change is step, gradient layer will contain two or more gradually changeables, they preferably be three to six, and the hole dimension scope on the thick side (upstream side) of layer (the thickest part of layer) can be from about 2 microns to about 50 microns, preferably from about 2 microns to 6 microns.
Each gradient filter element is made of the nonwoven stainless steel fibre of sintering.Special stainless steel is not a key point of the present invention, can adopt various stainless steel alloy yet.Austenitic stainless steel, promptly its main alloying element is chromium and nickel stainless steel is first-selected.Particularly preferred stainless steel is the 316L stainless steel, and this stainless composition is about carbon 0.03%, manganese 2.00%, silicon 1.00%, chromium 16.0-18.0%, nickel 10.0-14.0%, phosphorus 0.45%, sulphur 0.03% and molybdenum 2.0-3.0% (all percentages by weight).Other useful stainless steel example can be 304,304H, 304L, 304LN, 316,316F, 316H, 316LN, 316N, 317,317L, 321,321H, 347,347H, 348,348H and 384.
The preferable filter medium that can be used as gradient component at present is
Filter medium, especially
3AL3, it is the product of Belgian NV Bekaert SA, can buy from the Bekaert company in the Atlanta city of the Georgia State of the BekaertFibre Techonolies in Europe, Belgian Zwevegem and the U.S..This medium is made by the 316L stainless steel fibre, is compressed into non-woven constructions randomly and carries out sintering, and with the sheet material supply, typical lateral dimensions is 1180mm * 1500mm, and thickness is 0.4mm.These specialities have 3 microns absolute filtration rated value, 12, are 9L/dm when the bubble point pressure of 300Pa (ASTM E128061 is equivalent to ISO 4003), 200Pa
2The average air permeability of/min (NFA95-352 is equivalent to ISO 4022), 4.80 * 10
-13Permeability factor k, 975g/m
2Weight, 65% porosity and 6.40mg/cm
2The dirt hold facility (according to repeatedly by (Multipass) method ISO 4572 with 8 " initial pressure reduction).Also can adopt other medium of similar characteristics and make with similar material.
In some prefilter according to the present invention, gradient filter medium is the form of two distinct layers that make up with the non-graded porous layer in the prefilter of sandwich type, prefilter is arranged in the upstream of the box or the post of the continuous-flow system that is used for HPLC or other form.In this sandwich-type prefilter, gradient layer is layered on the non-graded multihole device, that is, the plane surface of each gradient layer contacts fully with the plane surface of non-graded multihole device.Sandwich-type prefilter in this specification is shown among Fig. 1 and 2.Prefilter 11 among Fig. 1 comprises basically the center multihole device 12 in the support ring 13 of being fixed on of even hole dimension or equally distributed hole dimension (that is, non-graded), and support ring 13 can be
Or any other can form the inert material of fluid sealing, adds a gradient filter layer 14 and second a gradient filter layer 15 that is positioned on the non-graded elements downstream that is positioned on the non-graded elements upstream side. Flow distribution dish 16,17 is included in the top and the bottom outer surface place of close prefilter sandwich in the filter housing.The flow direction that flows through prefilter is shown in arrow 21,22.Non-graded layer 12 among this embodiment is for the sintered stainless steel element of above-mentioned joint-stock company of biological SSRL product, has 0.5 micron hole dimension and the thickness of 1.9mm.Alternative non-graded multihole device is 2.0 microns the hole dimension and the element of same thickness.Prefilter 25 is identical with prefilter among Fig. 1 among Fig. 2, and difference is to have cancelled flow distribution dish 16,17.
Fig. 3 illustrates the sandwich-type prefilter 31 of different structure, wherein, comprises two gradient filter elements 32,33 and is placed to and draw close each other so that contact fully.Non-graded multihole device 34,35 is positioned at the upstream and downstream side of combination gradient component respectively.
In each embodiment shown in Fig. 1,2 and 3, upstream gradient element 14,32 (that is, the element at the most close each figure top) has porosity gradient, its along direction shown in the arrow from slightly up to thin (hole dimension diminishes).The porosity gradient that downstream gradient element 15,33 can have along equidirectional, so that the hole dimension that two elements have streamwise reduces, perhaps, porosity gradient in opposite direction, so that whole sandwich can be inserted in the flow path of the liquid along either direction, need not to instruct the user only to use this structure along a direction.
In appended claims, term " " refers to " one or more ".Term " comprises " and its variant, when carrying out the description of step or element, be mean add other step or element be can be for choosing inexclusive.All patents of being quoted in this specification, patent application and other publication reference material are all to be contained in this in full referring to mode.Here draw any reference material and this specification any difference between clearly introducing and all desire to be decided to be the narration that is beneficial to this specification.Definition and the same speech or any difference between the clear in this manual definition that provides of phrase of speech that the industry is understood or phrase are provided for this.
The narration purpose that more than provides is to describe.Falling into other variation, the modification within the scope of the invention and substitute will be conspicuous for those skilled in the art all.
Claims (13)
1. prefilter that is used for continuous-flow system, described prefilter has the prescribed direction that liquid flows through, and comprise the gradient filter element that the nonwoven stainless steel fibre by sintering forms, described gradient filter element has the classification interstitial channels of the size gradient that formation reduces along described flow direction, the shell that described gradient filter element places any functional parts except described prefilter with described continuous-flow system to separate, described prefilter can separate with described other functional parts with permission changes described gradient filter element, and does not disturb described other functional parts.
2. prefilter as claimed in claim 1 is characterized in that, described gradient filter element is enclosed by multihole device circle at the upstream side with respect to described flow direction, and described multihole device contains the uniform basically hole of average pore diameter.
3. prefilter as claimed in claim 1 is characterized in that, described gradient filter element is enclosed by multihole device circle in the downstream with respect to described flow direction, and described multihole device contains the uniform basically hole of average pore diameter.
4. prefilter as claimed in claim 1 is characterized in that, described gradient filter element is all enclosed by multihole device circle in the upstream and downstream side with respect to described flow direction, and described multihole device contains the uniform basically hole of average pore diameter.
5. prefilter as claimed in claim 1, it is characterized in that, described gradient filter element is defined as the first gradient filter element, described prefilter also comprises the second gradient filter element that the nonwoven stainless steel fibre by sintering forms, the described second gradient filter element has the classification interstitial channels that forms size gradient, the described first and second gradient filter elements place in the described shell, and, described prefilter also comprises multihole device, this multihole device contains the uniform basically hole of average pore diameter, and described porous filter element places between described first and second filter cells along described flow direction.
6. prefilter as claimed in claim 5 is characterized in that, the described gradient in the described second gradient filter element increases along described flow direction size.
7. prefilter as claimed in claim 5 is characterized in that, the described gradient in the described second gradient filter element reduces along described flow direction size.
8. prefilter as claimed in claim 1 is characterized in that, the permeability factor of described gradient filter element is about 4 * 10
-13To about 1 * 10
-10
9. as claim 2 and 3 described prefilters, it is characterized in that the permeability factor of described gradient filter element is about 4 * 10
-13To about 1 * 10
-10, the permeability factor of described multihole device is about 1 * 10
-12To about 1 * 10
-6
10. as claim 2 and 3 described prefilters, it is characterized in that the permeability factor of described gradient filter element is about 4 * 10
-13To about 4 * 10
-12, the permeability factor of described multihole device is about 1 * 10
-10To about 1 * 10
-8
11., it is characterized in that the thickness of each in the described main filter cell that described prefilter had and the described first and second gradient filter elements is than being about 1: 1 to about 30: 1 as claim 2 and 3 described prefilters.
12. as claim 2 and 3 described prefilters, it is characterized in that, described gradient filter element has the minimum aperture diameter surface, and the average pore diameter of the described minimum aperture diameter surface that described prefilter had is about 1: 1 to about 20: 1 with the ratio of the average pore diameter of described multihole device.
13. prefilter as claimed in claim 4, it is characterized in that, the described first and second gradient filter elements respectively have the minimum aperture diameter surface, and the average pore diameter of each in each described minimum aperture diameter surface of the described first and second gradient filter elements that described prefilter had is about 1: 1 to about 20: 1 with the ratio of the average pore diameter of described multihole device.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US82024506P | 2006-07-25 | 2006-07-25 | |
| US60/820,245 | 2006-07-25 | ||
| US11/780,266 | 2007-07-19 |
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| Publication Number | Publication Date |
|---|---|
| CN101495206A true CN101495206A (en) | 2009-07-29 |
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| CNA2007800286952A Pending CN101495206A (en) | 2006-07-25 | 2007-07-24 | Graded external prefilter element for continuous-flow systems |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105264372A (en) * | 2013-06-07 | 2016-01-20 | 沃特世科技公司 | Chromatographic filter |
| WO2018014465A1 (en) * | 2016-07-22 | 2018-01-25 | Nv Bekaert Sa | Filtration media and coalescing filter to remove water from liquid hydrocarbons |
-
2007
- 2007-07-24 CN CNA2007800286952A patent/CN101495206A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105264372A (en) * | 2013-06-07 | 2016-01-20 | 沃特世科技公司 | Chromatographic filter |
| US11389747B2 (en) | 2013-06-07 | 2022-07-19 | Waters Technologies Corporation | Chromatographic filter |
| WO2018014465A1 (en) * | 2016-07-22 | 2018-01-25 | Nv Bekaert Sa | Filtration media and coalescing filter to remove water from liquid hydrocarbons |
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Open date: 20090729 |