CN1389726A - Column head and column tail structure for liquid phase chromatographic column with zero dead volume and fine inner diameter - Google Patents
Column head and column tail structure for liquid phase chromatographic column with zero dead volume and fine inner diameter Download PDFInfo
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- CN1389726A CN1389726A CN 01115943 CN01115943A CN1389726A CN 1389726 A CN1389726 A CN 1389726A CN 01115943 CN01115943 CN 01115943 CN 01115943 A CN01115943 A CN 01115943A CN 1389726 A CN1389726 A CN 1389726A
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Abstract
This invention provides a head/tail structure of zero dead volume fine inner diameter liquid phase chromatographic column comprising a connecting two-way, a multi-hole filter leaf and an outgoing tube in which the end of the chromatographic column plugs in one side of the connecting two-way and the other side is plugged in by the capillary and a barrel to be fastened by cutting sleeves and screw covers. The two-way forms an equal diameter hole between the two cutting sleeves and the multi-filter leaf placed between the butted joint end of the chromatographic column and the outgoing tube to form a sealed ring naturally at the joint sealing completely slots between the outer wall of the column tube and inner wall of the two way and slot between end of the capillary and sleeve tube.
Description
The present invention relates to a kind of chromatographic technique, a kind of column cap/column end structure of zero dead volume fine inner diameter liquid-phase chromatographic column is provided especially.
Stainless steel filled capillary pipe liquid chromatography is a kind of separate analytical technique that attracts tremendous attention in recent years, and widespread use microtrabeculae liquid phase and mass spectrometry in particularly nearly two protein science researchs more press for further developing of this correlation technique.Compare with conventional liquid chromatography, it is low that it has a solvent consumption, pollutes little, analysis speed is fast, is easy to and advantage such as other detection method on-line coupling, has simple to operate simultaneously again, characteristics easy to use are acknowledged as 21 century and have one of compartment analysis means of future most.But up to the present, commercial stainless steel filled capillary pipe liquid-phase chromatographic column post is imitated the 25-50% that has only theoretical value usually, and this has just limited the promotion and application in practice of stainless steel filled capillary pipe liquid chromatography.Studies show that: different with conventional performance liquid chromatographic column point sample introduction is, the filled capillary pipe liquid-phase chromatographic column is the piston-shaped sample introduction basically, and the diffusion that post tail and fairlead junction take place is serious more than the former.Therefore, the quality of column cap/column end structure design has determined the chromatographic column post to imitate to a great extent.
In stainless steel filled capillary pipe liquid-phase chromatographic column, the two general formula column cap/column end structures identical with conventional liquid-phase chromatographic column are adopted at the post two ends usually at present.In this structure, the junction of chromatographic column column cap/post tail and two pass joints has the slit inevitably.Because stop that the porous filtering sheet thickness of monomer is 0.3-0.5mm, wherein diameter is crushed greater than the part of chromatographic column internal diameter (dI) and has reduced factor of porosity, but still have some holes to make the slit place (w) of moving phase porous to tube wall and two logical heads, big dead band is located also to exist in duct (k), and the smooth finish of duct tube wall is lower, as shown in Figure 3-Figure 5.The combined filtration sheet of outer lining polyphosphazene polymer ether ether ketone (PEEK) material (n) of Chu Xianing has avoided moving phase to be diffused into tube wall in recent years, has improved the post effect.When but this structure is used in internal diameter less than the filled capillary pipe liquid-phase chromatographic column of 2mm, because of the influence of the dead volume of the thicker generation of filter disc and the dead volume (R) between filter disc and the two pass joints bottom just fairly obvious.Sample can arrive tube wall after entering packed capillary column at once, and when bands of a spectrum moved to the binding site of column outlet and joint, the bands of a spectrum broadening all can be caused in slit herein, dead band and rough duct, and post is imitated and reduced.
The object of the present invention is to provide a kind of column cap/column end structure of zero dead volume fine inner diameter liquid-phase chromatographic column, make it be used for the stainless steel filled capillary pipe liquid-phase chromatographic column of internal diameter less than 2mm, can eliminate the slit and the dead volume at column cap/column end structure place effectively, improve duct smooth finish, improve the symmetry of chromatographic column post effect and chromatographic peak.
For achieving the above object, column cap/the column end structure of a kind of zero dead volume fine inner diameter liquid-phase chromatographic column provided by the invention, logical by connecting two, porous filtering sheet and fairlead are formed, fairlead comprises the kapillary and the overcoat flexible and that have chemical inert material to make of inner wall smooth, the terminal insertion of chromatographic column connects two logical sides, kapillary inserts with overcoat and is connected two logical opposite sides, and use cutting ferrule and fixed by nut respectively, connection two is led to an axial isometrical hole between two cutting ferrules, this bore dia is that chromatographic column and fairlead can snugly insert, placing porous filter between chromatographic column end and the fairlead, this filter diameter is between the internal diameter (dI) and external diameter (dO) of chromatographic column, the chromatographic column end directly docks through porous filtering sheet and fairlead, utilize the deformability of kapillary overcoat elastic tube material and the thrust of cutting ferrule pressure cap, make it to be subjected to prestress, naturally form O-ring seal at joint, sealing circle and porous filtering sheet and stainless steel column tail compress simultaneously, stopped up in the porous filtering sheet hole greater than the chromatographic column inner-diameter portion whose fully, its dilation has been sealed space between column jecket outer wall and the two logical inwalls and the slit between capillary column and the sleeve pipe fully.
Described chromatographic column is stainless steel or other metal material filled capillary pipe liquid-phase chromatographic column.
Described chromatographic column can also be polyetheretherketone or the nonmetal tubing filling liquid of hard phase chromatographic column.
Described porous filtering sheet be thickness less than 0.2mm, make less than the material with good strength of filling the carrier particle diameter in the aperture.
Described porous filter disc can be that soft stainless steel, titanium alloy or teflon made.
Below by embodiment and accompanying drawing the present invention is described in detail, and illustrates that simultaneously the present invention compares the useful effect that is had with background technology, wherein:
Fig. 1 is the present invention's zero dead volume column cap/column end structure synoptic diagram;
Fig. 2 is the local enlarged diagram of the present invention's zero dead volume column cap/column end structure;
Fig. 3 is the two general formulas column cap/column end structure synoptic diagram of known technology;
Fig. 4 is the two general formulas column cap/column end structure enlarged diagram of known technology;
Fig. 5 is the combined filtration sheet two general formulas column cap/column end structure enlarged diagram of the outer lining polyetheretherketonematerials materials of known technology;
Fig. 6 is sample with the naphthalene for the present invention, makes relation curve with reduced plate height to analysing interflow speed;
Fig. 7 is used for the analysis of spectra of specimen for the present invention.
Embodiment 1:
As shown in Figures 1 and 2, present embodiment is mainly by connecting two logical (a), porous filtering sheet (e) and fairlead (d) are formed, the overcoat (f) that fairlead (d) comprises the kapillary (b) of inner wall smooth and extracapillary is flexible and have chemically inert polytetrafluoroethylmaterial material to make, chromatographic column (g) is a stainless steel filled capillary pipe liquid-phase chromatographic column, its terminal side that connects two logical (a) of inserting, opposite side inserts fairlead (d) and sleeve pipe, and by cutting ferrule (c) and nut (i) both is fixed.Connection two logical (a) is positioned at an axial isometrical hole (j) is arranged between two cutting ferrules (c), this isometrical hole (j) diameter is that chromatographic column (g) and fairlead (d) can snugly insert, placing porous filter (e) between chromatographic column (g) end and the fairlead (d), porous filtering sheet (e) is that thickness is less than 0.2mm, the aperture is slightly less than the soft stainless steel filter disc of filling the carrier particle diameter, and its diameter is between the internal diameter (dI) and external diameter (dO) of chromatographic column (g).Chromatographic column (g) is terminal directly docks through porous filtering sheet (e) and fairlead (d), utilizes the deformability of extracapillary sleeve pipe elasticity tubing (f) and the thrust of cutting ferrule (c) pressure cap, makes it to be subjected to prestress, forms O-ring seal (h) naturally at joint.Sealing circle (h) compresses simultaneously with porous filtering sheet (e) and stainless steel column cap/post tail, stopped up in the porous filtering sheet (e) hole fully greater than chromatographic column (g) inner-diameter portion whose, its dilation has been sealed column jecket outer wall and the space of two logical inwalls and the slit between capillary column and the sleeve pipe fully, has eliminated the dead volume of column cap/post tail.
Embodiment 2:
Overcoat (f) is made with polyetheretherketonematerials materials, and chromatographic column (g) is that polyetheretherketone (PEEK) is filled liquid-phase chromatographic column, and porous filter disc (e) is the netted filter disc of stainless steel, and all the other are with embodiment 1.
Embodiment 3:
Overcoat (f) is made with poly-ethyl trifluoro-ethylene material, and chromatographic column (g) is filled liquid-phase chromatographic column for stainless steel, and porous filter disc (e) is the netted filter disc of titanium alloy, and all the other are with embodiment 1.
Embodiment 4: overcoat (f) is made with poly-ethyl trifluoro-ethylene material, and chromatographic column (g) is filled liquid-phase chromatographic column for titanium alloy, and porous filter disc (e) is the teflon screen plate, and all the other are with embodiment 1.
Embodiment 5:
Instrument: μ-HPLC system is made up of Jasco PU-1580 high-pressure pump and Jasco CE-975 UV, visible light detecting device (JASCO, Japan).Valco four-way sampling valve (VICI, Switzerland), quantitatively volume 500nL.
Operating conditions: chromatographic column is to fill out Kromasil ODS 5 μ m in 15cm * 0.8mm i.d., with zero dead volume fine inner diameter liquid-phase chromatographic column column cap/column end structure, moving phase is methyl alcohol: water=80: 20 (V/V), specimen: thiocarbamide, benzene, toluene, naphthalene, biphenyl, phenanthrene, anthracene, measure the dead time with thiocarbamide, detect wavelength: 254nm.
With the naphthalene is sample, makes relation curve with reduced plate height to analysing interflow speed, and as shown in Figure 6, at optimum flow rate place (V=4.0), reduced plate height is 2.67, and number of theoretical plate is 7.5 * 10
4/ M is imitated nearly 1 times of raising than the chromatographic column post that adopts conventional column cap/column end structure.Fig. 7 is the analysis of spectra that this chromatographic column is used for specimen, estimates peak shape with the dissymmetry factor at peak height 1/10 place, and the result is as shown in table 1.The dissymmetry factor of each chromatographic peak shows the peak shape symmetry of this chromatographic column in the table between 1.03-1.10, and the outer dead volume of post is little.
Embodiment 6:
Instrument and operating conditions are with embodiment 1.Chromatographic column is to fill out KromasilODS 5 μ m in 25cm * 1.0mm i.d..It is 7.9 * 10 that post is imitated
4/ M, the dissymmetry factor of chromatographic peak is between 1.02-1.09.
Need to prove that above-mentioned embodiment just can not limit the present invention to explanation of the present invention; Therefore; In implication suitable with claims of the present invention and any change in the scope, the luxuriant and rich with fragrance anthracene test of dissymmetry factor (b/a) the specimen benzene toluene naphthalene biphenyl of the different chromatographic peaks of all should think to be included in the scope of claims. table 1. mixture Benzene Toluene Naphthalene Biphenyl Phenanthrene Anthracene dissymmetry factor 1.10 1.09 1.07 1.04 1.03 1.03asymmetric factor k '=1.18 k '=1.85 k '=2.68 k '=3.93 k '=6.53 k '=7.34
Claims (6)
1, a kind of column cap/column end structure of zero dead volume fine inner diameter liquid-phase chromatographic column, logical by connecting two, porous filtering sheet and fairlead are formed, fairlead comprises the kapillary and the overcoat flexible and that have chemical inert material to make of inner wall smooth, it is characterized in that, the terminal insertion of chromatographic column connects two logical sides, kapillary inserts with overcoat and is connected two logical opposite sides, and use cutting ferrule and fixed by nut respectively, connection two is led to an axial isometrical hole between two cutting ferrules, this isometrical bore dia is that chromatographic column and fairlead can snugly insert, placing porous filter between chromatographic column end and the fairlead, this filter diameter is between the internal diameter and external diameter of chromatographic column, the chromatographic column end directly docks through porous filtering sheet and fairlead, utilize the deformability of kapillary overcoat elastic tube material and the thrust of cutting ferrule pressure cap, make it to be subjected to prestress, naturally form O-ring seal at joint, sealing circle and porous filtering sheet and stainless steel column tail compress simultaneously, stopped up in the porous filtering sheet hole greater than the chromatographic column inner-diameter portion whose fully, its dilation has been sealed space between column jecket outer wall and the two logical inwalls and the slit between capillary column and the sleeve pipe fully.
2, the column cap/column end structure of zero dead volume fine inner diameter liquid-phase chromatographic column according to claim 1 is characterized in that described chromatographic column is metal material or the nonmetal tubing filling liquid of hard phase chromatographic column.
3, the column cap/column end structure of zero dead volume fine inner diameter liquid-phase chromatographic column according to claim 2 is characterized in that, described chromatographic column is that stainless steel, titanium alloy or polyetheretherketone are filled liquid-phase chromatographic column.
4, the column cap/column end structure of zero dead volume fine inner diameter liquid-phase chromatographic column according to claim 1 is characterized in that the thickness of described porous filtering sheet is less than 0.2mm.
According to the column cap/column end structure of claim 1 or 4 described zero dead volume fine inner diameter liquid-phase chromatographic columns, it is characterized in that 5, described porous filtering sheet is that the aperture is slightly less than the material with good strength of filling the carrier particle diameter and makes.
6, the column cap/column end structure of zero dead volume fine inner diameter liquid-phase chromatographic column according to claim 5 is characterized in that described porous filtering sheet is that soft stainless steel, titanium alloy or teflon made.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB01115943XA CN1174247C (en) | 2001-06-06 | 2001-06-06 | Column head and column tail structure for liquid phase chromatographic column with zero dead volume and fine inner diameter |
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| CN1174247C CN1174247C (en) | 2004-11-03 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103823002A (en) * | 2012-11-15 | 2014-05-28 | 道尼克斯索芙特隆公司 | Connector unit and connecting system for connecting capillaries |
| CN104374850A (en) * | 2014-10-24 | 2015-02-25 | 王峰 | Diaphragm type sample injection device |
| US9322811B2 (en) | 2012-11-12 | 2016-04-26 | Dionex Corporation | Zero dead volume robust fluidic connection system |
| CN105670078A (en) * | 2016-01-29 | 2016-06-15 | 太仓卡斯特姆新材料有限公司 | Antistatic and antibacterial plastics and preparation method |
| CN107636457A (en) * | 2015-06-10 | 2018-01-26 | 阿尔卑斯电气株式会社 | Channel unit |
| CN107709984A (en) * | 2015-06-10 | 2018-02-16 | 恩姆菲舍尔科技公司 | Extraction column |
| CN110118724A (en) * | 2018-02-06 | 2019-08-13 | 中国科学院大连化学物理研究所 | A kind of pressure resistance light detection flow cell |
-
2001
- 2001-06-06 CN CNB01115943XA patent/CN1174247C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9322811B2 (en) | 2012-11-12 | 2016-04-26 | Dionex Corporation | Zero dead volume robust fluidic connection system |
| CN103823002A (en) * | 2012-11-15 | 2014-05-28 | 道尼克斯索芙特隆公司 | Connector unit and connecting system for connecting capillaries |
| CN103823002B (en) * | 2012-11-15 | 2015-09-16 | 道尼克斯索芙特隆公司 | For connecting plug unit and the connected system of kapillary |
| US10018604B2 (en) | 2012-11-15 | 2018-07-10 | Dionex Softron Gmbh | Connector unit and connecting system for connecting capillaries, in particular for high-performance liquid chromatography |
| CN104374850A (en) * | 2014-10-24 | 2015-02-25 | 王峰 | Diaphragm type sample injection device |
| CN104374850B (en) * | 2014-10-24 | 2016-01-06 | 王峰 | A kind of diaphragm type sampling device |
| CN107636457A (en) * | 2015-06-10 | 2018-01-26 | 阿尔卑斯电气株式会社 | Channel unit |
| CN107709984A (en) * | 2015-06-10 | 2018-02-16 | 恩姆菲舍尔科技公司 | Extraction column |
| CN107636457B (en) * | 2015-06-10 | 2020-07-28 | 阿尔卑斯阿尔派株式会社 | Flow path unit |
| CN105670078A (en) * | 2016-01-29 | 2016-06-15 | 太仓卡斯特姆新材料有限公司 | Antistatic and antibacterial plastics and preparation method |
| CN110118724A (en) * | 2018-02-06 | 2019-08-13 | 中国科学院大连化学物理研究所 | A kind of pressure resistance light detection flow cell |
| CN110118724B (en) * | 2018-02-06 | 2021-10-29 | 中国科学院大连化学物理研究所 | Withstand voltage light detects flow-through cell |
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| CN1174247C (en) | 2004-11-03 |
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