CN102012411B - Stagnation-eliminating chromatographic column, stagnation-eliminating chromatograph and analysis method thereof - Google Patents

Stagnation-eliminating chromatographic column, stagnation-eliminating chromatograph and analysis method thereof Download PDF

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CN102012411B
CN102012411B CN 201010516298 CN201010516298A CN102012411B CN 102012411 B CN102012411 B CN 102012411B CN 201010516298 CN201010516298 CN 201010516298 CN 201010516298 A CN201010516298 A CN 201010516298A CN 102012411 B CN102012411 B CN 102012411B
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column
analysis
chromatograph
smolder
voltage
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CN102012411A (en )
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戴朝政
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戴朝政
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Abstract

本发明所要解决的技术问题是提供一种能消除吸附剂颗粒表面滞流层且柱效能高的色谱柱、色谱仪及其分析方法。 The present invention solves the technical problem is to provide a high-efficiency elimination column chromatography and analysis of particles and stagnant layer surface of the adsorbent column. 消滞色谱柱,包括柱管和填充于其内腔中作为固定相的吸附剂,所述柱管采用不导电的绝缘材料制成,或所述柱管采用金属材料制成,但金属柱管内壁设置不导电的绝缘材料。 Xiaozhi column, and the column tube including a lumen thereof is filled as an adsorbent in the stationary phase, the column tube with the non-conductive insulating material, or a column tube made of metal material, but the metal vial an insulating wall is provided electrically non-conductive material. 由于本发明的色谱柱不存在中心电极,由过去的沿色谱柱的径向施加电压改变为轴向施压,色谱柱发热均匀,色谱柱中心与边缘温差小,能显著提高色谱柱的柱效能,使色谱仪具有更高的分离能力和更快的分析速度。 Since the column of the present invention is the absence of the center electrode, the applied voltage is changed by a radial direction past the axial pressure column, the column heating uniformity, small temperature difference between the center and edge column, the column can significantly improve the efficacy of the column the chromatograph having a higher separation capacity and faster analysis.

Description

消滞色谱柱、消滞色谱仪及其分析方法 Xiaozhi column chromatography and analysis of smolder

技术领域 FIELD

[0001] 本发明涉及液相色谱分析仪,特别涉及消滞色谱柱、消滞色谱仪及其分析方法。 [0001] The present invention relates to liquid chromatograph, and more particularly to Xiaozhi column chromatography and analysis of smolder.

背景技术 Background technique

[0002] 液相色谱分析仪主要由色谱柱、进样系统、输液泵、检测器、数据系统等部分组成。 Part [0002] Liquid chromatograph column mainly, injection system, infusion pumps, a detector, a data system components. 色谱柱包括柱管和填充于其内腔中作为固定相的吸附剂。 Column tube and comprising a column filled with the adsorbent as a stationary phase lumen thereto. 使用液相色谱分析仪时,样品被流动相带入色谱柱中,由于被检测样品中不同物质与固定相作用吸附能力的强弱不同,不同物质依吸附能力的强弱顺序离开色谱柱到达检测器,检测器检测到物质被洗提出来的信号,通过比对这些信号来进行待测定样品的定性和定量分析。 When using a liquid chromatograph, a sample is brought into the column mobile phase, due to the different strength of the test sample and the stationary phase separation material different adsorption capacity, leaving columns of different substances from reaching the detector by the strength of the order of adsorption capacity , a signal detector detecting the eluted material was analyzed by qualitative and quantitative ratio of these signals to the sample to be measured.

[0003] 色谱分析要求分离效能越高越好。 [0003] The chromatographic separation efficiency requirements better. 色谱仪分离性能的好坏很大程度决定于色谱柱的效能。 The quality of the chromatograph separation performance to a large extent depend on the effectiveness of the column. 长期以来人们对色谱柱不断地进行改进,以期具有更高的分离能力。 It has long been the column is constantly improved in order to have a higher separation ability. 色谱柱的柱效能是由许多因素决定的,理论研究表明,由于液体的粘滞作用,色谱柱在操作时作为吸附剂的固定相颗粒表面存在一个由流动相组成的几乎不可移动的滞流层,被分析物质在自由扩散的作用下,穿过滞流层与吸附剂颗粒表面的物质交换。 Column Column performance is determined by many factors, theoretical studies have shown that, due to the effect of the viscous fluid, operating as a column in the presence of the adsorbent particle surfaces of a stationary phase by the flow stagnant layer phase almost immovable , analyte under the action of free diffusion through the stagnant layer material exchange adsorbent particle surface. 吸附剂颗粒表面存在的滞流层阻碍了流动相与固定相之间物质的自由传输,因此成了制约液相色谱柱效能和分析速度的重要原因。 Stagnant layer of particles present in the surface of the adsorbent impede free flow of the substance transfer between the stationary phase and thus become an important reason for restricting liquid chromatography column efficiency and the speed of analysis. 显然,如果设法消除吸附剂颗粒表面的滞流层,使流动相中的被检测物质直接与吸附剂颗粒表面进行交换,色谱柱的柱效能将会得到显著提高,液相色谱仪的分析速度也将得到加快。 Obviously, if the try to eliminate stagnant layer of the adsorbent particle surfaces, so that the mobile phase is directly detected substance exchange surface of the adsorbent particle, column by column performance will be significantly improved, the speed of the liquid chromatograph analysis also will be accelerated.

[0004] 色谱柱内的吸附剂通常采用的是多孔、大比表面积的二氧化硅为载体。 [0004] The adsorbent in the column used is typically a porous, large surface area of ​​the silica support. 根据电化学理论,二氧化硅接触水溶液后其表面的硅醇基会电离,硅醇基电离后二氧化硅表面带电荷,靠近二氧化硅表面的溶液则会感应出相反电荷,这就是所谓的双电层结构。 The electrochemical theory, the silica is contacted with an aqueous silanol which would ionization surface, the silica surface silanol groups ionized charged, the solution will be close to the silica surface induces an opposite charge, which is called electric double layer structure. 双电层位于滞流层的底部,根据电荷相互作用的原理,如果对双电层结构施加一个电场,双电层结构的溶液在库伦力的作用下就会移动,溶液的这种运动被称为电渗流。 An electric double layer at the bottom of the stagnant layer, according to the principle of charge interaction, if an electric field is applied to the electric double layer structure, the structure of the electric double layer solution will move under the influence of Coulomb force, this movement is referred to the solution electrical flow. 随着电渗流的产生,电渗流带动吸附剂颗粒表面滞流层,滞流层也就随之消失。 With the flow of electricity generated, driven by electroosmotic flow surface of the adsorbent particles stagnant layer, stagnant layer will disappear. ZL200620034672.5公开了一种对消滞色谱柱采用径向施加电压的方法,如图1所示,径向施加电压的消滞色谱柱采用金属柱管,管壁作为一个电极,管中心有另外一个电极,因此其消滞电压是施加于管壁与中心电极上,色谱柱内固定相表面滞留层将会消失,流动相与固定相之间的传质得以加速,即传质阻力得以克服。 ZL200620034672.5 discloses a method of applying a voltage to the radial separation of the sample Xiaozhi, shown in Figure 1, a voltage is applied radially smolder column metal column tube, the tube wall as one of the electrodes, there is another control center an electrode, which voltage is applied to the smolder tube wall and the center electrode, the inner surface of the column stationary phase retention layer will disappear, the mobile phase mass transfer is accelerated between the stationary phase, i.e., the mass transfer resistance is overcome. 但由于这种办法存在中心电极,工作时,色谱柱中间电流密度大,温度高,柱管的中间和边缘存在较大温差,色谱柱的柱效能会受到影响,从而影响了液相色谱仪的分析效能。 However, this approach due to the presence of the center electrode, in operation, the column intermediate current density, high temperature, there is a large temperature difference between the middle and the edge of the column tube, column by column performance will be affected, thus affecting the liquid chromatograph analysis of efficacy.

发明内容 SUMMARY

[0005] 本发明所要解决的技术问题是提供一种能消除吸附剂颗粒表面滞流层且柱效能高的色谱柱、色谱仪及其分析方法。 [0005] The present invention solves the technical problem can be eliminated to provide a high-performance column chromatography and analysis of particles and stagnant layer surface of the adsorbent column.

[0006] 本发明解决技术问题所采用的技术方案是:消滞色谱柱,包括柱管和填充于其内腔中作为固定相的吸附剂,所述柱管采用不导电的绝缘材料制成,或所述柱管采用金属材料制成,但金属柱管内壁设置不导电的绝缘材料。 [0006] Technical Solution The present invention solves the technical problem: Xiaozhi column comprising a column tube and the lumen thereof is filled as an adsorbent stationary phase, the column tube electrically nonconductive insulating material, or said column tube made of metal material, metal pillar inner wall disposed non-conductive insulating material.

[0007]消滞色谱仪,包括色谱柱、进样系统、输液泵、检测器和数据系统,所述色谱柱采用权利要求1所述的消滞色谱柱。 [0007] Xiaozhi chromatography, including column, injector systems, infusion pumps, a detector and data system, the chromatography column using the column smolder claim 1.

[0008]消滞色谱仪的分析方法,分析时,沿色谱柱的轴向施加电压,在柱管内形成沿色谱柱的轴向电场,在电场作用下吸附剂表面产生电渗流,进而消除固定相表面的滞流层,使流动相中的被检测物质直接与吸附剂颗粒表面进行交换,色谱柱的柱效能得到显著提高,色谱仪的分析速度加快,从而提高色谱分析效率。 [0008] Analysis smolder chromatograph analysis, a voltage is applied in the axial direction of the column, the column to form an axial electric field in a vial, an electroosmotic flow generated surface of the adsorbent in the electric field, thereby eliminating the stationary phase the surface of the stagnant layer, the flow is subjected to phase detectable substance exchanged directly with the surface of the adsorbent particles, column by column performance has been significantly improved, accelerated chromatograph analysis speed, thereby improving the efficiency of chromatographic analysis.

[0009] 进一步的,所述电压施加于两片电极上,而两片电极分别放置于进样系统的溶剂瓶和废液瓶中,依靠金属管线和接头,将消滞电压引至色谱柱的进口和出口两端,使两个接头之间具有不同电势,从而在柱管内形成沿色谱柱的轴向电场。 [0009] Further, the voltage applied to the two electrodes, the two electrodes are placed in a vial and the solvent waste bottle injection system, relying on metal pipes and fittings, the voltage introduced to the column smolder inlet and outlet ends that have different potentials between the two connectors, thereby forming an electric field along the axial direction of the column in the column tube.

[0010] 更进一步的,所述电压是直流电、交流电或脉冲电。 [0010] Further still, the voltage is a DC, AC or pulse.

[0011] 本发明的有益效果是:由于本发明的色谱柱不存在中心电极,由过去的沿色谱柱的径向施加电压改变为轴向施压,色谱柱发热均匀,色谱柱中心与边缘温差小,能显著提高色谱柱的柱效能,使色谱仪具有更高的分离能力和更快的分析速度。 [0011] Advantageous effects of the present invention are: the column of the invention due to the absence of the center electrode, past the radial direction is applied by the column voltage is changed to axial pressure, even heating the column, the column temperature difference between the center and the edge small, can significantly improve the effectiveness of the column in the column, chromatographic separation apparatus having a higher capacity and faster analysis.

附图说明 BRIEF DESCRIPTION

[0012] 图1是现有技术的径向施加电压的消滞色谱仪示意图。 [0012] FIG. 1 is a schematic radial chromatography smolder prior art applied voltage.

[0013] 图2是本发明的轴向施加电压的消滞色谱仪示意图。 [0013] FIG. 2 is a schematic axial smolder chromatograph of the present invention applied voltage.

具体实施方式 detailed description

[0014] 色谱柱的柱管一般都是采用金属材料制成,本发明的消滞色谱柱的柱管采用不导电的绝缘材料制成;或柱管采用金属材料制成,但金属柱管内壁必须设置不导电的绝缘材料。 [0014] Column column tube are generally made of a metal material, the column of the present invention smolder vial made of non-conductive insulating material; the column tube, or made of metal materials, the metal inner wall of the column It must be set to non-conductive insulating material. 柱管内充填通常使用的作为固定相的吸附剂,使柱管内充满细小的固定相颗粒。 Filling the column tube is generally used as an adsorbent stationary phase, the stationary phase so that fine particles fill the column tube. 在色谱分析时,沿色谱柱的轴向施加适当的电压,由于本发明的消滞色谱柱的柱管采用不导电的绝缘材料制成,或采用内壁设置绝缘材料的金属材料制成,因此通电后可以在柱管内形成沿色谱柱的轴向电场,在电场作用下吸附剂表面产生电渗流,进而消除固定相表面的滞流层,使流动相中的被检测物质直接与吸附剂颗粒表面进行交换。 When chromatographic analysis, appropriate voltages are applied in the axial direction of the column, the column due smolder vial of the present invention uses non-conductive insulating material, or an insulating material is provided using the inner wall of a metal material, and therefore the energization after the column tube may be formed in the axial electric field along the column, the adsorbent generates an electroosmotic flow in the surface electric field, thereby eliminating stagnant layer of the stationary phase, the flow of particulate substance to be detected with the surface of the adsorbent phase direct exchange. 由于滞流层的传质阻力消除,色谱柱的柱效能得到显著提高,液相色谱仪流动相的最佳流速提高,而且由于本发明不存在中心电极,因此色谱柱发热均匀,温差小,色谱柱的柱效能更高,色谱分析速度也将加快,分析效率也会更高。 Mass transfer resistance due to the elimination of stagnant layer, column by column performance has been significantly improved, the optimal flow rate to improve liquid chromatography mobile phase, and since the central electrode of the present invention does not exist, even heating the column, the temperature difference is small, chromatography column column higher performance, will also accelerate the speed chromatographic analysis, analysis of efficiency will be higher.

[0015] 本发明施加的电压可以是直流电、交流电或脉冲电,根据色谱分析的实际要求,电压幅度可以连续调控。 [0015] The voltage applied to the present invention may be a DC, AC or pulse, according to the actual requirements of chromatographic analysis, the voltage amplitude can be continuously regulated.

[0016] 本发明采用沿色谱柱的轴向施加电压,具体可采用图2的方式,即将消除滞流层的电压施加于两片电极上,而两片电极分别放置于进样系统的溶剂瓶和废液瓶中,依靠金属管线和接头,将消滞电压引至色谱柱的进口和出口两端,使两个接头之间具有不同电势,产生一个电势差,从而在柱管内形成沿色谱柱的轴向电场。 [0016] The present invention employs a voltage applied to the column axial direction, can be specific embodiment of FIG. 2, the voltage is about to eliminate the stagnant layer is applied to the two electrodes, the two electrodes are placed in sample bottles solvent system and waste bottle, relying on metal pipes and fittings, the smolder voltage lead to the inlet and outlet ends of the column that have different potentials between the two connectors, generating a potential difference, thereby forming the column in the column direction of the tube axial electric field. 当然,电压也可以施加于色谱仪的其它部位,只要能在色谱柱内形成轴向电场就可以了。 Of course, the voltage may be applied to other parts of the chromatograph, as long as an electric field is formed axially in the column on it.

Claims (3)

  1. 1.消滞色谱仪的分析方法,其特征在于:分析时,沿色谱柱的轴向施加电压,在柱管内形成沿色谱柱的轴向电场,在电场作用下吸附剂表面产生电渗流,进而消除固定相表面的滞流层,使流动相中的被检测物质直接与吸附剂颗粒表面进行交换,色谱柱的柱效能得到显著提高,色谱仪的分析速度加快,从而提高色谱分析效率,所述柱管采用不导电的绝缘材料制成,或所述柱管采用金属材料制成,但金属柱管内壁设置不导电的绝缘材料。 Analysis 1. Chromatograph smolder, wherein: the analysis, the column voltage is applied in the axial direction, form an axial electric field along the column in the column tube, producing electroosmotic flow in the electric field adsorbent surface, and further eliminating stagnant layer of the stationary phase, mobile phase so that the test substance be exchanged directly with the surface of the adsorbent particles, column by column performance has been significantly improved, accelerated chromatograph analysis speed, thereby improving the efficiency of chromatographic analysis, the column tube made of electrically nonconductive insulating material, or a column tube made of metal material, metal pillar inner wall disposed non-conductive insulating material.
  2. 2.如权利要求1所述的消滞色谱仪的分析方法,其特征在于:所述电压施加于两片电极上,而两片电极分别放置于进样系统的溶剂瓶和废液瓶中,依靠金属管线和接头,将消滞电压引至色谱柱的进口和出口两端,使两个接头之间具有不同电势,从而在柱管内形成沿色谱柱的轴向电场。 2. The analysis method according to claim smolder chromatography, wherein: the voltage applied to the two electrodes, the two electrodes are placed in a vial and the solvent waste bottle injection system, rely on metal pipes and fittings, the smolder voltage lead to the inlet and outlet ends of the column that have different potentials between the two connectors, thereby forming an electric field along the axial direction of the column in the column tube.
  3. 3.如权利要求1或2所述的消滞色谱仪的分析方法,其特征在于:所述电压是直流电、交流电或脉冲电。 3. The analysis method of claim 12 or smolder chromatograph claim, wherein: said voltage is a DC, AC or pulse.
CN 201010516298 2010-10-22 2010-10-22 Stagnation-eliminating chromatographic column, stagnation-eliminating chromatograph and analysis method thereof CN102012411B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3023835A (en) 1958-10-20 1962-03-06 Phillips Petroleum Co Thermochromatographic analyzer heater
CN1846829A (en) 1998-09-17 2006-10-18 阿德文生物科学公司 Liquid chromatography system, chemical separating arrangement and apparatus and method for mass spectrometric analysis
CN101320021A (en) 2007-06-08 2008-12-10 中国科学院大连化学物理研究所 Interface between directly-heated metal capillary chromatography column and gas chromatograph

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CN2911691Y (en) * 2006-06-21 2007-06-13 戴朝政 Detention eliminating chromatograhic column

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3023835A (en) 1958-10-20 1962-03-06 Phillips Petroleum Co Thermochromatographic analyzer heater
CN1846829A (en) 1998-09-17 2006-10-18 阿德文生物科学公司 Liquid chromatography system, chemical separating arrangement and apparatus and method for mass spectrometric analysis
CN101320021A (en) 2007-06-08 2008-12-10 中国科学院大连化学物理研究所 Interface between directly-heated metal capillary chromatography column and gas chromatograph

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