CN2373793Y - 多用加压电色谱装置 - Google Patents

多用加压电色谱装置 Download PDF

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CN2373793Y
CN2373793Y CN99206093U CN99206093U CN2373793Y CN 2373793 Y CN2373793 Y CN 2373793Y CN 99206093 U CN99206093 U CN 99206093U CN 99206093 U CN99206093 U CN 99206093U CN 2373793 Y CN2373793 Y CN 2373793Y
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阎超
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    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
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    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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Abstract

本实用新型是一种分离检测装置,由高压电源、毛细色谱柱及检测设备构成,所不同的是:这种装置还带有高压泵。通过高压泵,可对毛细色谱柱进行正向、反向、双向加压及正、反向冲洗,从而可以保证毛细色谱柱内无气泡,不断流,柱效高。只要更换不同的色谱柱,即可成为多种新型分离检测装置。附图中有:流动相1,流动相2,泵3,泵4,三通5,三通6,固定架7,单向阀8,单向阀9,进样器10,三通11,毛细色谱柱12,单向阀13,高压电源14,检测仪15,检测槽16,毛细管17,毛细管18,三通19,单向阀20,限流柱21,计算机22。

Description

多用加压电色谱装置
本实用新型是一种涉及分离分析领域的分离检测装置，即一种多用加压电色谱装置。
目前，分离检测装置多由驱动装置、色谱柱以及检测设备所构成。常见的有如下几种：一是气相色谱装置，由气源、气相色谱柱及检测设备构成，主要适用于分离气体混合物和沸点低，易汽化的物质。二是液相色谱装置，由高压泵，带填料的钢色谱柱和检测设备构成，主要适用于分离液态混合物，分离选择性好，但由于驱动力不是电而是压力，流动相在固定相上呈抛物线式前移，有扩散，因而柱效较低。三是毛细管电泳装置，由高压电源、毛细空管和检测设备构成，其特点是驱动力是电，流动相在毛细管内呈柱塞式前移，无扩散，因此可以获得较高的柱效，但对中性样品(不带电的)分离选择性不好。四是毛细电色谱装置，由高压电源，带填料的毛细色谱柱和检测设备构成，这种装置既具有液相色谱的高选择性，又具有毛细管电泳的高柱效，但实用过程中常因产生气泡而使电流中断。
本实用新型的目的是研制一种既能保持毛细电色谱的高柱效和高选择性，又可不断地去除气泡，保证电流不断，同时能冲洗电解产物的新型分离检测装置。
上述目的是由以下技术方案实现的：这种装置也是由驱动装置，色谱柱及检测设备所构成，所不同的是，这种装置还带有高压泵和高压电源。
所说的高压泵，其吸入端通过吸管通入流动相中，其输出端与两支毛细管相连接，其中一支毛细管18通过单向阀9，其末端与色谱柱的尾端以及带有单向阀20的限流柱相接；另一支毛细管17通过单向阀8和单向阀13伸出末端，在单向阀8与13之间又通过毛细管与进样器相接，进样器与色谱柱前端相接。
所说的高压泵的数量可以是一台以上。
所说的色谱柱可以是带填料的毛细色谱柱。
所说的色谱柱可以是毛细空管。
所说的色谱柱可以是带填料的钢色谱柱。
采用上述方案制成的分离检测装置，可以对色谱柱正向、反向或两端进行加压，从而可以保证作电色谱时色谱柱内无气泡，不断流。还可以对毛细色谱柱进行正向或反向冲洗。通过对色谱柱两端加压，可使两端基本无压差，从而可以使流动相的移动只受电驱动而不受压力驱动，保证电色谱的高柱效。此外，更换不同的色谱柱，本装置即可分别代替毛细电色谱装置，毛细管电泳装置，液相色谱装置，而其性能又大大优于现有设备。
附图1是本实用新型的结构示意图。
图中可见：流动相1、流动相2、泵3、泵4、三通5、三通6、固定架7、单向阀8、单向阀9、进样器10、三通11、色谱柱12、单向阀13、高压电源14、检测仪15、检测槽16、毛细管17、毛细管18、三通19、单向阀20、限流柱21、计算机22。
下面结合附图介绍一种实施例。
由图可见，这套装置有两个高压泵3和4，高压泵3的吸入端由吸管插入流动相2中，高压泵4的吸入端由吸管插入流动相1中，两个高压泵的输出端进入三通5的两个孔，三通5的另一孔连接另一个三通6，由三通6的另两个孔接出两支毛细管17和18，毛细管17通过单向阀8联接三通11，并通过三通11连接单向阀13向外伸出末端，三通11的另一孔通过管路连接进样器10。进样器的另外三个口，一口联接色谱柱12，一口进样，另一口接收多余的样品废液。毛细管18通过一个单向阀9连接三通19，三通19的另一孔接色谱柱12的尾端，另一孔伸出限流柱21，限流柱21上设有单向阀20。高压电源14将负高压电源的正端(地线)接在金属进样器10上，负端接在金属三通19上。色谱柱12后部开一检测窗口与检测器15的光路相对。检测器15接计算机22。使用时，只要打开一个泵，调整单向阀，即可实现正向、反向或双向加压。也可进行正、反向冲洗。
工作举例：
一、加压电色谱装置。采用内径320μm，外径630μm，有效柱长20cm，总长40cm，3μmODS填料毛细色谱柱，以加压电色谱法分离硫脲，苯甲醇，萘混合样品。
流动相1用75％乙醇，流动相2选用70％乙腈与30％4mM硼砂混合。先将单向阀9和13关闭，单向阀8和20打开，打开泵3，用流动相2将毛细色谱柱冲洗干净，使其达到平衡。然后，将单向阀13关闭，单向阀9、8、20打开，对毛细色谱柱两端加压。这里要说明的是：由于限流柱21是由有填料的毛细管或细内径毛细空管制成，具有较强的限流作用，所以打开单向阀20以后，既可以回收柱尾液，又不影响两端加压。此时，可在毛细色谱柱两端加上高压电，看是否有电流，电流是否平稳。若电流平稳，可以开启检测系统，准备进行检测。首先通过1个20nl的进样器，用注射器将样品从进样口打入进样器，然后将进样旋钮扭到进样位置即可进样。进样前，先将高压电关闭，进样后立刻加上高压电，几分钟后即可见到三种样品峰。重复实验三次，可见实验的可靠性。实验完毕后，关闭泵3，开启泵4，将单向阀9和13关闭，单向阀8和20打开，用流动相1将毛细色谱柱冲洗干净。如果使用过程中毛细色谱柱堵塞，也可以反冲，即关闭单向阀8和20，打开单向阀9和13即可。
二、毛细管电泳。取毛细空管为色谱柱，即成为一种新型毛细管电泳装置。与普通毛细管电泳装置相比，这种装置的进样不是蘸取，而是通过进样器，同样可以进行正向、反向或两端的加压和冲洗，性能优于普通毛细管电泳装置。
三、微型液相色谱装置。关闭高压电，只用泵正向驱动，此时关闭单向阀9和13，打开单向阀8和20，调节限流柱21使-其通畅，这时，选细内径的带填料的毛细色谱柱或钢色谱柱，即成为一种微型液相色谱装置。当用单泵时，即相当于普通微型液相色谱装置。当用双泵或多泵时，各个泵选用浓度配比不同的流动相做替换，可以做梯度微型液相色谱。由于可以进行正反向冲洗，工作非常方便。

Claims (6)

1、一种多用加压电色谱装置，也是由驱动装置、色谱柱及检测设备等组成，其特征在于：所说的驱动装置是高压泵和高压电源。
2、根据权利要求1所述的多用加压电色谱装置，其特征在于：所说的高压泵，其吸入端通过吸管通入流动相中，其输出端分别与两支毛细管(17)和(18)相连接，其中一支毛细管(18)通过单向阀(9)，其末端分别与色谱柱(12)的尾端以及带有单向阀(20)的限流柱(21)相接；另一支毛细管(17)通过单向阀(8)和单向阀(13)伸出末端，在单向阀(8)和(13)之间，又通过毛细管与进样器(10)相接，进样器(10)与色谱柱(12)前端相接。
3、根据权利要求1所述的多用加压电色谱装置，其特征在于：所说的高压泵的数量可以是一台以上。
4、根据权利要求1所述的多用加压电色谱装置，其特征在于：所说的色谱柱可以是带填料的毛细色谱柱。
5、根据权利要求1所述的多用加压电色谱装置，其特征在于：所说的色谱柱可以是毛细空管。
6、根据权利要求1所述的多用加压电色谱装置，其特征在于：所说的色谱柱可以是带填料的钢色谱柱。
CN99206093U 1999-03-23 1999-03-23 多用加压电色谱装置 Expired - Fee Related CN2373793Y (zh)

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PCT/CN2000/000055 WO2000057172A1 (fr) 1999-03-23 2000-03-20 Appareil de chromatographie electrique polyvalent a pression
US09/914,194 US6569325B1 (en) 1999-03-23 2000-03-20 Multiuse pressure electric chromatographic device
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Cited By (8)

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CN1296122C (zh) * 2004-11-25 2007-01-24 上海交通大学 制备型电层析分离化学物质和生物物质的仪器
CN100447567C (zh) * 2004-09-22 2008-12-31 杭州生源医疗保健技术开发有限公司 构建组合离子膜微电色谱的方法
CN103884814A (zh) * 2014-04-17 2014-06-25 厦门大学 万伏高压电场增强液相色谱系统
CN104330502A (zh) * 2014-11-27 2015-02-04 王峰 一种液相色谱仪
CN104502472A (zh) * 2014-12-05 2015-04-08 上海交通大学 加压制备型电色谱在线检测与样品收集用电安全保护装置
CN104614457A (zh) * 2015-01-13 2015-05-13 上海交通大学 一套中压制备型电色谱分离装置
CN105699465A (zh) * 2016-03-09 2016-06-22 福州大学 一种加压毛细管电色谱多模式连续分离合成色素的方法
CN110672761A (zh) * 2019-09-26 2020-01-10 上海通微分析技术有限公司 一种用于定量定性分析的加压毛细管电色谱装置

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CN100447567C (zh) * 2004-09-22 2008-12-31 杭州生源医疗保健技术开发有限公司 构建组合离子膜微电色谱的方法
CN1296122C (zh) * 2004-11-25 2007-01-24 上海交通大学 制备型电层析分离化学物质和生物物质的仪器
CN103884814A (zh) * 2014-04-17 2014-06-25 厦门大学 万伏高压电场增强液相色谱系统
CN103884814B (zh) * 2014-04-17 2015-10-14 厦门大学 万伏高压电场增强液相色谱系统
CN104330502A (zh) * 2014-11-27 2015-02-04 王峰 一种液相色谱仪
CN104502472A (zh) * 2014-12-05 2015-04-08 上海交通大学 加压制备型电色谱在线检测与样品收集用电安全保护装置
CN104614457A (zh) * 2015-01-13 2015-05-13 上海交通大学 一套中压制备型电色谱分离装置
CN104614457B (zh) * 2015-01-13 2016-08-17 上海交通大学 一套中压制备型电色谱分离装置
CN105699465A (zh) * 2016-03-09 2016-06-22 福州大学 一种加压毛细管电色谱多模式连续分离合成色素的方法
CN105699465B (zh) * 2016-03-09 2018-08-17 福州大学 一种加压毛细管电色谱多模式连续分离合成色素的方法
CN110672761A (zh) * 2019-09-26 2020-01-10 上海通微分析技术有限公司 一种用于定量定性分析的加压毛细管电色谱装置

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US6569325B1 (en) 2003-05-27

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