CN107413072B - Modularized multi-stage chromatographic column and sampling and separating method thereof - Google Patents

Modularized multi-stage chromatographic column and sampling and separating method thereof Download PDF

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CN107413072B
CN107413072B CN201710734224.9A CN201710734224A CN107413072B CN 107413072 B CN107413072 B CN 107413072B CN 201710734224 A CN201710734224 A CN 201710734224A CN 107413072 B CN107413072 B CN 107413072B
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CN107413072A (en
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张广维
雷佳琪
罗孟成
魏颖
解令海
黄维
仲涛涛
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Nanjing University of Posts and Telecommunications
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/18Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
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    • G01N1/10Devices for withdrawing samples in the liquid or fluent state

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Abstract

The invention provides a modularized multi-stage chromatographic column and a sampling and separating method thereof. Compared with the prior art, the invention has the beneficial effects that: in the separation and purification process, the inside of the column can be sampled in real time so as to monitor the separation condition of the chromatographic column and realize dynamic monitoring; the number of the columns can be increased or reduced flexibly according to the requirement; when different components are separated in the column body, the column body with different components can be separated and respectively combined with the column top and the column bottom to be assembled into a plurality of chromatographic columns for use; the method has the characteristics of strong practicability, high flexibility and wide application range.

Description

模块化多级层析柱及其取样、分离方法Modular multi-stage chromatography column and sampling and separation methods

技术领域Technical field

本发明涉及一种模块化多级层析柱及其取样、分离方法,对柱内液体可实时取样分析、可分离自由组合的层析柱,其主要用于化学实验中分离提纯,尤其是在有机化学实验中,将会使用得更为广泛。The invention relates to a modular multi-stage chromatography column and a sampling and separation method thereof. The chromatography column can sample and analyze the liquid in the column in real time and can be separated and combined freely. It is mainly used for separation and purification in chemical experiments, especially in chemical experiments. It will be used more widely in organic chemistry experiments.

背景技术Background technique

目前,在有机化学合成实验室中,通常用到的层析柱,柱顶、柱体和柱底为一个整体,不可分离,不可对柱体内部液体取样分析;柱高固定且规格繁多。这些层析柱在使用过程中,存在着许多不足之处,在分离提纯过程中,对柱内组份无法取样分析,只能通过柱底出液口取样分析是否分离得到纯的化合物,分离过程充满不确定性,并且对于未分离纯的混合组份束手无策,只能重新分离提纯,浪费大量资源和人力成本,极大影响分离提纯效率;在分离两种极性差别大的化合物组份时,在分离出极性小的组份时,无法立即将上部未展开的组份洗脱下来,需要使用大量洗脱剂使上部组份走完整个装柱高度,从出液口分出,耗费大量洗脱剂,不够经济环保;在分离极性相近的化合物,特别是同分异构体时,难于分离,增加柱高又受层析柱高度的限制,定制更高的层析柱,耗费大量成本,且利用率不高,还受操作场地限制,操作难度大。以上缺陷决定了当前层析柱不能经济环保、节能高效,极不适应当前日趋复杂的分离体系。Currently, in organic chemistry synthesis laboratories, chromatography columns are commonly used. The column top, column body and column bottom are a whole and cannot be separated. The liquid inside the column cannot be sampled and analyzed; the column height is fixed and the specifications are various. There are many shortcomings in the use of these chromatography columns. During the separation and purification process, the components in the column cannot be sampled and analyzed. Only the liquid outlet at the bottom of the column can be sampled to analyze whether pure compounds can be separated. The separation process It is full of uncertainty and has no choice but to re-separate and purify the unseparated pure mixed components, which wastes a lot of resources and labor costs and greatly affects the separation and purification efficiency; when separating two compound components with large polar differences, When separating components with low polarity, the upper undeveloped components cannot be eluted immediately. A large amount of eluent needs to be used to make the upper components travel the entire height of the column and be separated from the liquid outlet, which consumes a lot of time. The eluent is not economical and environmentally friendly enough; it is difficult to separate compounds with similar polarity, especially isomers. Increasing the column height is also limited by the height of the chromatography column. Customizing a higher chromatography column costs a lot of money. The cost is low, and the utilization rate is not high. It is also limited by the operating site and is difficult to operate. The above defects determine that current chromatography columns cannot be economical, environmentally friendly, energy-saving and efficient, and are extremely unsuitable for the current increasingly complex separation systems.

随着对层析分离的要求不断提高,对层析柱的改进也逐渐增多,例如:为灵活设定分离过程层析柱以及吸附剂的高度,CN201320200721.8公开了一种组合式层析柱,但是其只能在分离提纯操作前自由配置柱体数目进行使用;为了节约洗脱剂的用量,提高样品的产率,CN201521102771.8公开了一种组合式色谱分离柱,但其并没有解决在柱体分离过程前如何更有效的确定分离开柱体内是否分离得到纯的化合物;为了实现柱体分离,同时进行分别洗脱分离,CN201420693338.5公开了一种可拆分式多节层析柱,但其无法精确检测柱内组份是否分离进入不同柱节,而且在分离提纯的过程中难以克服巨大的真空压力将充满液体的层析柱分离,且在分别洗脱产物时需要将单级柱体中填料取出,增加操作步骤。综合分析,没有一种很好的方案能够在层析柱分离提纯过程中对柱内分离情况及时检测,根据检测分析结果进行柱体分离分别洗脱或者增减柱体数目继续提纯分离。As the requirements for chromatography separation continue to increase, improvements to chromatography columns have gradually increased. For example, in order to flexibly set the height of the chromatography column and adsorbent during the separation process, CN201320200721.8 discloses a combined chromatography column. , but it can only be used by freely configuring the number of columns before the separation and purification operation; in order to save the amount of eluent and improve the yield of the sample, CN201521102771.8 discloses a combined chromatography separation column, but it does not solve the problem How to more effectively determine whether pure compounds are separated from the column before the column separation process; in order to achieve column separation and perform separate elution separations at the same time, CN201420693338.5 discloses a detachable multi-section chromatography column, but it cannot accurately detect whether the components in the column are separated into different column sections, and it is difficult to overcome the huge vacuum pressure to separate the liquid-filled chromatography column during the separation and purification process, and it is necessary to separate the individual components when eluting the products separately. Take out the packing from the first-stage column and add additional steps. Comprehensive analysis shows that there is no good solution that can detect the separation situation in the column in a timely manner during the chromatographic column separation and purification process. According to the detection and analysis results, the columns can be separated and eluted separately or the number of columns can be increased or decreased to continue purification and separation.

因此,为满足在层析分离化合物过程中的取样和柱体分离,设计一种新的分析分离方案十分必要。Therefore, in order to meet the requirements of sampling and column separation during chromatographic separation of compounds, it is necessary to design a new analytical separation scheme.

发明内容Contents of the invention

针对背景技术存在的问题,本发明提供一种实用性强,灵活性高,操作性强,适用面广的层析柱。In view of the problems existing in the background technology, the present invention provides a chromatography column with strong practicability, high flexibility, strong operability and wide application.

本发明是这样实现的:模块化多级层析柱,包括由上至下依次嵌套的柱顶、至少一节柱体和柱底,柱顶、柱体和柱底间的嵌套处相互配合的嵌套面均为磨砂面,柱顶上设有进样口,柱底下设有出液口,出液口上设有控制阀,柱顶的嵌套面上贯通有一个柱顶取样小孔,柱体上端的嵌套面上贯通有一个上部取样小孔,柱体下端的嵌套面上贯通有一个下部取样小孔,柱体下部位于下部取样小孔的上方设有砂芯,柱底的嵌套面上贯通有一个柱底取样小孔,柱顶取样小孔与上部取样小孔之间可通过旋转柱顶与柱体的相对位置相通或不相通,上节柱体的下部取样小孔与下节柱体的上部取样小孔之间通过旋转柱体间的相对位置相通或不相通,下部取样小孔与柱底取样小孔之间可通过旋转柱体与柱底的相对位置相通或不相通。The invention is implemented as follows: a modular multi-stage chromatography column includes a column top, at least one column body and a column bottom that are nested in sequence from top to bottom. The nesting parts between the column top, the column body and the column bottom are mutually exclusive The matching nesting surfaces are all frosted surfaces. There is a sampling port on the top of the column, a liquid outlet on the bottom of the column, a control valve on the liquid outlet, and a top sampling hole running through the nesting surface of the column top. , there is an upper sampling hole running through the nesting surface at the upper end of the cylinder, and there is a lower sampling hole running through the nesting surface at the lower end of the cylinder. The lower part of the cylinder is equipped with a sand core above the lower sampling hole. The bottom of the cylinder There is a sampling hole at the bottom of the column running through the nesting surface. The sampling hole at the top of the column and the sampling hole at the upper part can be connected or disconnected by rotating the relative position of the column top and the cylinder. The sampling hole at the lower part of the upper cylinder The hole and the upper sampling hole of the lower cylinder are connected or not connected through the relative position of the rotating cylinder. The lower sampling hole and the sampling hole at the bottom of the column can be connected through the relative position of the rotating cylinder and the column bottom. Or not connected.

嵌套处的磨砂面间涂抹有真空硅脂。Vacuum silicone grease is applied between the matte surfaces of the nesting area.

柱顶取样小孔、上部取样小孔、下部取样小孔和柱底取样小孔的孔径均相同。The sampling holes at the top of the column, the upper sampling holes, the lower sampling holes and the sampling holes at the bottom of the column all have the same diameter.

砂芯的直径与柱体的内径相匹配。The diameter of the sand core matches the inner diameter of the cylinder.

进样口上可拆卸连接磨口塞。The ground port plug can be detachably connected to the injection port.

模块化多级层析柱的取样方法,分为柱内常压取样和柱内负压取样;柱内常压取样通过旋转嵌套处的上下节柱体的相对位置使上节柱体的下部取样小孔与下节柱体的上部取样小孔对齐,柱内液体由于压强而流出,进行取样;柱内负压取样,取样前在柱顶上部嵌套处加上一个对应的磨口塞密闭,然后使柱底出液口处溶剂继续流出,当柱底出液口液体缓慢滴下时,即关闭柱底的控制阀,旋转上下两节柱体,溶剂上方空腔负压和取样小孔外部大气压的共同作用下减缓取样小孔处溶剂流出速率,可对取样小孔流出的微量溶剂进行取样。The sampling method of the modular multi-stage chromatography column is divided into normal pressure sampling in the column and negative pressure sampling in the column; normal pressure sampling in the column rotates the relative positions of the upper and lower cylinders at the nesting point so that the lower part of the upper cylinder The sampling holes are aligned with the upper sampling holes of the lower column. The liquid in the column flows out due to pressure and is sampled. The column is sampled under negative pressure. Before sampling, a corresponding grinding plug is added to the upper nesting part of the column top to seal it. , and then allow the solvent to continue to flow out from the liquid outlet at the bottom of the column. When the liquid from the liquid outlet at the bottom of the column drips slowly, the control valve at the bottom of the column is closed, and the upper and lower cylinders are rotated. The negative pressure in the cavity above the solvent and the outside of the sampling hole The atmospheric pressure slows down the outflow rate of the solvent from the sampling hole, and can sample trace amounts of solvent flowing out of the sampling hole.

模块化多级层析柱的分离方法,柱体分离前,在柱顶加上密封的磨口塞,同时使在出液口溶剂继续流出至完全停止,此时关闭柱底的控制阀,将每一级的取样小孔处与大气相通,此时取样小孔处会有空气进入砂芯以下的嵌套处,即可将取样小孔上方的部分整体分离开,砂芯以上的溶剂会因为在砂芯处表面张力和液体上方的负压作用而不会流出,即可将柱体自由分离或组合。In the separation method of modular multi-stage chromatography column, before column separation, a sealing ground plug is added to the top of the column, and at the same time, the solvent at the outlet continues to flow out until it completely stops. At this time, the control valve at the bottom of the column is closed, and the The sampling holes at each level are connected to the atmosphere. At this time, air will enter the nesting area below the sand core at the sampling holes, which can separate the entire part above the sampling holes. The solvent above the sand core will be The cylinders can be separated or combined freely due to the surface tension at the sand core and the negative pressure above the liquid without flowing out.

与现有技术相比,本发明的有益效果是:对柱内溶剂分离物质情况进行动态监测,可自由分离组合柱体,组装为多支层析柱,增减柱高;在不影响普通加压减压分离的情况下,具有实用性强,灵活性高,操作性强,适用面广,能够满足日益复杂多样的有机物分离需要。Compared with the existing technology, the beneficial effects of the present invention are: dynamic monitoring of solvent separation material conditions in the column, free separation of combined columns, assembly into multiple chromatography columns, and increase or decrease of column height; without affecting ordinary processing In the case of pressure and vacuum separation, it has strong practicability, high flexibility, strong operability and wide application, and can meet the increasingly complex and diverse organic separation needs.

附图说明Description of drawings

图1为柱顶的结构示意图;Figure 1 is a schematic structural diagram of the column top;

图2为柱体的结构示意图;Figure 2 is a schematic structural diagram of the column;

图3为柱底的结构示意图;Figure 3 is a schematic structural diagram of the column bottom;

图4为包括三节层析柱的模块化多级层析柱及其取样、分离方法的结构示意图;Figure 4 is a schematic structural diagram of a modular multi-stage chromatography column including three sections of chromatography column and its sampling and separation method;

图5为图4中E截面处的取样孔不相通时的结构示意图;Figure 5 is a schematic structural diagram when the sampling holes at section E in Figure 4 are not connected;

图6为图4中E截面处的取样孔相通时的结构示意图。Figure 6 is a schematic structural diagram when the sampling holes at section E in Figure 4 are connected.

其中,1-柱顶,2-柱体,3-柱底,4-进样口,5-出液口,6-控制阀,7-柱顶取样小孔,8-上部取样小孔,9-下部取样小孔,10-柱底取样小孔,11-砂芯。Among them, 1-column top, 2-column body, 3-column bottom, 4-inlet, 5-liquid outlet, 6-control valve, 7-column top sampling hole, 8-upper sampling hole, 9 -Lower sampling holes, 10-sampling holes at the bottom of the column, 11-sand core.

具体实施方案Specific implementation plan

为了使本发明的目的、技术方案和优点更加清楚明白,以下结合附图及实施例对本发明做进一步详细说明。In order to make the purpose, technical solutions and advantages of the present invention more clear, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

针对背景技术存在的问题,本发明提供一种实用性强,灵活性高,操作性强,适用面广的层析柱,提供在层析分离过程中,对柱内组份进行取样分析的动态监测方案和柱体分离并自由组装组合的方案。In view of the problems existing in the background technology, the present invention provides a chromatography column with strong practicability, high flexibility, strong operability and wide application, and provides a dynamic method for sampling and analyzing the components in the column during the chromatographic separation process. Monitoring solutions and columns are separated and freely assembled combined solutions.

图中包括以下部件:柱顶1、柱体2、柱底3、进样口4、出液口5、控制阀6、柱顶取样小孔7、上部取样小孔8、下部取样小孔9、柱底取样小孔10和砂芯11。The figure includes the following components: column top 1, column body 2, column bottom 3, inlet 4, liquid outlet 5, control valve 6, column top sampling hole 7, upper sampling hole 8, lower sampling hole 9 , sampling holes 10 and sand core 11 at the bottom of the column.

如图1-6所示,模块化多级层析柱及其取样、分离方法,包括由上至下依次嵌套的柱顶、至少一节柱体和柱底,柱顶、柱体和柱底间的嵌套处相互配合的嵌套面均为磨砂面,柱顶上设有进样口,柱底下设有出液口,出液口上设有控制阀,柱顶的嵌套面上贯通有一个柱顶取样小孔,柱体上端的嵌套面上贯通有一个上部取样小孔,柱体下端的嵌套面上贯通有一个下部取样小孔,柱体下部位于下部取样小孔的上方设有砂芯,柱底的嵌套面上贯通有一个柱底取样小孔,柱顶取样小孔与上部取样小孔之间可通过旋转柱顶与柱体的相对位置相通或不相通,上节柱体的下部取样小孔与下节柱体的上部取样小孔之间通过旋转柱体间的相对位置相通或不相通,下部取样小孔与柱底取样小孔之间可通过旋转柱体与柱底的相对位置相通或不相通。As shown in Figure 1-6, the modular multi-stage chromatography column and its sampling and separation methods include a column top, at least one column and a column bottom nested in sequence from top to bottom. The column top, column and column The matching nesting surfaces at the bottom are all frosted surfaces. There is an inlet on the top of the column, a liquid outlet on the bottom of the column, a control valve on the liquid outlet, and the nesting surface on the top of the column is connected through There is a small sampling hole on the top of the column. There is an upper sampling hole running through the nesting surface at the upper end of the cylinder. There is a lower sampling hole running through the nesting surface at the lower end of the cylinder. The lower part of the cylinder is located above the lower sampling hole. There is a sand core, and there is a small sampling hole at the bottom of the column running through the nesting surface of the bottom of the column. The sampling hole at the top of the column and the sampling hole at the upper part can be connected or not connected by rotating the relative position of the column top and the column. The lower sampling hole of the segment cylinder and the upper sampling hole of the lower segment cylinder are connected or not connected through the relative position of the rotating cylinder. The lower sampling hole and the sampling hole at the bottom of the column can be connected through the rotating cylinder. Connected or disconnected from the relative position of the column bottom.

嵌套处的磨砂面间涂抹有真空硅脂。Vacuum silicone grease is applied between the matte surfaces of the nesting area.

柱顶取样小孔、上部取样小孔、下部取样小孔和柱底取样小孔的孔径均相同。The sampling holes at the top of the column, the upper sampling holes, the lower sampling holes and the sampling holes at the bottom of the column all have the same diameter.

砂芯的直径与柱体的内径相匹配。The diameter of the sand core matches the inner diameter of the cylinder.

进样口上可拆卸连接磨口塞。The ground port plug can be detachably connected to the injection port.

模块化多级层析柱的取样方法,分为柱内常压取样和柱内负压取样;柱内常压取样通过旋转嵌套处的上下节柱体的相对位置使上节柱体的下部取样小孔与下节柱体的上部取样小孔对齐,柱内液体由于压强而流出,进行取样;柱内负压取样,取样前在柱顶上部嵌套处加上一个对应的磨口塞密闭,然后使柱底出液口处溶剂继续流出,当柱底出液口液体缓慢滴下时,即关闭柱底的控制阀,旋转上下两节柱体,溶剂上方空腔负压和取样小孔外部大气压的共同作用下减缓取样小孔处溶剂流出速率,可对取样小孔流出的微量溶剂进行取样。The sampling method of the modular multi-stage chromatography column is divided into normal pressure sampling in the column and negative pressure sampling in the column; normal pressure sampling in the column rotates the relative positions of the upper and lower cylinders at the nesting point so that the lower part of the upper cylinder The sampling holes are aligned with the upper sampling holes of the lower column. The liquid in the column flows out due to pressure and is sampled. The column is sampled under negative pressure. Before sampling, a corresponding grinding plug is added to the upper nesting part of the column top to seal it. , and then allow the solvent to continue to flow out from the liquid outlet at the bottom of the column. When the liquid from the liquid outlet at the bottom of the column drips slowly, the control valve at the bottom of the column is closed, and the upper and lower cylinders are rotated. The negative pressure in the cavity above the solvent and the outside of the sampling hole The atmospheric pressure slows down the outflow rate of the solvent from the sampling hole, and can sample trace amounts of solvent flowing out of the sampling hole.

模块化多级层析柱的分离方法,柱体分离前,在柱顶加上密封的磨口塞,同时使在出液口溶剂继续流出至完全停止,此时关闭柱底的控制阀,将每一级的取样小孔处与大气相通,此时取样小孔处会有空气进入砂芯以下的嵌套处,即可将取样小孔上方的部分整体分离开,砂芯以上的溶剂会因为在砂芯处表面张力和液体上方的负压作用而不会流出,即可将柱体自由分离或组合。In the separation method of modular multi-stage chromatography column, before column separation, a sealing ground plug is added to the top of the column, and at the same time, the solvent at the outlet continues to flow out until it completely stops. At this time, the control valve at the bottom of the column is closed, and the The sampling holes at each level are connected to the atmosphere. At this time, air will enter the nesting area below the sand core at the sampling holes, which can separate the entire part above the sampling holes. The solvent above the sand core will be The cylinders can be separated or combined freely due to the surface tension at the sand core and the negative pressure above the liquid without flowing out.

实施例Example

每一节柱体都可以单独与柱顶和柱底组装成一支层析柱,亦可将多节柱体与柱顶、柱底组合使用;还可以在使用过程中调节相邻柱体嵌套处的取样小孔的位置,进行取样分析,实现动态检测,根据取样过程的要求,可以进行对溶剂少量损失的柱内常压取样和溶剂微量损失的柱内负压取样;还可以在分离提纯过程中,分离柱体,各自组装成新的层析柱,分别洗脱分离;还可以在未分离开组份的柱体,减少上方无组份的柱体数,增加下方填充分离材料的柱体数,灵活应对分离提纯过程中出现的问题。Each column section can be assembled separately with the column top and column bottom to form a chromatography column, or multi-section columns can be used in combination with the column top and column bottom; the nesting of adjacent columns can also be adjusted during use. At the position of the sampling hole, sampling and analysis can be carried out to achieve dynamic detection. According to the requirements of the sampling process, normal pressure sampling in the column with a small loss of solvent and negative pressure sampling in the column with a small loss of solvent can also be carried out during separation and purification. During the process, the separation columns are each assembled into a new chromatography column, which is eluted and separated separately. You can also reduce the number of columns without components on the top of the columns that have not been separated, and increase the number of columns filled with separation materials on the bottom. number of cells to flexibly respond to problems that arise during the separation and purification process.

实施例1:动态监测—柱内常压取样Example 1: Dynamic monitoring—normal pressure sampling in the column

柱内常压取样利用液体压强的原理,通过旋转嵌套处的上下节柱体的相对位置使上节柱体的下部取样小孔与下节柱体的上部取样小孔对齐,柱内液体由于压强而流出,进行取样,为减少溶剂损失,需快速旋转,减少两个取样小孔正对的时间。Normal pressure sampling in the column uses the principle of liquid pressure. By rotating the relative positions of the upper and lower cylinders at the nesting point, the lower sampling holes of the upper cylinder are aligned with the upper sampling holes of the lower cylinder. The liquid in the column is It flows out under high pressure and takes samples. In order to reduce the loss of solvent, it needs to be rotated quickly to reduce the time for the two sampling holes to face each other.

如图4所示,以3节柱体组合成一支三级层析柱为例,其第2节柱体与第3节柱体的嵌套处的剖面图见图5。本实施例包括:柱顶1,3节柱体2和柱底3,各模块间通过磨砂处理的嵌套面套接保证密封性,在嵌套面间涂抹润滑剂,如真空硅脂,真空硅脂既可以保证气密性又能保证各模块之间可自由相对转动,不影响分离。As shown in Figure 4, taking the combination of three cylinder sections to form a three-stage chromatography column as an example, the cross-sectional view of the nesting point of the second column section and the third column section is shown in Figure 5. This embodiment includes: a column top 1, a three-section column 2 and a column bottom 3. The modules are connected through frosted nesting surfaces to ensure sealing. Lubricant, such as vacuum silicone grease, is applied between the nesting surfaces. Silicone grease can not only ensure air tightness but also ensure that each module can rotate freely relative to each other without affecting separation.

如图5和图6所示,对第2节柱体的分离情况进行取样分析,直接通过固定第3节柱体及以下的部分,转动第2节柱体及以上的部份使第2节柱体的下部取样小孔9与第3节柱体的上部取样小孔8相对,此时柱体在此取样小孔处与大气相通,柱内溶剂在液体压力作用下从取样小孔流出,即可对此处进行溶剂取样。As shown in Figure 5 and Figure 6, the separation of the second section of the cylinder was sampled and analyzed. The section 2 was directly fixed by fixing the section of the third column and below, and rotating the section of the second section of the column and above. The sampling hole 9 at the lower part of the cylinder is opposite to the sampling hole 8 at the upper part of the cylinder in section 3. At this time, the cylinder is connected to the atmosphere at the sampling hole, and the solvent in the column flows out from the sampling hole under the action of liquid pressure. Solvent sampling can be done here.

为减少取样对层析分离的溶剂损失,需快速旋转缩短两取样小孔正对的时间。In order to reduce the solvent loss caused by sampling to chromatographic separation, it is necessary to rotate quickly to shorten the time when the two sampling holes are facing each other.

实施例2:动态监测—柱内负压取样Example 2: Dynamic monitoring—negative pressure sampling in the column

柱内负压取样,取样前在柱顶上部嵌套处加上一个对应的磨口塞密闭,然后使柱底出液口处溶剂继续流出,此时层析柱内溶剂上方空腔产生负压,当柱底出液口液体缓慢滴下时,即关闭柱底的控制阀,此时,溶剂上方空腔的负压产生的压力足以平衡掉大部分的溶剂重力,若使嵌套处的内外取样小孔相对,与大气相通,溶剂上方空腔负压和取样小孔外部大气压的共同作用下减缓取样小孔处溶剂流出速率,快速旋转上下两节柱体,可对取样小孔流出的微量溶剂进行取样分析。Negative pressure sampling in the column. Before sampling, add a corresponding grinding plug to the upper nest of the column top to seal it, and then let the solvent continue to flow out of the liquid outlet at the bottom of the column. At this time, a negative pressure is generated in the cavity above the solvent in the chromatography column. , when the liquid drips slowly from the outlet at the bottom of the column, the control valve at the bottom of the column is closed. At this time, the pressure generated by the negative pressure in the cavity above the solvent is enough to balance out most of the gravity of the solvent. If the inside and outside of the nest are sampled The small holes are opposite and connected to the atmosphere. The negative pressure in the cavity above the solvent and the atmospheric pressure outside the sampling holes slow down the outflow rate of the solvent at the sampling holes. The upper and lower cylinders are quickly rotated to detect trace amounts of solvent flowing out of the sampling holes. Carry out sampling analysis.

在取样前在柱顶1的进样口4处添加磨口塞,实现柱体的密封,让柱内溶剂继续流出,使第1节柱体溶剂上部空腔由于溶剂减少产生负压,当柱底3的出液口5溶剂缓慢滴下,使溶剂上方空腔内负压产生的压力抵消掉大部分的溶剂重力,此时重复上述取样操作,即可明显较少取样小孔处溶剂流出量,达到控制溶剂损失的目的。Before sampling, add a ground plug at the injection port 4 of column top 1 to seal the column and allow the solvent in the column to continue to flow out, so that the upper cavity of the column solvent in section 1 will generate negative pressure due to the reduction of solvent. When the column The solvent is slowly dripped from the liquid outlet 5 of the bottom 3, so that the pressure generated by the negative pressure in the cavity above the solvent offsets most of the gravity of the solvent. At this time, repeating the above sampling operation can significantly reduce the amount of solvent flowing out of the sampling hole. To achieve the purpose of controlling solvent loss.

根据上述操作,即可对多节层析柱柱体的各个取样小孔处进行取样分析,以达到动态监测的目的。According to the above operations, sampling and analysis can be performed on each sampling hole of the multi-section chromatography column to achieve the purpose of dynamic monitoring.

实施例3:自由组合—柱体分离Example 3: Free combination—column separation

柱体分离前,在柱顶加上密封的磨口塞,同时使在出液口溶剂继续流出至完全停止,即能在柱内液体上方形成完全负压,柱内负压产生的压强差与整个层析柱液体的重力平衡,此时关闭柱底的控制阀,每一级的取样小孔处与大气相通时,取样小孔处形成的压强差大于取样小孔上方的液体重力,此时取样小孔处会有空气进入砂芯以下的嵌套处,即可将取样小孔上方的部分整体分离开,砂芯以上的溶剂会因为在砂芯处表面张力和液体上方的负压作用而不会流出,这样就能实现层析柱的自由分离组合,分别洗脱,增加减少柱高等灵活操作。Before the column is separated, a sealed ground plug is added to the top of the column, and at the same time, the solvent continues to flow out of the liquid outlet until it completely stops, that is, a complete negative pressure can be formed above the liquid in the column. The pressure difference generated by the negative pressure in the column is equal to The gravity of the liquid in the entire chromatography column is balanced. At this time, the control valve at the bottom of the column is closed. When the sampling hole at each stage is connected to the atmosphere, the pressure difference formed at the sampling hole is greater than the gravity of the liquid above the sampling hole. At this time At the sampling hole, air will enter the nest below the sand core, which can completely separate the part above the sampling hole. The solvent above the sand core will be dissolved due to the surface tension at the sand core and the negative pressure above the liquid. It will not flow out, so that flexible operations such as free separation and combination of chromatography columns can be realized, elution can be performed separately, column height can be increased or reduced, etc.

同样以第2节柱体和第3节柱体的嵌套处为例,分离两节柱体,参见上述负压取样操作,同样条件下,在柱顶1的进样口处添加磨口塞,实现柱体的密封,让柱内溶剂继续流出至完全停止,使溶剂上方空腔产生的负压产生的压力与溶剂重力达到平衡,此时转动第3节柱体的上方部分,使取样小孔相对,并与大气相通,由于柱内空腔产生的负压与整支层析柱内溶剂平衡,因此其负压产生的压力大于取样小孔上方溶剂的重力,空气进入柱体内部砂芯以下,且砂芯以上的溶剂不会继续流出,此时及可分离第2节柱体和第3节柱体。Take the nesting of the 2nd and 3rd cylinders as an example. Separate the two cylinders. Refer to the above negative pressure sampling operation. Under the same conditions, add a ground plug to the injection port of column top 1. , to achieve the sealing of the column, let the solvent in the column continue to flow out until it completely stops, so that the pressure generated by the negative pressure generated in the cavity above the solvent and the gravity of the solvent can reach a balance. At this time, rotate the upper part of the third column to make sampling smaller The holes are opposite and connected to the atmosphere. Since the negative pressure generated by the cavity in the column is balanced with the solvent in the entire chromatography column, the pressure generated by the negative pressure is greater than the gravity of the solvent above the sampling hole, and the air enters the sand core inside the column. below, and the solvent above the sand core will not continue to flow out. At this time, the 2nd cylinder and the 3rd cylinder can be separated.

将三级层析柱分为上下两部分,原柱顶及第1、2节柱体与1个新柱底组合即可重新组装为一支新的层析柱,1个新柱顶与第3节柱体及原柱底组合即可组装为另一只新的层析柱;还可以根据需要在分离开的第3节柱体与原柱底之间再增加一节或多节填充好填料和溶剂的柱体,组装起来继续层析分离。这样就能达到该层析柱柱体分离和自由组合的目的。Divide the three-stage chromatography column into upper and lower parts. The original column top and the first and second column sections can be reassembled into a new column bottom by combining the original column top and the first and second column sections. The combination of the 3-section column and the original column bottom can be assembled into another new chromatography column; you can also add one or more filling sections between the separated 3-section column and the original column bottom as needed. The column of packing material and solvent is assembled to continue the chromatographic separation. In this way, the purpose of separation and free combination of the chromatography column can be achieved.

以上仅为本发明的较佳实施例而已,并不用以限定本发明,凡在本发明的精神和原则内所作的任何修改、等同替换和改进,均应包含在本发明的范围之内。The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention shall be included in the scope of the present invention.

Claims (7)

1. The utility model provides a multistage chromatographic column of modularization, includes from top to bottom nested post top in proper order, at least one section cylinder and post end, and the nested face of mutually supporting of nested department between post top, cylinder and the post end is the frosting, is equipped with the inlet on the post top, is equipped with the liquid outlet below the post, is equipped with the control valve on the liquid outlet, its characterized in that: a column top sampling small hole is communicated with the nesting surface of the column top, an upper sampling small hole is communicated with the nesting surface of the upper end of the column body, a lower sampling small hole is communicated with the nesting surface of the lower end of the column body, a sand core is arranged above the lower sampling small hole of the column body, a column bottom sampling small hole is communicated with the nesting surface of the column bottom, the column top sampling small hole and the upper sampling small hole can be communicated or not communicated with each other through the relative position of the rotary column top and the column body, the lower sampling small hole of the upper section of column body and the upper sampling small hole of the lower section of column body are communicated or not communicated through the relative position of the rotary column body and the column bottom sampling small hole, and the lower sampling small hole and the column bottom sampling small hole can be communicated or not communicated through the relative position of the rotary column body and the column bottom.
2. The modular multi-stage chromatography column of claim 1, wherein: vacuum silicone grease is smeared between the frosting surfaces of the nested parts.
3. The modular multi-stage chromatography column of claim 1, wherein: the apertures of the column top sampling small hole, the upper sampling small hole, the lower sampling small hole and the column bottom sampling small hole are the same.
4. The modular multi-stage chromatography column of claim 1, wherein: the diameter of the sand core is matched with the inner diameter of the cylinder.
5. The modular multi-stage chromatography column of claim 1, wherein: and the sample inlet is detachably connected with a grinding plug.
6. The method for sampling a modular multi-stage chromatography column according to claim 1, wherein: the method is divided into in-column normal pressure sampling and in-column negative pressure sampling; the normal pressure sampling in the column aligns the lower sampling small hole of the upper section column with the upper sampling small hole of the lower section column by rotating the relative positions of the upper section column and the lower section column at the nesting position, and the liquid in the column flows out due to pressure intensity to sample; the negative pressure sampling is carried out in the column, a corresponding grinding plug is added at the upper nested part of the top of the column before sampling, then the solvent at the liquid outlet of the bottom of the column continuously flows out, when the liquid at the liquid outlet of the bottom of the column slowly drops, the control valve at the bottom of the column is closed, the upper column and the lower column are rotated, the solvent outflow rate at the position of the sampling small hole is slowed down under the combined action of the cavity negative pressure above the solvent and the atmospheric pressure outside the sampling small hole, and the trace solvent flowing out of the sampling small hole can be sampled.
7. The method of separating a modular multi-stage chromatography column of claim 1, wherein: before the cylinder is separated, a sealed grinding plug is added on the top of the cylinder, and simultaneously, the solvent at the liquid outlet is continuously flowed out to be completely stopped, at the moment, a control valve at the bottom of the cylinder is closed, the sampling small hole of each stage is communicated with the atmosphere, at the moment, air enters the nesting position below the sand core at the sampling small hole, the part above the sampling small hole can be wholly separated, the solvent above the sand core can not flow out due to the surface tension at the sand core and the negative pressure above the liquid, and the cylinder can be freely separated or combined.
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