JP2004093344A - Separate column attitude control mechanism of liquid chromatography - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a separate column attitude control mechanism of a liquid chromatography allowing a connection operation to be easily performed when a temperature-controlled separate column is connected to equipment through piping. <P>SOLUTION: An HPLC 10 comprises a pump 12, an automatic specimen filler 14, a micro column 16, and a detector 18. The inlet side of the micro column 16 is connected to the automatic specimen filler 14 through a fused silica glass pipe 24 and the outlet side of the micro column 16 is connected to the detection part 40 of the detector 18 through a fused silica glass pipe 41. The micro column 16 is stored in a thermostatic container 26, and the thermostatic container 26 is installed in a mounting device 28. The thermostatic container 26 is formed so that the attitude thereof can be three-dimensionally controlled relative to the mounting device 28 according to the position of the disposed detector 18 by an attitude control part formed of a slit and a screw member. <P>COPYRIGHT: (C)2004,JPO

Description

図１０に示すクロマトグラムを見ると、上記３試料の全てについて再現性に優れたデータが得られていることがわかる。
【発明の効果】
本発明に係る液体クロマトグラフィの分離カラム姿勢制御機構によれば、溶離液を送る送液ポンプ、試料を注入する試料注入器、物質を分離する分離カラム、分離した物質を検出する検出器を備え、試料注入器と該分離カラムの入口との間が入口配管により、および分離カラムの出口と検出器とが出口配管により、それぞれ接続される液体クロマトグラフィにおいて、分離カラムがヒータを備えた恒温容器の内部に収容され、恒温容器の姿勢を制御することにより、分離カラムの姿勢を一次元的乃至三次元的に制御する姿勢制御部を有し、また、本発明に係る液体クロマトグラフィの分離カラム姿勢制御機構において、恒温容器を取り付ける取り付け装置を備え、姿勢制御部は、取り付け装置に対する該恒温容器の姿勢を制御するように構成してなるため、温度制御された分離カラムと各機器とを接続するときに、分離カラムの姿勢を変えることで、接続作業を容易に行うことができる。
【００５８】
また、本発明に係る液体クロマトグラフィの分離カラム姿勢制御機構によれば、姿勢制御部は、恒温容器および取り付け装置の双方に対応して設けた長孔と、長孔に係合する留具とからなるため、簡易で安価な構成の姿勢制御部を用いて本発明の効果を奏することができる。
【図面の簡単な説明】
【図１】ミクロＨＰＬＣの分離カラムの出口配管の端部自体をフローセルとして吸光光度検出器等に接続した状態を説明するための図である。
【図２】本実施の形態例に係る分離カラム姿勢制御機構を備えたＨＰＬＣの概略構成を示す図である。
【図３】本実施の形態例に係るＨＰＬＣの、分離カラムを収容した恒温容器の概略断面図である。
【図４】本実施の形態例に係るＨＰＬＣの概略斜視図である。
【図５】図４中、矢印Ｖ１方向からみたＨＰＬＣの一部省略して示す概略側面図である。
【図６】図４中、矢印Ｖ２方向からみたＨＰＬＣの一部省略して示す概略側面図である。
【図７】図４中、矢印Ｖ３方向からみたＨＰＬＣの一部省略して示す概略平面図である。
【図８】本実施の形態例に係るＨＰＬＣの第１実施例の概略構成を示す図である。
【図９】本実施の形態例に係るＨＰＬＣの第２実施例の概略構成を示す図である。
【図１０】第２実施例のＨＰＬＣを用いて測定して得たクロマトグラムを示すグラフ図である。
【符号の説明】
１０　ＨＰＬＣ
１２、８６　ポンプ
１４　自動試料注入器
１６　ミクロカラム
１８　検出器
２０　容器
２２、２４、３６、３８、４１　配管
２５、３９　ねじ
２６　恒温容器
２８　取り付け装置
４０、８０　検出部
４２、５６　筐体
４２ａ、４２ｂ　筐体半体
４４ａ、４４ｂ　ブロック半体
５４　ヒータ
５８　スプリット機構
６０　調整板
６１　固定板
６２、６４、６６、６８、７０、７２スリット
７４ａ、７４ｂ、７４ｃ、７４ｄ　ねじ部材
７６　質量分析計
７８、８４　装置本体
８２　ＵＶ分析計[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to liquid chromatography, and more particularly to a connection structure between a separation column and a peripheral device.
[0002]
[Prior art]
Liquid chromatography (hereinafter abbreviated as HPLC) includes a liquid sending pump for sending an eluent, a sample injector for injecting a sample, a separation column for separating a substance, and a detector for detecting the separated substance. And the inlet of the separation column are connected by an inlet pipe, and the outlet of the separation column and the detector are connected by an outlet pipe. HPLC is widely used as a means of separating and quantifying chemical substances. If necessary, the sample may be directly injected into the separation column using a syringe without using a sample injector.
[0003]
Generally, temperature control is important not only in HPLC but also in chromatography. By increasing the temperature, a large number of theoretical plates can be obtained, the peak resolution can be improved, and the viscosity of the liquid decreases, so that the treatment can be performed at a low pressure. This means that a change in the temperature during processing has a significant effect on the measurement accuracy (accurately, the reproducibility), especially in the reverse phase mode or the ion exchange mode.
[0004]
For this reason, in the HPLC, in order to suppress the temperature change of the separation column within about ± 0.1 ° C., the separation column is usually housed in a column constant temperature bath such as a constant temperature water bath, a hot water jacket, a circulating air bath, and the like. It is to be noted that the provision of a column thermostat is optional according to JIS regulations.
[0005]
Depending on the inner diameter of the separation column to be used, HPLC is, for example, general-purpose HPLC using a general-purpose column having an internal diameter exceeding 3 mm, semi-micro HPLC using a semi-micro column having an internal diameter of 1 to 3 mm, and micro-HPLC using a micro column having an internal diameter of less than 1 mm. It can be classified into three types.
[0006]
The inlet pipe connecting the sample injector and the inlet of the separation column and the outlet pipe connecting the outlet of the separation column and the detector have inner diameters corresponding to the dimensions of the separation column.
[0007]
These inlet pipes and outlet pipes are selected from various kinds of materials, such as resins and metals, having flexibility to some extent, depending on the conditions of use. The inlet and outlet pipes and the separation column are connected and fixed using connection members such as screws and unions.
[0008]
In this case, when the separation column is accommodated in the column thermostat as described above, the posture of the separation column is fixed substantially uncontrollably. For this reason, when connecting a separation column to a device such as a detector, not only the layout of each device is devised, but also the inlet piping and the like are bent and connected to the device according to the relative arrangement of each device. In addition, it is necessary to form an inlet pipe or the like with a plurality of pipe sections and connect the respective pipe sections with connecting members. In addition, without using these connection methods, the separation column is also set up on a stand and connected to each device by piping while changing the posture of the separation column. However, in this case, since a column thermostat is not provided, a problem in measurement accuracy due to a change in room temperature is included as described above.
[0009]
In the case of general-purpose HPLC, it can be appropriately selected from the above connection methods and adopted.
[0010]
On the other hand, in the case of the micro HPLC, since the flow rate of the liquid flowing through the inlet pipe and the outlet pipe is extremely small, about 1/100 to 1/200 of that of the general-purpose HPLC, especially in the case of the outlet pipe, a joint is provided in the pipe. This causes a stagnation of the liquid at the joint, greatly affecting the measurement accuracy. In addition, since the inlet pipe and the outlet pipe use a pipe having a fine diameter corresponding to the size of the micro separation column, it is actually difficult to add a bending operation to the pipe. In the case of micro HPLC, if the outlet pipe has a long spiral flow path, the peak of the chromatogram becomes broad, resulting in a decrease in measurement accuracy.
[0011]
By the way, when a general-purpose detector such as an absorbance detector or a fluorescence detector is used as a detector, it is necessary to provide a cell for transmitting light in a form corresponding to the type of the detector. In this case, for general-purpose HPLC, an outlet pipe can be connected to a cell provided in the detector. On the other hand, micro HPLC cannot take measures such as providing a connection pipe between the outlet pipe and the detector or replacing the outlet pipe from the viewpoint of avoiding stagnation of the liquid as described above. Therefore, for example, as shown in FIG. 1, it is necessary to use the end itself of the outlet pipe 1 as a flow cell. In addition, when using a mass spectrometer as a detector in micro HPLC, it is necessary to process the end of the outlet pipe into a nozzle shape in order to vaporize and introduce the liquid in the outlet pipe into the ionization chamber of the mass spectrometer. It is.
[0012]
For these various reasons, as the material for the outlet piping of the micro HPLC, metals and resins that are generally opaque and relatively complicated to process are rarely used, and have a seamless and substantially straight shape. It is common to use a single fused silica capillary tube. This capillary tube made of fused silica is formed with high processing accuracy by optical fiber manufacturing technology, and has uniform optical characteristics in each part. The outlet pipe 1 shown in FIG. 1 is a fused silica capillary pipe having a structure in which a fused silica glass pipe 2 is coated with a polyimide layer 3 as a protective layer. As shown in FIG. 1, in order to attach the outlet pipe 1 to the holder 4 of the detector, the polyimide layer 3 in a portion of the outlet pipe 1 used as a flow cell is peeled off to expose a transparent fused silica glass tube 2, and the portion is removed. After being heated and bent into a predetermined shape, it is attached to the holder 4.
[0013]
In addition, as a material of the inlet pipe, a PEEK (polyether ether ketone) resin or the like can be used.
[0014]
[Problems to be solved by the invention]
However, in the case of the general-purpose HPLC, when connecting the inlet pipe and the outlet pipe to each device as described above, there is a large degree of freedom in selecting a pipe material and processing the pipe, but the pipe may be bent and connected. In addition, it is complicated to use connection pipes. In addition, when fused silica glass is used as a piping material, bending processing is limited even if the degree is different.
[0015]
On the other hand, in the case of micro HPLC, as described above, at least the outlet pipe uses a seamless, substantially straight fused silica capillary pipe, so that the outlet pipe is connected to each device. Can not be done easily. For this reason, as a second best measure, allowing the influence on the measurement accuracy due to temperature change, as described above, without storing the separation column in the column constant temperature bath, standing the separation column on a stand, etc. The actual situation is that the piping and each device are connected while changing the position of the separation column below.
[0016]
The present invention has been made in view of the above problems, and is directed to a liquid chromatography (HPLC) that can easily perform a connection operation when connecting a temperature-controlled separation column and each device using piping. An object of the present invention is to provide a separation column attitude control mechanism.
[0017]
[Means for Solving the Problems]
The separation column attitude control mechanism of the liquid chromatography according to the present invention includes a liquid sending pump for sending an eluent, a sample injector for injecting a sample, a separation column for separating a substance, and a detector for detecting the separated substance, and the sample In a liquid chromatography in which an inlet is connected between an injector and an inlet of the separation column by an inlet pipe, and an outlet of the separation column and the detector are connected by an outlet pipe, a constant temperature vessel provided with a heater in the separation column. And a posture control unit that controls the posture of the separation column one-dimensionally or three-dimensionally by controlling the posture of the thermostatic container.
[0018]
Further, in the separation column attitude control mechanism of the liquid chromatography according to the present invention, an attachment device for attaching the thermostatic container is provided, and the attitude control unit is configured to control the attitude of the thermostatic container with respect to the attachment device. It is characterized by the following.
[0019]
Thus, when the separation column whose temperature is controlled is connected to each device, the connection operation can be easily performed by changing the posture of the separation column.
[0020]
In this case, when the posture control unit includes a long hole provided for both the constant temperature container and the mounting device, and a fastener engaging with the long hole, the posture control unit moves the fastener in the long hole. Thereby, the thermostatic container can be displaced, and the effects of the present invention can be achieved using the posture control unit having a simple and inexpensive configuration.
[0021]
At this time, one-dimensional to three-dimensional attitude control can be performed by appropriately adjusting the mounting positions of one to three sets of the long holes and the fasteners as design conditions. In the present invention, the attachment device may include an apparatus main body and an intermediate member to which the thermostatic container is directly fixed. In this case, the elongated hole is formed through the intermediate member having the elongated hole. The constant temperature container is attached to the apparatus main body by inserting and fixing the fastener to the apparatus main body. The fastener can be appropriately selected and used from various fastening members such as bolts and nuts. Also, it is easily understood by those skilled in the art that the attitude control unit is not limited to the above-described one and various types such as a gear structure can be adopted in accordance with the gist of the present invention.
[0022]
Further, in this case, when the separation column is a micro column and the outlet pipe is a seamless, substantially straight fused silica capillary tube, the effects of the present invention can be more suitably achieved. Can be.
[0023]
BEST MODE FOR CARRYING OUT THE INVENTION
A preferred embodiment (hereinafter, referred to as an embodiment) of a separation column attitude control mechanism for liquid chromatography according to the present invention will be described below with reference to the drawings.
[0024]
First, the overall configuration and operation of a liquid chromatography (hereinafter, referred to as HPLC) having a separation column attitude control mechanism according to the present embodiment will be described with reference to FIG.
[0025]
The HPLC 10 includes a pump (liquid sending pump) 12, an automatic sample injector (sample injector) 14, a microcolumn (separation column) 16, and a detector 18.
[0026]
The pump 12 is for sending an eluent, that is, a liquid serving as a mobile phase (hereinafter, simply referred to as a mobile phase). The capacity of the pump 12 is, for example, a liquid sending amount of about 1 to 3000 μL / min and a discharge pressure of about 0 to 35 MPa. A container 20 storing the mobile phase is connected to a suction side of the pump 12 by a pipe 22 made of, for example, polytetrafluoroethylene.
[0027]
The automatic sample injector 14 is for injecting into the microcolumn 16 a sample prepared by dissolving a liquid to be measured in a split mobile phase described later. The automatic sample injector 14 has an injection volume of, for example, about 0.1 to 80 μL / min.
[0028]
The micro column 16 is, for example, Capcell Pak C18 MG 5μ (“Capcell Pak” manufactured by Shiseido is a registered trademark), and has an inner diameter of 0.5 mm and a length of 150 mm. The inlet side of the microcolumn 16 and the automatic sample injector 14 are connected by a fused silica glass pipe (inlet pipe) 24 shown in the conventional example. The pipe 24 has, for example, an inner diameter of 75 μm and an outer diameter of 375 μm. The connection between the microcolumn 16 and the pipe 24 (end fitting of the column) is performed by a screw 25.
[0029]
The microcolumn 16 is housed in a thermostat (constant temperature chamber) 26, and the thermostat 26 is attached to a mounting device 28. The structure of the constant temperature container 26 and the structure for attaching the constant temperature container 26 to the attachment device 28 will be described later.
[0030]
The external dimensions of the housing of the mounting device 28 are, for example, 58 cm in length, 21 cm in width, and 46 cm in height. The mounting device 28 is provided with three ports 30, 32, 34, of which port 30 is the outlet for the split mobile phase and port 32 is the inlet for the mobile phase before splitting. The port 34 is an outlet for the surplus mobile phase after splitting. The port 30 and the automatic sample injector 14 are connected by a pipe 36 made of, for example, PEEK having, for example, an inner diameter of 0.065 mm and an outer diameter of 1.59 mm. The port 32 and the pump 12 are connected by a pipe 38 made of, for example, PEEK having an inner diameter of 0.25 mm and an outer diameter of 1.59 mm. The excess mobile phase from port 34 is processed by any suitable means. The ports 30, 32, and 34 are respectively connected to a split mechanism 60 provided in the mounting device 28 by piping (not shown) (see FIG. 5). The mobile phase sent from the pump 12 is precisely split by the split mechanism 60 at, for example, a split ratio of 1/50.
[0031]
In this case, the detector 18 is a mass spectrometer and includes a detection unit 40 including an ionization chamber. The detection section 40 and the outlet of the microcolumn 16 are connected by a pipe (outlet pipe) 41 made of fused silica glass, similarly to the case of the inlet of the microcolumn 16. The pipe 41 has, for example, an inner diameter of 75 μm and an outer diameter of 375 μm. The connection between the microcolumn 16 and the pipe 41 is made using a screw 39 as in the case of the inlet of the microcolumn 16.
[0032]
The constant temperature container 26 and a structure for attaching the constant temperature container 26 to the attachment device 28 will be described below.
[0033]
First, the structure of the thermostatic container 26 will be described with reference to FIG.
[0034]
The constant temperature container 26 has two housing halves 42a and 42b made of, for example, metal engaged on one side, and forms the rectangular parallelepiped housing 42 by closing the housing halves 42a and 42b. . The outer dimensions of the housing 42 are, for example, 6 cm in length (T1), 6 cm in width (Y1), and 23 cm in height (H1). In the housing 42, two aluminum block halves 44a and 44b are arranged corresponding to the housing halves 42a and 42b. Each of the block halves 44a, 44b has outer wall portions 46a, 46b, 48a, 48b opposed to both ends in the longitudinal direction, and has partition wall portions 50a, 50b, 52a, 52b opposed inside. By closing the block halves 44a and 44b, the outer wall portions 46a and 48a, 46b and 48b and the partition wall portions 50a and 52a, 50b and 52b come into contact with each other, and 3 Spaces A1, A2, A3 divided into chambers are formed. A belt-shaped heater 54 is attached to the outer periphery of the block half 44b.
[0035]
Inside each of the closed block halves 44a and 44b of the thermostatic container 26, the three micro columns 16 are supported by the partition walls 50a and 52a and 50b and 52b, and the three micro columns 16 are arranged in the lateral (Y1) direction of the housing 42. Can be installed in parallel. First, the microcolumn 16 is disposed, for example, in a state supported by the outer wall portions 48a, 48b. Thereafter, the pipes 24, 41 are connected and fixed to both ends of the microcolumn 16 by screws 25, 39. At this time, the connection work of the pipes 24 and 41 can be easily performed due to the presence of the spaces A1 and A3.
[0036]
The constant temperature container 26 is PID controlled by a control device (not shown) to a predetermined temperature within a temperature range of 5 to 75 ° C. higher than room temperature.
[0037]
Next, an attachment structure of the constant temperature container 26 to the attachment device 28 will be described with reference to FIGS.
[0038]
The mounting device 28 has a rectangular parallelepiped housing 56 made of, for example, metal. The outer dimensions of the housing 56 are, for example, 39 cm in length (T2), 12 cm in width (Y2), and 45 cm in height (H2). The split mechanism 58 described above is accommodated in a lower portion of the housing 56.
[0039]
The constant temperature container 26 is movably attached to the attachment device 28 via the adjustment plate 60. Note that a fixed plate 61 is provided between the thermostatic container 26 and the adjustment plate 60.
[0040]
The adjustment plate 60 is a thin metal plate having an angled shape, for example. The adjustment plate 60 is arranged so as to cover a part of the upper surface and one side surface of the mounting device 28 in FIG. The depth dimension L1 covering the upper surface of the mounting device 28 of the adjustment plate 60 is a predetermined length sufficient to allow the constant temperature container 26 to be able to move a predetermined distance in the horizontal direction (depth direction) in FIG. A portion covering one side surface of the mounting device 28 of the adjustment plate 60 has a height L2 having a predetermined length sufficient to allow the constant temperature container 26 to be vertically moved a predetermined distance by a method described later in FIG. It is. The width of the preparation plate 60 (the size in the left-right direction in FIG. 6) is formed to be substantially the same as the width (Y2) of the housing 56 of the mounting device 28. A single slit (long hole) 62 is formed in a portion of the adjustment plate 60 that covers the upper surface of the mounting device 28, and corresponding to the slit 62, the upper surface of the mounting device 28 has the same center as the slit 62. A slit 64 is formed on the line. On the other hand, two slits (long holes) 66, 68 extending in the height direction (the direction of the height dimension L2) are provided in a portion covering one side surface of the mounting device 28 of the adjustment plate 60, on both sides in the width direction in FIG. It is formed parallel to the vicinity.
[0041]
The fixed plate 61 is a rectangular thin plate made of, for example, a metal, and has a width dimension larger than the width Y1 dimension of the constant temperature container 26 in FIG. At the same time, the height dimension is formed to be approximately the same as the height H1 dimension of the thermostatic container 26. In the vicinity of both sides of the fixing plate 61 in the width direction in FIG. 6, two slits 70 and 72 having the same center line as the slits 66 and 68 are formed corresponding to the slits 66 and 68 of the adjustment plate 60. ing.
[0042]
The constant temperature container 26 is fixed to a center position in the width direction of the fixing plate 61 in FIG. 6 using a fastening member (not shown). In this state, slits (long holes) 70 and 72 are exposed on both sides in the width direction of the fixed plate 61 with the constant temperature container 26 interposed therebetween.
[0043]
The adjusting plate 60 is attached to the attaching device 28 by engaging the screw members (fastenings) 74a and 74b with the slits 62 and 64, while the thermostatic container 26 is configured to slit the screw member (fastening) 74c. By engaging with the slit 66 and the slit 70 and the screw member (fastener) 74d with the slit 68 and the slit 72, respectively, it is attached to the attaching device 28 via the fixing plate 61 and the adjusting plate 60.
[0044]
By adjusting the engagement position between each screw member and each slit in a state where the constant temperature container 26 is attached to the attachment device 28, the constant temperature container 26 is three-dimensionally attached to the attachment device 28 as described later in a specific example. The posture can be freely controlled in the direction. In other words, the attitude of the microcolumn 16 housed in the thermostatic container 26 can be freely controlled in the three-dimensional direction with respect to the mounting device 28. That is, each screw member and each slit attached to the constant temperature container 26, the attachment device 28, and the like constitute an attitude control unit of the present invention.
[0045]
When it is not necessary to provide the thermostatic vessel 26 so as to be movable in the three-dimensional direction, for example, the screw members and the slits provided on the upper surface of the mounting device 28 of the adjustment plate 60 are omitted, and appropriate fastening is performed. The adjusting plate 60 can be fixed to the mounting device 28 using a member, or the configuration of each screw member and each slit on one side of the mounting device 28 of the adjusting plate 60 can be changed, for example, by one screw member and It can be changed as appropriate, for example, by providing only one slit.
[0046]
Next, two embodiments of a method of controlling the attitude of the separation column when connecting the separation column to various detectors and a method of connecting the detector and the separation column will be described with reference to FIGS. 8 and 9.
[0047]
In the first embodiment, as shown in FIG. 8, a mass spectrometer 76 is used as a detector.
[0048]
The mass spectrometer 76 includes an apparatus main body 78 and a detection unit 80. The pipe 41 attached to the outlet side of the separation column is connected to the detection unit 80. The pipe 24 attached to the inlet side of the separation column is connected to the automatic sample injector 14 as described above.
[0049]
At this time, in a state where the mass spectrometer 76 is arranged on the machine side of the attachment device 28 to which the constant temperature vessel 26 is attached, the length of the pipe 41 is minimized and the connection operation of the pipe 41 is operated. The posture control unit controls the posture of the constant temperature container 26 so that the posture can be performed easily.
[0050]
That is, for example, the screw members 74c and 74d are loosened from the initial state in which the constant temperature container 26 stands upright on the base (not shown) together with the mounting device 28 shown in FIG. Then, while moving the screw members 74c and 74d in the respective slits 66 and 70 and the slits 68 and 72, the constant temperature container 26 is moved with respect to the mounting device 28 to position the constant temperature container 26 in a desired posture. I do. Finally, the screw members 74c and 74d are tightened again with the constant temperature container 26 positioned, and the constant temperature container 26 is fixed to the mounting device 28. In this case, the posture of the thermostatic container 26 is controlled two-dimensionally. However, if necessary, the screw members 74c and 74d are further loosened to adjust the mounting position, so that the posture of the thermostatic container 26 is three-dimensionally controlled. It may be controlled.
[0051]
Next, in the second embodiment, as shown in FIG. 9, a UV analyzer 82 is used as a detector. In FIG. 9, a part of the display, such as the attitude control unit, is omitted.
[0052]
The UV analyzer 82 includes an apparatus main body 84 having a detection unit (not shown) and a pump 86. The UV analyzer 82 is arranged, for example, on the machine side of the mounting device 28 opposite to the mass spectrometer 76 with the mounting device 28 interposed therebetween. The pipe 41 attached to the outlet side of the separation column is fixed by rotating the thermostatic container 26 by about 90 ° counterclockwise from the state of FIG. 8 by the same method as that described in the first embodiment. . Then, the pipe 41 attached to the outlet side of the separation column is connected to the detection unit of the apparatus main body 84.
[0053]
According to the first and second embodiments described above, the attitude of the separation column is changed one-dimensionally or three-dimensionally by using the attitude controller having a simple and inexpensive configuration, so that the temperature-controlled separation column and each device can be changed. Connection work with the device can be easily performed.
[0054]
Also, the connection operation can be suitably performed using a single, substantially straight fused silica capillary tube.
[0055]
Next, an example of a measurement result by HPLC using a UV analyzer as a detector provided with the separation column attitude control mechanism according to the present embodiment will be described with reference to FIG.
[0056]
The measurement conditions are as follows.
[0057]

From the chromatogram shown in FIG. 10, it can be seen that data with excellent reproducibility was obtained for all of the three samples.
【The invention's effect】
According to the separation column attitude control mechanism of the liquid chromatography according to the present invention, a liquid sending pump for sending an eluent, a sample injector for injecting a sample, a separation column for separating a substance, a detector for detecting the separated substance, In liquid chromatography in which a sample injector and an inlet of the separation column are connected by an inlet pipe and an outlet of the separation column and a detector are connected by an outlet pipe, in a liquid chromatography, a separation column is provided inside a thermostatic vessel equipped with a heater. And a posture control unit that controls the posture of the separation column one-dimensionally to three-dimensionally by controlling the posture of the thermostatic container, and also has a separation column posture control mechanism for liquid chromatography according to the present invention. , Comprising a mounting device for mounting the thermostatic container, wherein the posture control unit controls the posture of the thermostatic container with respect to the mounting device. To become Te, when connecting the separation column and the devices that are temperature controlled, by changing the attitude of the separation column, it is possible to easily perform the connection work.
[0058]
Further, according to the separation column posture control mechanism of the liquid chromatography according to the present invention, the posture control unit includes a long hole provided corresponding to both the constant temperature container and the mounting device, and a fastener engaging with the long hole. Therefore, the effects of the present invention can be achieved by using a simple and inexpensive attitude control unit.
[Brief description of the drawings]
FIG. 1 is a diagram for explaining a state in which an end of an outlet pipe of a separation column of a micro HPLC is itself connected as a flow cell to an absorbance detector or the like.
FIG. 2 is a diagram showing a schematic configuration of an HPLC equipped with a separation column attitude control mechanism according to the present embodiment.
FIG. 3 is a schematic cross-sectional view of a thermostatic container accommodating a separation column of the HPLC according to the present embodiment.
FIG. 4 is a schematic perspective view of an HPLC according to the present embodiment.
FIG. 5 is a schematic side view showing a part of the HPLC as viewed from the direction of arrow V1 in FIG. 4;
FIG. 6 is a schematic side view showing a part of the HPLC as viewed in the direction of arrow V2 in FIG. 4;
FIG. 7 is a schematic plan view showing a part of the HPLC viewed from the direction of arrow V3 in FIG. 4;
FIG. 8 is a diagram showing a schematic configuration of a first example of the HPLC according to the present embodiment.
FIG. 9 is a diagram showing a schematic configuration of a second example of the HPLC according to the present embodiment.
FIG. 10 is a graph showing a chromatogram obtained by using the HPLC of the second example.
[Explanation of symbols]
10 HPLC
12, 86 Pump 14 Automatic sample injector 16 Micro column 18 Detector 20 Vessel 22, 24, 36, 38, 41 Piping 25, 39 Screw 26 Thermostatic vessel 28 Mounting device 40, 80 Detector 42, 56 Housing 42a, 42b Housing halves 44a, 44b Block halves 54 Heater 58 Split mechanism 60 Adjustment plate 61 Fixing plates 62, 64, 66, 68, 70, 72 Slits 74a, 74b, 74c, 74d Screw member 76 Mass spectrometer 78, 84 Apparatus Main unit 82 UV analyzer

Claims (4)

Equipped with a liquid sending pump for sending an eluent, a sample injector for injecting a sample, a separation column for separating a substance, and a detector for detecting the separated substance, and an inlet pipe is provided between the sample injector and an inlet of the separation column. And in liquid chromatography in which the outlet of the separation column and the detector are connected by an outlet pipe, respectively.
The separation column is housed inside a thermostat provided with a heater,
A separation column attitude control mechanism for liquid chromatography, comprising: an attitude control unit that controls the attitude of the separation column one-dimensionally to three-dimensionally by controlling the attitude of the thermostatic vessel. Comprising a mounting device for mounting the thermostatic container,
The separation column attitude control mechanism for liquid chromatography according to claim 1, wherein the attitude control section is configured to control the attitude of the thermostatic container with respect to the mounting device. 3. The liquid chromatography apparatus according to claim 2, wherein the attitude control unit includes a long hole provided corresponding to both the thermostatic container and the mounting device, and a fastener engaging with the long hole. 4. Separation column attitude control mechanism. The said separation column is a micro column, The said outlet piping is a seamless and substantially straight-shaped one capillary tube made of fused silica, The Claims characterized by the above-mentioned. Attitude control mechanism for liquid chromatography separation column.

Images