JP7081136B2 - Liquid mixer - Google Patents

Liquid mixer Download PDF

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JP7081136B2
JP7081136B2 JP2017240685A JP2017240685A JP7081136B2 JP 7081136 B2 JP7081136 B2 JP 7081136B2 JP 2017240685 A JP2017240685 A JP 2017240685A JP 2017240685 A JP2017240685 A JP 2017240685A JP 7081136 B2 JP7081136 B2 JP 7081136B2
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mixing device
liquid
recess
mixing
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JP2019109079A (en
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達也 生井
寛人 久保田
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Tosoh Corp
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本発明は、異なる液体を混合する混合装置及び前記混合装置が流路に組み込まれている液体クロマトグラフ用の送液システムに関するものである。 The present invention relates to a mixing device for mixing different liquids and a liquid feeding system for a liquid chromatograph in which the mixing device is incorporated in a flow path.

液体クロマトグラフでは、異なる液体を均一に混合するための混合装置が色々な場面で使用される。例えば、異なる濃度又は組成の溶離液を制御された割合で混合してカラムに供給する場面、濃縮された溶離液に希釈水をオンラインで混合して調整した溶離液をカラムに供給する場面、カラムからの溶出液に反応試薬を混合してポストカラム反応を起こす場面等で、混合装置は重要な役割を果たす。この混合装置には、撹拌子等の可動部を持つダイナミックミキサーや可動部を持たないスタティックミキサーがある。スタティックミキサーは、ダイナミックミキサーと比べて安価であり、流路管内径を小さくした後に大径部に噴射させるタイプの混合装置（例えば、特許文献１参照）や、複雑な流路を構成し、液体に回転運動を与えて混合する混合装置（例えば、特許文献２参照）等がある。 In a liquid chromatograph, a mixing device for uniformly mixing different liquids is used in various situations. For example, a scene in which eluents of different concentrations or compositions are mixed at a controlled ratio and supplied to the column, a scene in which diluted water is mixed online with a concentrated eluent and a prepared eluate is supplied to the column, a column. The mixing device plays an important role in a situation where a reaction reagent is mixed with the eluate from the water to cause a post-column reaction. This mixing device includes a dynamic mixer having a moving part such as a stirrer and a static mixer having no moving part. The static mixer is cheaper than the dynamic mixer, and has a mixing device of a type in which the inner diameter of the flow path tube is reduced and then injected into a large diameter portion (see, for example, Patent Document 1), or a complicated flow path is formed and a liquid is formed. There is a mixing device (see, for example, Patent Document 2) that applies a rotational motion to the mixture to mix the mixture.

しかしながら、特許文献１に記載されたような同軸上で内径を変化させた混合装置では、大径部に噴射させた際に混合装置内部の端部に密度の大きい液体の一部が溜まり、均一に混合されない場合や液体中に含まれていた気泡が端部に引っ掛かって残る場合があった。また、特許文献２に記載されたような混合装置では、液体に回転運動を与えるために密度の大きい液体の一部が溜まる可能性は低いものの、非常に複雑な流路であるために圧力損失も大きく、液体中に含まれていた気泡が複雑な流路の途中で引っ掛かって残ってしまう場合があった。 However, in the mixing device whose inner diameter is changed coaxially as described in Patent Document 1, a part of the liquid having a high density is accumulated at the end inside the mixing device when the liquid is sprayed onto the large diameter portion, and the liquid is uniform. In some cases, it was not mixed with the liquid, or air bubbles contained in the liquid were caught on the edges and remained. Further, in a mixing device as described in Patent Document 2, although it is unlikely that a part of a liquid having a high density is accumulated in order to give a rotational motion to the liquid, the pressure loss is due to a very complicated flow path. In some cases, the bubbles contained in the liquid were caught in the middle of the complicated flow path and remained.

特開２００５－６９８１８号公報Japanese Unexamined Patent Publication No. 2005-69818 特開２００８－１２４５３号公報Japanese Unexamined Patent Publication No. 2008-12453

本発明の目的は、製造コストを抑えながらも混合装置内部に密度の大きい液体の一部が溜まらず、液体中の気泡が内部に残存しづらく、さらには圧力損失の小さい混合装置を提供することである。 An object of the present invention is to provide a mixing device in which a part of a liquid having a high density does not accumulate inside the mixing device while suppressing the manufacturing cost, bubbles in the liquid are hard to remain inside, and the pressure loss is small. Is.

上記問題を解決するために、本発明者らは液体の流入方向及び流出方向に着目し、本発明を完成させるに至った。 In order to solve the above problems, the present inventors have focused on the inflow direction and the outflow direction of the liquid, and have completed the present invention.

すなわち、本発明は、
円柱状の凹部を有し、液体の流入方向が前記凹部の底面及び側面に沿った方向となるような流入口が前記凹部の側面に設けられた第１の部材と、
円錐状の凹部を有し、液体の流出口が円錐の頂点の位置に設けられた第２の部材と、を備え、
前記第１の部材と前記第２の部材は互いの凹部を対向させるようにして接合されていることを特徴とする混合装置である。 That is, the present invention
A first member having a columnar recess and having an inflow port provided on the side surface of the recess so that the inflow direction of the liquid is along the bottom surface and the side surface of the recess.
A second member having a conical recess with a liquid outlet at the apex of the cone.
The mixing device is characterized in that the first member and the second member are joined so that their recesses face each other.

本発明の混合装置は前記第１の部材の凹部の縁と、前記第２の部材の凹部の縁との間にＯリングを介して接合されていてもよい。また、前記第１の部材と前記第２の部材との接合態様は互いの凹部を対向させるための嵌合部を設ける、ネジ止めまたはクランプ止めにより接合するといった態様が可能である。 The mixing device of the present invention may be joined via an O-ring between the edge of the recess of the first member and the edge of the recess of the second member. Further, the joining mode of the first member and the second member can be such that a fitting portion for facing each other's recesses is provided, or the first member and the second member are joined by screwing or clamping.

また、本発明の混合装置は複数用いて、一つの混合装置における前記流出口に、流路を介して他の混合装置における前記流入口を接続する態様で直列接続してもよい。 Further, a plurality of mixing devices of the present invention may be used and connected in series to the outlet in one mixing device by connecting the inlet in another mixing device via a flow path.

さらに、本発明の混合装置における前記流入口に、切替弁及び／又は流路を介して溶離液タンクを接続し、前記流出口に送液ポンプを接続して液体クロマトグラフ用の送液システムとしてもよく、上述したように混合装置を複数用いた場合であっても、一端にある混合装置の前記流入口に切替弁及び／又は流路を介して溶離液タンクを接続し、他端にある混合装置の前記流出口に流路を介して送液ポンプを接続して液体クロマトグラフ用の送液システムとしてもよい。 Further, as a liquid feeding system for a liquid chromatograph, an eluent tank is connected to the inlet of the mixing device of the present invention via a switching valve and / or a flow path, and a liquid feed pump is connected to the outlet. Also, even when a plurality of mixing devices are used as described above, the eluent tank is connected to the inlet of the mixing device at one end via a switching valve and / or a flow path, and is located at the other end. A liquid feed pump may be connected to the outlet of the mixing device via a flow path to form a liquid feed system for a liquid chromatograph.

本発明の混合装置によれば、液体を効率よく混合することができ、混合装置内部に密度の大きい液体の一部が溜まりにくく、気泡も引っ掛かりにくい。また、従来の液体に回転運動を与える混合装置に比べて構造が非常に単純であり、製造コストも抑えることができる。さらには、流路径の小さい部分や複雑な流路を用いないため圧力損失も小さい。 According to the mixing device of the present invention, the liquid can be efficiently mixed, a part of the liquid having a high density is less likely to be accumulated inside the mixing device, and bubbles are less likely to be caught. In addition, the structure is very simple as compared with the conventional mixing device that gives a rotary motion to a liquid, and the manufacturing cost can be suppressed. Furthermore, the pressure loss is small because a portion having a small flow path diameter or a complicated flow path is not used.

本発明の一実施例である混合装置の内部構造を表した（a）斜視図、（ｂ）上面図、（ｃ）側面図である。It is (a) perspective view, (b) top view, (c) side view which showed the internal structure of the mixing apparatus which is one Example of this invention. 本発明の一実施例において、流入口が２つある混合装置の内部構造を表した（a）斜視図、（ｂ）上面図、（ｃ）側面図である。In one embodiment of the present invention, (a) a perspective view, (b) a top view, and (c) a side view show the internal structure of a mixing device having two inlets. 本発明の一実施例である混合装置の分解斜視図である。It is an exploded perspective view of the mixing apparatus which is an Example of this invention. 第１の部材と第２の部材の接合態様を示した図である。It is a figure which showed the joining mode of the 1st member and the 2nd member. 本発明の混合装置を備えたイオンクロマトグラフシステムの一例を説明するための図である。It is a figure for demonstrating an example of an ion chromatograph system provided with the mixing apparatus of this invention. 本発明に至る前の混合装置の内部構造を表した（a）斜視図、（ｂ）上面図、（c）側面図である。It is (a) perspective view, (b) top view, (c) side view which showed the internal structure of the mixing apparatus before leading to this invention. 混合装置を備えたイオンクロマトグラフシステムにおいて、用いた混合装置の違いによるベースラインの比較図である。It is a comparison diagram of the baseline by the difference of the mixing apparatus used in the ion chromatograph system equipped with the mixing apparatus.

以下、本発明の混合装置を備えたイオンクロマトグラフシステムについて、図面に表した形態に基づき詳細な説明を行うが、これらは本発明を限定するものではない。 Hereinafter, the ion chromatograph system provided with the mixing apparatus of the present invention will be described in detail based on the embodiments shown in the drawings, but these are not limited to the present invention.

図１（ａ）は、本発明の混合装置の内部構造斜視図であり、図１（ｂ）は上面図、図１（ｃ）は側面図である。側面部の流入口４１、円錐頂点部の流出口４３および円錐形状の内部空間４４を有している。流入口４１は、液体の流入方向が内部空間４４の底面及び側面に沿った方向となるように接続されており、これにより液体に回転運動を与えることができる。さらに、円錐形状の上部より液体が出ていくため、内部空間内に密度の大きい液体の一部が溜まりにくい構造となっており、効率よく混合でき、気泡も引っ掛かりにくい。 1 (a) is a perspective view of the internal structure of the mixing device of the present invention, FIG. 1 (b) is a top view, and FIG. 1 (c) is a side view. It has an inlet 41 on the side surface, an outlet 43 on the apex of the cone, and an internal space 44 in the shape of a cone. The inflow port 41 is connected so that the inflow direction of the liquid is along the bottom surface and the side surface of the internal space 44, whereby the liquid can be given a rotational motion. Further, since the liquid is discharged from the upper part of the conical shape, a part of the liquid having a high density does not easily collect in the internal space, so that the liquid can be mixed efficiently and bubbles are not easily caught.

図２（ａ）は、本発明の混合装置において流入口が２つある混合装置の内部構造斜視図であり、図２（ｂ）は上面図、図２（ｃ）は側面図である。流入口４１および４２は、共に液体の流入方向が内部空間４４の底面及び側面に沿った方向となるように接続されており、同様に液体に回転運動を与えることができ、２種類の液体を混合するのに好適である。３種類以上の液体を混合する際にも同様に３つの流入口を設ければ良い。流入口が１つの場合であっても切替弁を介して２種類以上の液体を混合することが可能であることは言うまでもない。 2A is a perspective view of the internal structure of the mixing device having two inlets in the mixing device of the present invention, FIG. 2B is a top view, and FIG. 2C is a side view. The inflow ports 41 and 42 are both connected so that the inflow direction of the liquid is along the bottom surface and the side surface of the internal space 44, and similarly, the liquid can be given a rotational motion, and two types of liquid can be transferred. Suitable for mixing. Similarly, when mixing three or more kinds of liquids, three inlets may be provided. Needless to say, even when there is only one inflow port, it is possible to mix two or more kinds of liquids through the switching valve.

図３は、本発明の混合装置の分解斜視図である。本発明の混合装置は、図の様に単純に２つの部品（第１の部材、第２の部材）より構成されており、互いの凹部を対向させるようにして接合すれば問題ない。例えば、図３の態様では、第１の部材に嵌合用の凹部を形成し、第２の部材に嵌合用の凸部を形成し、内部空間を形成するための凹部をその嵌合用の凹部、凸部にそれぞれ形成している。このように、それぞれの部材に嵌合用の凹部、凸部を形成して、嵌め合うことで１つの混合装置となるため、高い加工精度も必要無く、流路も複雑ではない。そのため製造コストが高くならず、また圧力損失も小さいことが分かる。 FIG. 3 is an exploded perspective view of the mixing device of the present invention. As shown in the figure, the mixing device of the present invention is simply composed of two parts (first member and second member), and there is no problem as long as the recesses face each other and are joined. For example, in the embodiment of FIG. 3, a concave portion for fitting is formed in the first member, a convex portion for fitting is formed in the second member, and a concave portion for forming an internal space is a concave portion for fitting. It is formed on each convex part. In this way, by forming concave portions and convex portions for fitting in each member and fitting them into one mixing device, high processing accuracy is not required and the flow path is not complicated. Therefore, it can be seen that the manufacturing cost is not high and the pressure loss is small.

第１の部材と第２の部材の接合態様としては前述したように、嵌合用の凹部、凸部を内部空間を形成するための凹部がある場所に形成する（図４（ａ）参照）他にも、内部空間を形成するための凹部がある場所以外に嵌合用の凹部、凸部を形成する（図４（ｂ）参照）、一方の凹部以外の位置に２以上の貫通穴を設け、他方の部材に前記貫通穴と位置合わせされた貫通していない穴を有しており、前記貫通穴と前記貫通していない穴をネジ止めする（図４（ｃ）参照）等であっても問題はない。また、第１の部材と第２の部材の接合態様として、間にＯリングを介して（図４（ｄ）参照）、ネジやクランプを用いて止めても問題はない。 As a mode of joining the first member and the second member, as described above, a concave portion for fitting and a convex portion are formed in a place where there is a concave portion for forming an internal space (see FIG. 4A) and the like. Also, a recess for fitting and a convex portion are formed in a place other than the place where there is a concave portion for forming an internal space (see FIG. 4 (b)), and two or more through holes are provided at positions other than one concave portion. Even if the other member has a non-penetrating hole aligned with the through hole and the through hole and the non-penetrating hole are screwed together (see FIG. 4C). No problem. Further, as a mode of joining the first member and the second member, there is no problem even if the first member and the second member are stopped by using an O-ring (see FIG. 4D) and a screw or a clamp.

部材の材質は、金属、樹脂等と特に制限は無いが、化学的に不活性な材質が求められ、アセトニトリル等の一部の有機溶媒を使用するイオンクロマトグラフにおいては、ポリテトラフルオロエチレンやポリエーテルエーテルケトンの様な、化学的に不活性で且つ耐溶媒性の高い樹脂が好ましい。凹部の容量については、特に制限するものでは無いが、一定の間隔で異なる液体を繰り返し切替えて送液するようなケースにおいては、繰り返す容量の２～３倍程度の容量であることが好ましい。なお、部材の形状は、円柱、三角柱、四角柱等と特に制限は無いが、部材側面が曲面となるような形状の場合は、加工時の液体入口の位置ずれを防ぐために流入口付近は平面状に切り出しておくことが好ましい。 The material of the member is not particularly limited to metal, resin, etc., but a chemically inert material is required, and in an ion chromatograph using a part of organic solvent such as acetonitrile, polytetrafluoroethylene or poly A chemically inert and highly solvent resistant resin such as ether ether ketone is preferred. The capacity of the recess is not particularly limited, but in a case where different liquids are repeatedly switched and sent at regular intervals, the capacity is preferably about 2 to 3 times the repeating capacity. The shape of the member is not particularly limited to a cylinder, a triangular prism, a square prism, etc., but if the shape is such that the side surface of the member is a curved surface, the vicinity of the inflow port is flat to prevent the position of the liquid inlet during processing. It is preferable to cut it into a shape.

図５は、図１にて示した本発明の混合装置を直列に複数接続して、イオンクロマトグラフのポンプの溶離液吸引流路部に組み入れた図である。圧力損失が小さいためポンプの吸引流路部に組み入れることが可能である。 FIG. 5 is a diagram in which a plurality of mixing devices of the present invention shown in FIG. 1 are connected in series and incorporated into an eluent suction flow path portion of a pump of an ion chromatograph. Since the pressure loss is small, it can be incorporated into the suction flow path of the pump.

以下、実施例を用いて説明を行うが、本発明はこれに限定されるものではない。 Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited thereto.

図１にて示した本発明の混合装置と図６にて示した混合装置をそれぞれ２個直列にプランジャー式のポンプ吸引流路に組み入れたイオンクロマトグラフシステムを作製した。図６にて示した混合装置は、側面部の流入口４１、上部の流出口４３、３つの円筒形状を合成した内部空間４４を有している。流入口４１は、最下部の円筒中心方向へと接続されており、液体へ回転運動を与えることが難しい構造となっている。なお、図１で示した混合装置の内部空間の底面の直径は１５ｍｍ、高さは８６ｍｍ、内部空間容積は７１０μＬであり、図６にて示した混合装置の最下部と最上部の円筒の直径は６ｍｍ、中央部の円筒の直径は１２ｍｍ、全体の高さは１１ｍｍであり、内部空間容積は６８０μＬである。 An ion chromatograph system was produced in which two mixing devices of the present invention shown in FIG. 1 and two mixing devices shown in FIG. 6 were incorporated in series in a plunger-type pump suction flow path. The mixing device shown in FIG. 6 has an inflow port 41 on the side surface, an outflow port 43 on the upper side, and an internal space 44 in which three cylindrical shapes are combined. The inflow port 41 is connected toward the center of the lowermost cylinder, and has a structure in which it is difficult to give a rotational motion to the liquid. The diameter of the bottom surface of the internal space of the mixing device shown in FIG. 1 is 15 mm, the height is 86 mm, and the internal space volume is 710 μL. Is 6 mm, the diameter of the central cylinder is 12 mm, the total height is 11 mm, and the internal space volume is 680 μL.

図７は、１０倍に濃縮された溶離液と希釈用純水をプランジャー式ポンプのストローク単位にて２液を１対９の比にて交互に切替えて送液した際の電気伝導度検出器のベースラインの比較である。具体的には、１ストローク当たりに送液する容積が９．４μＬであるプランジャー式ポンプを用いて、３ストローク分１０倍に濃縮された溶離液を送液し、液体を希釈用純水に切替えた後に２７ストローク分送液することを繰り返し行った。使用した１０倍に濃縮された溶離液は、３８ｍＭ炭酸水素ナトリウムおよび３０ｍＭ炭酸ナトリウムの混合水溶液であり、流量１．５ｍＬ／ｍｉｎにて測定を行った。図６にて示した混合装置を使用したベースラインａは、１０倍に濃縮された溶離液と希釈用純水を切替えたことに由来する周期的なゆらぎが明確に残っており、混合が不十分である。それに対して、図１にて示した本発明の混合装置を使用したベースラインｂでは、１０倍に濃縮された溶離液と希釈用純水を切替えたことに由来する周期的なゆらぎがほとんど見えなくなっており、高い混合効率であることが分かる。 FIG. 7 shows the electric conductivity detection when the eluent concentrated 10 times and the pure water for dilution are alternately switched at a ratio of 1: 9 for each stroke of the plunger type pump. It is a comparison of the baseline of the vessel. Specifically, using a plunger-type pump having a volume of 9.4 μL per stroke, the eluent concentrated 10 times for 3 strokes is sent, and the liquid is converted into pure water for dilution. After switching, the liquid was repeatedly fed for 27 strokes. The 10-fold concentrated eluent used was a mixed aqueous solution of 38 mM sodium hydrogen carbonate and 30 mM sodium carbonate, and measurements were taken at a flow rate of 1.5 mL / min. In the baseline a using the mixing device shown in FIG. 6, periodic fluctuations due to switching between the eluent concentrated 10 times and the pure water for dilution clearly remain, and the mixing is not possible. It is enough. On the other hand, in the baseline b using the mixing device of the present invention shown in FIG. 1, periodic fluctuations due to switching between the eluent concentrated 10 times and the pure water for dilution can be almost seen. It has disappeared, and it can be seen that the mixing efficiency is high.

１０ タンク１（１０倍に濃縮された溶離液）
２０ タンク２（希釈用純水）
３１ 液体切替用電磁弁１
３２ 液体切替用電磁弁２
４０ 混合装置
４１ 流入口
４２ 別の流入口
４３ 流出口
４４ 混合装置内部空間
４５ 嵌合部
４６ ネジ止め部
４７ Ｏリング
５０ プランジャー式ポンプ
６０ サンプラー
７０ 分析カラム
８０ サプレッサー
９０ 電気伝導度検出器 10 Tank 1 (10-fold concentrated eluent)
20 Tank 2 (pure water for dilution)
31 Solenoid valve for liquid switching 1
32 Solenoid valve for liquid switching 2
40 Mixing device 41 Inlet 42 Another inflow port 43 Outlet 44 Mixing device internal space 45 Fitting part 46 Screwing part 47 O-ring 50 Plunger type pump 60 Sampler 70 Analytical column 80 Suppressor 90 Electrical conductivity detector

Claims (4)

円柱状の凹部を有し、液体の流入方向が前記凹部の底面及び側面に沿った方向となるような流入口が前記凹部の側面に設けられた第１の部材と、
円錐状の凹部を有し、液体の流出口が円錐の頂点の位置に設けられた第２の部材と、を備え、
前記第１の部材と前記第２の部材は互いの凹部を対向させるようにして接合されていることを特徴とする混合装置。 A first member having a columnar recess and having an inflow port provided on the side surface of the recess so that the inflow direction of the liquid is along the bottom surface and the side surface of the recess.
A second member having a conical recess with a liquid outlet at the apex of the cone.
A mixing device characterized in that the first member and the second member are joined so that their recesses face each other. 前記第１の部材の凹部の縁と、前記第２の部材の凹部の縁との間にＯリングを介して接合され、前記第１の部材と、前記第２の部材とが互いの凹部を密接対向させるための嵌合部をそれぞれ有して、前記第１の部材と前記第２の部材とがネジ止めにより接合されていることを特徴とする請求項１に記載の混合装置。 The edge of the recess of the first member and the edge of the recess of the second member are joined via an O-ring, and the first member and the second member form each other's recess. The mixing device according to claim 1 , further comprising fitting portions for closely facing each other, wherein the first member and the second member are joined by screwing . 請求項１～２のいずれかに記載の混合装置を複数備え、一つの混合装置における前記流出口に、流路を介して他の混合装置における前記流入口を接続する態様で混合装置を直列接続してなる混合装置群。 A plurality of mixing devices according to any one of claims 1 and 2 are provided, and the mixing devices are connected in series in such a manner that the inflow port in another mixing device is connected to the outlet in one mixing device via a flow path. Mixing device group. 請求項３に記載の混合装置群の一端にある混合装置の前記流入口に切替弁及び／又は流路を介して溶離液タンクを接続し、他端にある混合装置の前記流出口に流路を介して送液ポンプを接続してなる液体クロマトグラフ用の送液システム。 An eluent tank is connected to the inlet of the mixing device at one end of the mixing device group according to claim 3 via a switching valve and / or a flow path, and a flow path to the outlet of the mixing device at the other end. A liquid feeding system for liquid chromatographs that is made by connecting a liquid feeding pump via.
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JP3172222U (en) 2011-09-27 2011-12-08 株式会社島津製作所 Sample injection unit and liquid chromatograph

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JPH0250678U (en) * 1988-09-30 1990-04-09
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