JP6862765B2 - Stirring container and stirring dispenser using it - Google Patents

Stirring container and stirring dispenser using it Download PDF

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JP6862765B2
JP6862765B2 JP2016213806A JP2016213806A JP6862765B2 JP 6862765 B2 JP6862765 B2 JP 6862765B2 JP 2016213806 A JP2016213806 A JP 2016213806A JP 2016213806 A JP2016213806 A JP 2016213806A JP 6862765 B2 JP6862765 B2 JP 6862765B2
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stirring
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成治 川口
成治 川口
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本発明は、懸濁液を収容し、攪拌した状態でノズルにより吸入するのに適した攪拌容器及びそれを用いた攪拌分注装置に関する。 The present invention relates to a stirring container suitable for containing a suspension and sucking it through a nozzle in a stirred state, and a stirring dispensing device using the stirring container.

懸濁液中固形物の微量分注は、保存液中で均一濃度の懸濁状態にして所定量の懸濁液を分注するのが一般的である。生物化学や臨床化学領域において微量高感度分析に用いる試薬材料は、固定化するタンパク質や不溶性粒子が高価であるケースが多く、廃棄量を少なくし、無駄なく分注できるように、デッドボリューム率(最大投入液量に対するデッドボリュームの割合)の小さい容器が要求される。 For a small amount of solid matter in a suspension, it is common to dispense a predetermined amount of the suspension in a suspended state having a uniform concentration in the preservation solution. Reagent materials used for micro-sensitive analysis in the fields of biochemistry and clinical chemistry often have expensive proteins and insoluble particles to be immobilized, and the dead volume ratio (dead volume ratio) so that the amount of waste can be reduced and the particles can be dispensed without waste. A container with a small dead volume ratio to the maximum charge amount) is required.

前記懸濁液の攪拌は、できる限り泡立たない、緩和な条件にて行う必要があり、攪拌子を攪拌機に接続して回転攪拌する方法や、マグネット攪拌子を容器に入れてマグネチックスターラーにより回転攪拌する方法等が一般的に用いられる。攪拌子と容器内底面が干渉しないように、さらに固形物の攪拌が容易になるよう底面全体が均一な高さをもつ平底の円筒形や直方形などの容器を使用することが多いが、沈降速度の速い固形物の懸濁液においては、所定回数のノズル分注を行う間、攪拌子を常時懸濁液中に浸漬して連続的に又は間欠的に攪拌しなければならない。そのため、容器デッドボリュームは攪拌子の厚み及び攪拌子から容器内底面までの距離に大きく左右される。 It is necessary to stir the suspension under mild conditions that do not foam as much as possible, and a method of connecting the stirrer to a stirrer to rotate and stir, or putting a magnet stirrer in a container and rotating it with a magnetic stirrer. A method of stirring or the like is generally used. In many cases, a flat-bottomed cylindrical or rectangular container having a uniform height on the entire bottom surface is used so that the stirrer and the inner bottom surface of the container do not interfere with each other and the solid matter can be easily agitated. In a fast solid suspension, the stir bar must be constantly immersed in the suspension and stirred continuously or intermittently during a predetermined number of nozzle dispensings. Therefore, the container dead volume is greatly affected by the thickness of the stirrer and the distance from the stirrer to the inner bottom surface of the container.

特許文献1では、マグネット攪拌子の回転支承部と兼用するように円筒形攪拌容器の平底面の中心に凸状部を設けて、ノズル吸引時にノズルと攪拌子との当接を回避するために攪拌子停止位置をずらし、ノズルを容器内底面に近接することにより試料を無駄なく分注することが可能な攪拌容器が提案されている。しかしながら、ノズルは容器内底面に対して可及的に近接下降するように条件設定できるが、液量に関わらず常に攪拌を必要とする比重の大きな固形物の懸濁液の場合は、容器に攪拌子をセットした状態において攪拌子上端が攪拌時に露出しない水位が液面の下降限界水位となるため、デッドボリューム率の低減は困難であった。 In Patent Document 1, a convex portion is provided in the center of the flat bottom surface of the cylindrical stirring container so as to also serve as a rotary support portion of the magnet stirrer, in order to avoid contact between the nozzle and the stirrer during nozzle suction. A stirring container has been proposed in which the sample can be dispensed without waste by shifting the stirrer stop position and moving the nozzle closer to the inner bottom surface of the container. However, although the conditions can be set so that the nozzle descends as close as possible to the inner bottom surface of the container, in the case of a suspension of a solid substance having a large specific gravity that always requires stirring regardless of the amount of liquid, the container can be used. It was difficult to reduce the dead volume ratio because the water level at which the upper end of the stirrer is not exposed during stirring in the state where the stirrer is set becomes the lowering limit water level of the liquid level.

特開2005−169303号公報Japanese Unexamined Patent Publication No. 2005-169303

本発明は、液体中の固形物を攪拌子にて均一濃度の懸濁液に攪拌し、ノズル吸引により固形物を分注するために用いる攪拌容器において、デッドボリューム率を小さくした攪拌容器及びそれを用いた攪拌分注装置を提供することを目的とする。 The present invention is a stirring container used for stirring a solid substance in a liquid into a suspension having a uniform concentration with a stirrer and dispensing the solid substance by nozzle suction, the stirring vessel having a reduced dead volume ratio, and the stirring vessel. It is an object of the present invention to provide a stirring and dispensing device using.

前記目的を達成するためになされた本発明は、以下の発明を包含する:
すなわち本発明の第一の態様は、
攪拌子で回転攪拌された懸濁液を収容する攪拌容器であって、
前記攪拌容器の内底面に、前記攪拌子の攪拌時に形成する回転体の水平投影面を内包する水平投影面をもつ内底面と前記攪拌子の厚み以上の深さを有する凹部が設けられていることを特徴とする攪拌容器である。
The present invention made to achieve the above object includes the following inventions:
That is, the first aspect of the present invention is
A stirring container for containing a suspension that has been rotationally stirred with a stirrer.
The inner bottom surface of the stirring container is provided with an inner bottom surface having a horizontal projection surface including a horizontal projection surface of a rotating body formed during stirring of the stirrer and a recess having a depth equal to or greater than the thickness of the stirrer. It is a stirring container characterized by this.

また、前記攪拌容器の内底面であって前記凹部の内底面より高い位置に、略方形又は略トラック形の内底面が設けられていることが好ましく、前記凹部の略方形又は略トラック形の内底面側にある側壁部は傾斜状となっていることが好ましい。 Further, it is preferable that the inner bottom surface of the stirring container is provided at a position higher than the inner bottom surface of the recess, and the inner bottom surface of the substantially square or substantially track shape is provided. The side wall portion on the bottom surface side is preferably inclined.

また、前記凹部の傾斜状側壁部は、前記略方形又は略トラック形の内底面の長辺に対して垂直な面の少なくとも一つと重なる位置にあることが好ましく、さらに前記傾斜状側壁部の平面形状は凹部の内底面から前記略方形又は略トラック形の内底面の長辺に向けて末広がりに形成された略台形状であることが好ましい。攪拌容器の形状は、略角形筒体又は略トラック形筒体であることが好ましい。 Further, the inclined side wall portion of the concave portion is preferably located at a position overlapping with at least one of the surfaces perpendicular to the long side of the inner bottom surface of the substantially square or substantially track shape, and further, the flat surface of the inclined side wall portion. The shape is preferably a substantially trapezoidal shape formed in a divergent shape from the inner bottom surface of the recess toward the long side of the inner bottom surface of the substantially square or substantially track shape. The shape of the stirring container is preferably a substantially square cylinder or a substantially truck-shaped cylinder.

さらに、前記攪拌容器の外底面の高低差を解消するように攪拌容器外筒部を下方に延長してあることが好ましい。 Further, it is preferable that the outer cylinder portion of the stirring container is extended downward so as to eliminate the height difference of the outer bottom surface of the stirring container.

次に、本発明の第二の態様は、
上述した攪拌容器と、
前記攪拌容器を昇降可能に保持する保持座と、
懸濁液を攪拌する攪拌子を回転可能に設けた攪拌手段と、
前記懸濁液を吸引吐出可能な一以上のノズルを移動自在に設けた吸引吐出手段と、
を備えた攪拌分注装置である。
Next, the second aspect of the present invention is
With the above-mentioned stirring container
A holding seat that holds the stirring container up and down,
A stirring means provided with a rotatably stirrer for stirring the suspension, and
A suction / discharge means provided with one or more nozzles capable of sucking / discharging the suspension so as to be movable.
It is a stirring and dispensing device equipped with.

また、攪拌分注装置には前記懸濁液の液面を検知する液面検知手段をさらに備えていることが好ましく、前記液面検知手段から得られた情報にもとづいて、前記攪拌子の上端が液面から所定の深度に位置するように前記攪拌子を移動させることが可能な駆動手段をさらに備えていることが好ましい。 Further, it is preferable that the stirring dispenser further includes a liquid level detecting means for detecting the liquid level of the suspension, and the upper end of the stirrer is based on the information obtained from the liquid level detecting means. It is preferable that the stirrer is further provided with a driving means capable of moving the stirrer so that the stirrer is located at a predetermined depth from the liquid surface.

本発明の攪拌容器は、デッドボリューム率が低減されることにより、無駄になる試薬原料の少量化が図れ、試薬製造コストを低減することができる。 In the stirring container of the present invention, the dead volume ratio is reduced, so that the amount of wasted reagent raw material can be reduced, and the reagent manufacturing cost can be reduced.

本発明の4.8Lの最大投入液量に対応した攪拌容器と、攪拌子及びノズルとの位置関係を示した見取図である。It is a sketch which showed the positional relationship between a stirrer, a stirrer and a nozzle corresponding to the maximum amount of liquids of 4.8L of this invention. 図1に示す容器の、(a)上面図、(b)A−A面での正面断面図、(c)B−B面での正面断面図、(d)C−C面での側面断面図、(e)D−D面での側面断面図である。The container shown in FIG. 1 is (a) a top view, (b) a front sectional view on the AA plane, (c) a front sectional view on the BB plane, and (d) a side sectional view on the CC plane. FIG. 3 (e) is a side sectional view taken along the line DD. 本発明の2.0Lの最大投入液量に対応した攪拌容器と、攪拌子及びノズルとの位置関係を示した見取図である。It is a sketch which showed the positional relationship between a stirrer, a stirrer, and a nozzle corresponding to the maximum liquid charge amount of 2.0L of this invention. 図3に示す容器の、(a)上面図、(b)A−A面での正面断面図、(c)B−B面での正面断面図、(d)C−C面での側面断面図、(e)D−D面での側面断面図である。The container shown in FIG. 3 is (a) a top view, (b) a front sectional view on the AA plane, (c) a front sectional view on the BB plane, and (d) a side sectional view on the CC plane. FIG. 3 (e) is a side sectional view taken along the line DD. 図1に示す容器を用いて、4.8L、2.0L、1.0Lの各液量条件にて4時間攪拌した場合の磁性微粒子の分散性を経時的に評価した結果である。This is the result of evaluating the dispersibility of the magnetic fine particles over time when the container shown in FIG. 1 was stirred under the respective liquid volume conditions of 4.8 L, 2.0 L, and 1.0 L for 4 hours. 図3に示す容器を用いて、2.0L、1.0L、0.5Lの各液量条件にて4時間攪拌した場合の磁性微粒子の分散性を経時的に評価した結果である。This is the result of evaluating the dispersibility of the magnetic fine particles over time when the container shown in FIG. 3 was stirred under the respective liquid volume conditions of 2.0 L, 1.0 L, and 0.5 L for 4 hours. 本発明の4.8Lの最大投入液量に対応した攪拌容器をセットした攪拌分注装置の配置図である。It is a layout drawing of the stirring dispensing apparatus which set the stirring container corresponding to the maximum input liquid amount of 4.8L of this invention.

以下に本発明を詳細に説明する。 The present invention will be described in detail below.

本発明の攪拌容器の開口部は、攪拌容器上方から容器内に攪拌子及びノズルが挿入可能に、それぞれに、又は一体に設けた開口部が例示される。容器天面全体が開口した蓋無し形状の容器であってもよく、容器天面形状と重なるように一体成形した蓋に攪拌子及びノズルが挿入可能な開口部をそれぞれに、又は一体に設けてもよい。 The opening of the stirring container of the present invention is exemplified by an opening provided individually or integrally so that a stirrer and a nozzle can be inserted into the container from above the stirring container. The container may have a lidless shape with the entire top surface of the container open, and an opening into which a stirrer and a nozzle can be inserted is provided in each or integrally with a lid integrally molded so as to overlap the top surface of the container. May be good.

本発明において攪拌容器の凹部とは、前記攪拌容器の内底面に、前記攪拌子の攪拌時に形成する回転体の水平投影面を内包する水平投影面をもつ底面と、前記攪拌子の厚み以上の深さを有する攪拌容器内部の空間を指す。すなわち、攪拌時に前記攪拌子が容器内壁に衝突することがない十分な空間であれば良く、攪拌子を相対移動可能に、又は固定してセットすることができる。攪拌子をセットする際は、凹部内底面の略中心延長線上に攪拌子の中心が重なるように配置、さらに凹部内底面からの高さを決めて配置、又は懸濁液投入後に液面から所定の深度になるよう配置すればよい。なお、攪拌子が相対移動するとは、攪拌容器内の懸濁液量の減少にともなって下降する液面に対して攪拌子の液面下深度を変更する必要がある攪拌条件においては、攪拌子を下降させる、又は攪拌容器を上昇させることにより、凹部内底面から攪拌子下端までの距離(又は懸濁液面から攪拌子上端までの距離)を調整することを指す。 In the present invention, the concave portion of the stirring container is a bottom surface having a horizontal projection surface including a horizontal projection surface of a rotating body formed at the time of stirring the stirrer on the inner bottom surface of the stirring container, and a thickness equal to or larger than the thickness of the stirrer. Refers to the space inside the stirring container with depth. That is, any space is sufficient as long as the stirrer does not collide with the inner wall of the container during stirring, and the stirrer can be set so as to be relatively movable or fixed. When setting the stirrer, arrange it so that the center of the stirrer overlaps approximately on the extension line of the center of the inner bottom surface of the recess, determine the height from the inner bottom surface of the recess, or determine from the liquid level after adding the suspension. It may be arranged so as to have a depth of. It should be noted that the relative movement of the stirrer means that the stirrer moves under a stirring condition in which the depth below the liquid level of the stirrer needs to be changed with respect to the liquid level that descends as the amount of suspension in the stirring container decreases. Refers to adjusting the distance from the inner bottom surface of the recess to the lower end of the stir bar (or the distance from the suspension surface to the upper end of the stir bar) by lowering or raising the stir bar.

凹部内底面の形状は、攪拌子の攪拌時に形成する回転体の水平投影面を内包する水平投影面をもつ内底面であれば特に形状は限定されず、平面であっても曲面であっても問題はないが、水平投影面の直径と同等又はそれ以上、より具体的には水平投影面の直径の1乃至2倍の直径をもつ略円形平面状の内底面が例示される。凹部内底面の直径は、攪拌子周辺に必要なスペースと攪拌容器の液投入量に対して要求されるデッドボリュームを勘案して決定すれば特に問題はない。 The shape of the inner bottom surface of the recess is not particularly limited as long as it has a horizontal projection surface including the horizontal projection surface of the rotating body formed when the stirrer is stirred, and the shape may be a flat surface or a curved surface. There is no problem, but a substantially circular planar inner bottom surface having a diameter equal to or larger than the diameter of the horizontal projection surface, more specifically, one to two times the diameter of the horizontal projection surface is exemplified. There is no particular problem if the diameter of the inner bottom surface of the recess is determined in consideration of the space required around the stirrer and the dead volume required for the amount of liquid charged in the stirrer container.

また、攪拌子が薄くなれば、当然、凹部が浅く形成できるため、デッドボリューム率が低下する。一方で、攪拌子を薄くすると攪拌流が弱くなり攪拌効率も低下するため、攪拌子の厚みと攪拌効率の関係を予備的に評価し、薄くできる限界を確認しておくことが望ましい。 Further, if the stirrer becomes thinner, naturally, the recesses can be formed shallowly, so that the dead volume ratio decreases. On the other hand, if the stirrer is made thinner, the stirring flow becomes weaker and the stirring efficiency is also lowered. Therefore, it is desirable to preliminarily evaluate the relationship between the thickness of the stirrer and the stirring efficiency and confirm the limit of thinning.

なお、凹部は容器内底面に1つとは限らず、2つ以上あっても問題はないが、多くなるほどデッドボリューム率の上昇を引き起こすため、攪拌効率とのバランスを考慮して、その数を決定すべきである。 The number of recesses is not limited to one on the inner bottom surface of the container, and there is no problem if there are two or more recesses, but the larger the number, the higher the dead volume rate, so the number is determined in consideration of the balance with the stirring efficiency. Should.

本発明は、前記攪拌容器の内底面であって前記凹部の内底面より高い位置に、略方形又は略トラック形の内底面(以下、「トラック内底面」と呼ぶことがある)が設けられていることが好ましい。トラック内底面から複数のノズルで懸濁液を吸引する場合、ノズルの先端からトラック内底面までの距離が一定となるよう攪拌容器を容易に位置決めしやすくなるからである。 In the present invention, a substantially square or substantially track-shaped inner bottom surface (hereinafter, may be referred to as “track inner bottom surface”) is provided at a position higher than the inner bottom surface of the recess on the inner bottom surface of the stirring container. It is preferable to have. This is because when the suspension is sucked from the inner bottom surface of the truck by a plurality of nozzles, the stirring container can be easily positioned so that the distance from the tip of the nozzles to the inner bottom surface of the truck is constant.

上述したように、前記凹部の内底面より高い位置に、トラック内底面が設けられている場合、凹部の深さは、デッドボリューム率低減のため、(攪拌時に攪拌子上端の露出による懸濁液の発泡が生じない下限液面から凹部内底面までの距離)―(下降限界まで近接したノズル先端からトラック内底面までの距離)としておくことが好ましい。 As described above, when the inner bottom surface of the truck is provided at a position higher than the inner bottom surface of the recess, the depth of the recess is set to reduce the dead volume ratio (suspension due to exposure of the upper end of the stirrer during stirring). It is preferable to set the distance from the lower limit liquid level at which foaming does not occur to the inner bottom surface of the recess)-(the distance from the tip of the nozzle close to the lowering limit to the inner bottom surface of the truck).

また、トラック内底面の周縁から容器外筒部に向けて斜め上外方に形成した勾配(長手方向に垂直な断面は略V字形状を含む)又は斜め上外方に下凸に形成した曲面(長手方向に垂直な断面は略U字形状を含む)を形成すれば、底面形状によるデッドボリューム率の低減ができる点において好ましい。 In addition, a gradient formed diagonally upward and outward from the peripheral edge of the inner bottom surface of the truck toward the outer cylinder of the container (the cross section perpendicular to the longitudinal direction includes a substantially V-shape) or a curved surface formed diagonally upward and outward. It is preferable to form (the cross section perpendicular to the longitudinal direction includes a substantially U-shape) in that the dead volume ratio due to the bottom shape can be reduced.

凹部のトラック内底面側の側壁部は傾斜状であることが好ましい(以下、「傾斜状側壁部」と呼ぶことがある)。傾斜状側壁部の形状としては、凹部内底面の周縁部からトラック内底面に向けて斜め上の平面勾配又は曲面勾配を形成する形状、又は凹部内底面の周縁部から上方に形成された側壁部の途中からトラック内底面に向けて斜め上の平面勾配又は曲面勾配を形成する形状が例示できる。 The side wall portion of the recess on the inner bottom surface side of the track is preferably inclined (hereinafter, may be referred to as “inclined side wall portion”). The shape of the inclined side wall portion is a shape that forms a plane gradient or a curved surface gradient diagonally upward from the peripheral edge portion of the inner bottom surface of the recess toward the inner bottom surface of the track, or a side wall portion formed upward from the peripheral edge portion of the inner bottom surface of the recess. An example is a shape that forms a plane gradient or a curved surface gradient diagonally upward from the middle of the track toward the inner bottom surface of the track.

本発明において、凹部を設ける位置は、傾斜状側壁部がトラック内底面の長辺に対して垂直な面の少なくとも一つと重なる位置にあることが好ましく、さらに凹部の内底面及び傾斜状側壁部の両方がトラック内底面の長辺に対して垂直な面の少なくとも一つと重なる位置にあればより好ましい。 In the present invention, the position where the recess is provided is preferably a position where the inclined side wall portion overlaps with at least one of the surfaces perpendicular to the long side of the inner bottom surface of the truck, and further, the inner bottom surface of the recess and the inclined side wall portion. It is more preferable that both of them overlap with at least one of the planes perpendicular to the long side of the inner bottom surface of the track.

傾斜状側壁部の平面形状は、凹部の内底面からトラック内底面の長辺に向けて末広がりに形成された略台形状が例示される。攪拌子を凹部内底面に近接させた攪拌条件においては、略台形における二つの脚の延長線の交差角を大きく設定する方が、攪拌流が広い領域に伝わるため攪拌効率を向上させる点から好ましい。一方、前記交差角を大きく設定するほど凹部全体の容量が大きくなり攪拌容器のデッドボリュームも増えるため、前記交差角の設定に当たっては、攪拌容器の大きさと形状、攪拌効率とデッドボリュームを総合的に勘案して決定すればよい。 An example of the planar shape of the inclined side wall portion is a substantially trapezoidal shape formed in a divergent shape from the inner bottom surface of the recess toward the long side of the inner bottom surface of the truck. Under the stirring condition in which the stirrer is close to the inner bottom surface of the recess, it is preferable to set a large crossing angle of the extension lines of the two legs in a substantially trapezoidal shape from the viewpoint of improving the stirring efficiency because the stirring flow is transmitted to a wide area. .. On the other hand, the larger the crossing angle is set, the larger the capacity of the entire recess and the dead volume of the stirring container are increased. Therefore, when setting the crossing angle, the size and shape of the stirring container, the stirring efficiency and the dead volume are comprehensively considered. It should be decided in consideration.

しかし、傾斜状側壁部は、攪拌子を凹部内底面の近傍にセットする条件において、攪拌子により生成する攪拌流が攪拌子より高い位置にあるトラック内底面にまで、攪拌流の勢いが極端に減衰することなく伝達できるような傾斜角及び形状であればよく、攪拌容器全体において懸濁液の良好な分散性が確認できれば傾斜角及び形状は特に限定されるものではない。 However, in the inclined side wall portion, under the condition that the stirrer is set near the inner bottom surface of the recess, the momentum of the agitating flow is extremely high up to the inner bottom surface of the truck where the stirring flow generated by the stirrer is higher than the stirrer. The inclination angle and shape may be such that transmission can be performed without attenuation, and the inclination angle and shape are not particularly limited as long as good dispersibility of the suspension can be confirmed in the entire stirring container.

本発明の攪拌容器は、その形状が略角形筒体又は略トラック形筒体であることが好ましい。略角形筒体の攪拌容器形状とは、底面が略長方形又は略正方形(頂点は5mmから20mm程度にR加工又はC加工したほうが懸濁液の滞留部が無くなり、攪拌効率があがる点において好ましい)で筒体形状に形成したもので、前記筒体の辺(略方形内底面の長辺と平行な辺)又は頂点と重なり、かつ攪拌容器の外側に一部突出するように凹部を一体に設けた形状が例示できる。略トラック形筒体の攪拌容器形状とは、底面が略トラック形の筒体の辺(トラック内底面の長辺と平行な辺)と重なり、かつ攪拌容器の外側に一部突出するように凹部を一体に設けた形状が例示できる。 The stirring container of the present invention preferably has a substantially square cylinder or a substantially truck-shaped cylinder. The shape of the stirring container of the substantially square cylinder is that the bottom surface is approximately rectangular or approximately square (it is preferable that the apex is R-processed or C-processed to about 5 mm to 20 mm in that the retention portion of the suspension is eliminated and the stirring efficiency is improved). It is formed in the shape of a cylinder, and a recess is integrally provided so as to overlap the side (the side parallel to the long side of the substantially rectangular inner bottom surface) or the apex and partially project to the outside of the stirring container. The shape can be exemplified. The shape of the stirring container of the substantially truck-shaped cylinder is a recess so that the bottom surface overlaps with the side of the substantially truck-shaped cylinder (the side parallel to the long side of the bottom surface of the truck) and partially protrudes to the outside of the stirring container. Can be illustrated as an example of a shape in which the above are integrally provided.

さらに筒体の外筒部は底面に対して垂直である必要はなく、テーパー形状又は曲面形状にしたものでも差し支えない。 Further, the outer cylinder portion of the cylinder does not have to be perpendicular to the bottom surface, and may be tapered or curved.

攪拌容器の大きさは、例えば5L程度の懸濁液を攪拌するためには、縦200mm、横500mm、高さ150mm程度の寸法に成形した略角形筒体又は略トラック形筒体の容器を使用すればよい。さらに大量又は少量の懸濁液に対応するには、攪拌するのに必要なサイズの攪拌子及びその攪拌子をセットするのに適した寸法の攪拌容器を使用すればよく、攪拌容器の寸法は特に限定されない。 As for the size of the stirring container, for example, in order to stir a suspension of about 5 L, a container having a substantially square cylinder or a substantially truck-shaped cylinder formed into dimensions of about 200 mm in length, 500 mm in width and 150 mm in height is used. do it. In order to handle a larger amount or a small amount of suspension, a stirrer of a size required for stirring and a stirrer having a size suitable for setting the stirrer may be used. There is no particular limitation.

本発明では、内底面のみならず、高低差のある外底面を有する攪拌容器を安定に自立静置するためのサポートとして、例えば攪拌容器外筒部を下方に延長し、攪拌容器の外底面の高低差を解消できるように容器スカートを設けると、試料の容器内投入も容易に行うことができる点においてより好ましい。 In the present invention, as a support for stably and independently standing a stirring container having not only the inner bottom surface but also the outer bottom surface having a height difference, for example, the outer cylinder portion of the stirring container is extended downward to cover the outer bottom surface of the stirring container. It is more preferable to provide a container skirt so that the height difference can be eliminated, because the sample can be easily charged into the container.

本発明の攪拌容器の材質は、特に限定はないが、成形が容易な点及び容器内固形物の拡散状態が容易に目視できる点において透明又は半透明の材質が好ましい。一例として、オレフィン系樹脂、スチレン系樹脂、ビニル系樹脂、カーボネート系樹脂、エポキシ系樹脂、アクリル系樹脂、ポリエステル系樹脂、ポリアミド系樹脂といった熱可塑性樹脂又はガラスが挙げられる。また、容器を通して内容物を目視することはできないが、ステンレスやアルミなどの金属、アルミナやジルコニアなどのセラミック、さらには陶器や磁器等であっても所望する形状に成形することにより特に問題なく使用できる。 The material of the stirring container of the present invention is not particularly limited, but a transparent or translucent material is preferable in that molding is easy and the diffusion state of the solid matter in the container can be easily visually observed. Examples thereof include thermoplastic resins such as olefin resins, styrene resins, vinyl resins, carbonate resins, epoxy resins, acrylic resins, polyester resins, and polyamide resins, or glass. In addition, although the contents cannot be visually observed through the container, it can be used without any problem by molding metals such as stainless steel and aluminum, ceramics such as alumina and zirconia, and even pottery and porcelain into the desired shape. it can.

本発明の攪拌容器の成形加工法は、射出成形、押し出し成形、ブロー成形、真空成形、圧縮成形、光造形、切削加工、等が例示され、攪拌容器の形状と要求される精度等とを勘案して最適な成形加工法を選択すればよい。使用する材料はそれぞれの成形加工法に使用可能な材料の中から、懸濁液成分への影響を予備的に評価し、問題がないことの確認が取れたものを選べば、特に限定されない。 Examples of the molding method of the stirring container of the present invention include injection molding, extrusion molding, blow molding, vacuum molding, compression molding, optical molding, cutting, etc., and the shape of the stirring container and the required accuracy are taken into consideration. Then, the optimum molding method may be selected. The material to be used is not particularly limited as long as the material that can be used for each molding processing method is selected by preliminarily evaluating the influence on the suspension components and confirming that there is no problem.

本発明の攪拌容器に用いる攪拌子とは、剪断力を利用して攪拌するプロペラ翼、パドル翼、タービン翼等の翼状の攪拌子、遠心力を利用して攪拌する、半球型や貫通型の羽根のない形状の攪拌子、さらにはマグネチックスターラーに使用するシリンダー型、テーパー型、ハブ型等の回転子、等が例示される。固形物懸濁液の発泡が抑制される点においては、剪断力を利用した攪拌子に比べて、遠心力を利用した攪拌子の方がより好ましい。さらに、本発明のように攪拌容器のデッドボリュームを小さくする目的のためには、攪拌子を容器内底面に近づけて攪拌する必要があることから、遠心方式の攪拌子の中では、薄いディスク状が選択できる貫通型がより好ましい。 The stirrer used in the stirring container of the present invention is a hemispherical or penetrating type stirrer that uses shearing force to stir propeller blades, paddle blades, turbine blades and other blade-shaped stirrers, and centrifugal force to stir. Examples thereof include a stirrer having no blade shape, and a rotor such as a cylinder type, a taper type, and a hub type used for a magnetic stirrer. In terms of suppressing foaming of the solid suspension, a stirrer using centrifugal force is more preferable than a stirrer using shearing force. Further, in order to reduce the dead volume of the stirring container as in the present invention, it is necessary to bring the stirrer closer to the inner bottom surface of the container for stirring. The penetration type that can be selected is more preferable.

本発明の攪拌容器に投入する固形物は、ポリエチレン、ポリプロピレン、エチレン−酢酸ビニル共重合体、ナイロン、アクリル樹脂、メタクリル樹脂、ポリスチレン、スチレン−アクリル共重合体、スチレン−ブタジエン共重合体、ポリ塩化ビニル、もしくはこれらを主成分とする共重合体、又は混合物といった、熱可塑性樹脂製の粒子、さらには、前記粒子にマンガン−亜鉛フェライトなどのソフトフェライト、四三酸化鉄を主成分とするマグネタイト等の磁気感応性成分を含有させた粒子が例示できる。また、さらにはシリカ、チタニア、ジルコニア等の無機ポリマーの粒子、フェライト、マグネタイト等の金属酸化物の粒子等が例示できる。固形物の粒径は0.01乃至1000μmが例示でき、固形物の比重は均一濃度の懸濁液が調製でき、ノズルによる分注が可能な固形物であれば粒径は特に限定されない。 The solid matter to be charged into the stirring vessel of the present invention is polyethylene, polypropylene, ethylene-vinyl acetate copolymer, nylon, acrylic resin, methacrylic resin, polystyrene, styrene-acrylic copolymer, styrene-butadiene copolymer, polyvinyl chloride. Particles made of thermoplastic resin such as vinyl, copolymers containing these as main components, or mixtures, and soft ferrites such as manganese-zinc ferrite, magnesium containing triiron tetraoxide as main components, etc. Examples of particles containing the magnetically sensitive component of. Further, particles of an inorganic polymer such as silica, titania and zirconia, particles of a metal oxide such as ferrite and magnetite, and the like can be exemplified. The particle size of the solid matter can be exemplified by 0.01 to 1000 μm, and the specific gravity of the solid matter is not particularly limited as long as it can prepare a suspension having a uniform concentration and can be dispensed by a nozzle.

次に、攪拌分注装置について説明する。 Next, the stirring dispensing device will be described.

本発明の攪拌分注装置は
上述した攪拌容器と、
前記攪拌容器を昇降可能に保持する保持座と、
懸濁液を攪拌する攪拌子を回転可能に設けた攪拌手段と、
懸濁液を吸引吐出可能な一以上のノズルを移動自在に設けた吸引吐出手段と、
を備えた攪拌分注装置である。
The stirring and dispensing device of the present invention includes the above-mentioned stirring container and the stirring container.
A holding seat that holds the stirring container up and down,
A stirring means in which a stirrer for stirring the suspension is rotatably provided, and a stirring means.
A suction / discharge means provided with one or more nozzles capable of sucking / discharging the suspension so as to be movable,
It is a stirring and dispensing device equipped with.

前記保持座は、位置決め可能に前記攪拌容器を保持することができ、攪拌子下端から凹部内底面までの距離、又は攪拌子上端から液面までの距離が攪拌容器の凹部内の液面高さに対応して調整できるように昇降可能に設けた保持座が例示できる。 The holding seat can hold the stirring container in a positionable manner, and the distance from the lower end of the stirrer to the inner bottom surface of the recess or the distance from the upper end of the stirrer to the liquid level is the height of the liquid level in the recess of the stirring container. An example is a holding seat provided so as to be able to move up and down so that it can be adjusted in accordance with the above.

前記攪拌手段は、攪拌子の回転動作において
(1)所定の定常回転数で、一方向に回転する
(2)所定の定常回転数及び所定サイクル時間で時計回り―反時計回りに反転する
(反転時は攪拌子を減速後、一時停止させる)
(3)回転数及び/又は回転方向及び/又はサイクル時間を経時的に変更する
などの制御が可能な攪拌手段が例示できる。
攪拌子の高さ制御において
(4)液量に関係なく、凹部内底面から攪拌子までの距離を一定の高さに維持する
(5)液量に合わせて、液面から攪拌子上端までの距離を調整する
などが例示できる。
(5)については、攪拌子を昇降させても、前記保持座を昇降させてもよい。
In the rotation operation of the stirrer, the stirring means (1) rotates in one direction at a predetermined steady rotation speed (2) reverses clockwise-counterclockwise at a predetermined steady rotation speed and a predetermined cycle time (reversal). When the stirrer is decelerated and then paused)
(3) An example of a stirring means capable of controlling such as changing the rotation speed and / or the rotation direction and / or the cycle time with time.
In controlling the height of the stirrer, (4) maintain the distance from the inner bottom surface of the recess to the stirrer at a constant height regardless of the amount of liquid (5) from the liquid surface to the upper end of the stirrer according to the amount of liquid. For example, adjusting the distance.
Regarding (5), the stirrer may be raised or lowered, or the holding seat may be raised or lowered.

したがって、攪拌子動作としては、(1)から(5)の前記回転動作及び前記攪拌子の容器内底面からの高さを適宜最適に組み合わせることができる攪拌手段が例示できる。 Therefore, as the stirrer operation, a stirring means capable of appropriately and optimally combining the rotation operation of (1) to (5) and the height of the stirrer from the inner bottom surface of the container can be exemplified.

前記吸引吐出手段は、縦n本×横m本(n,mは自然数)、より具体的には縦1〜3本×横4〜15本に、ノズル先端高さが揃うように配列したノズルをセットし、
(1)前記攪拌容器内の懸濁液を吸引する位置
(2)吸引した懸濁液を分注容器に吐出する位置
(3)ノズルに残留する懸濁液を廃棄する位置
へ移動自在に移動手段を備えたものが例示できる。
The suction / discharge means is a nozzle arranged so that the nozzle tip heights are aligned with n vertical × m horizontal (n and m are natural numbers), more specifically, 1 to 3 vertical × 4 to 15 horizontal. Set,
(1) Position for sucking the suspension in the stirring container (2) Position for discharging the sucked suspension to the dispensing container (3) Moveable to a position where the suspension remaining in the nozzle is discarded An example is provided with means.

さらに懸濁液を吸引する際の、ノズル先端の液面下深度を吸引動作毎に得られた情報に基づいて決定したい場合、液面検知手段をさらに備えることが好ましい。液面検知手段としては、攪拌容器内の懸濁液の液面レベルを測定し、ノズル又は攪拌子の液面下深度を決定するものであり、フロート式、電極式、静電容量式、差圧式、ガイドパルス式などの液面接触方式、又は、超音波式、電波式、レーザ式などの液面非接触方式が例示される。それぞれの方式において長所短所があるが、懸濁液によるコンタミネーションがなく(クリーン度が高く)、液体の種類に依存しないで使用できる液面非接触方式がより好ましい。 Further, when it is desired to determine the depth below the liquid level at the tip of the nozzle when sucking the suspension based on the information obtained for each suction operation, it is preferable to further provide a liquid level detecting means. The liquid level detecting means measures the liquid level of the suspension in the stirring container to determine the depth below the liquid level of the nozzle or the stirrer, and is a float type, an electrode type, a capacitance type, or a difference. Examples thereof include a liquid level contact method such as a pressure type and a guide pulse type, and a liquid level non-contact method such as an ultrasonic type, a radio wave type, and a laser type. Although each method has advantages and disadvantages, a liquid level non-contact method that does not cause contamination due to suspension (high cleanliness) and can be used regardless of the type of liquid is more preferable.

また、攪拌容器内の懸濁液量の減少にともなって下降する液面に対して攪拌子の高さを変更する必要がある場合、凹部内底面から攪拌子下端までの距離(又は懸濁液面から攪拌子上端までの距離)を相対的に調整するように、攪拌容器の凹部にセットした攪拌子を移動させる駆動手段をさらに備えていてもよい。また、前記距離の調整について攪拌容器を保持する前記保持座を同時に駆動させても問題ない。 When it is necessary to change the height of the stirrer with respect to the liquid level that descends as the amount of suspension in the stirring container decreases, the distance (or suspension) from the inner bottom surface of the recess to the lower end of the stirrer A driving means for moving the stirrer set in the recess of the stirrer container may be further provided so as to relatively adjust the distance from the surface to the upper end of the stirrer. Further, there is no problem in simultaneously driving the holding seat that holds the stirring container for adjusting the distance.

以下、実施例を用いて本発明をさらに詳細に説明するが、これら実施例は本発明を限定するものではない。 Hereinafter, the present invention will be described in more detail with reference to Examples, but these Examples do not limit the present invention.

(分散性の評価)
磁性微粒子(粒径2.5μm)を用い、5%牛血清アルブミンを含む希釈液にて0.08%に調製した懸濁液を、各液量条件(実施例1:4.8L、2.0L、1.0L、実施例2:2.0L、1.0L、0.5L)にて4時間攪拌した場合の磁性微粒子の分散性を評価した。攪拌子には遠心方式攪拌子(M−Revo、φ48mm、実施例1:厚さ35mm、実施例2:厚さ19mm)を用い、市販の攪拌機(アズワン社製)に装着して回転攪拌した。攪拌条件は、回転数600rpm、1分毎の反転(正転―反転を1分毎に繰り返す)攪拌とした。また攪拌子の液面からの距離は、
実施例1 10mm(4.8L、2.0Lの各攪拌時)、3mm(1.0Lの攪拌時)
実施例2 10mm(2.0L、1.0Lの各攪拌時)、2mm(0.5Lの攪拌時)
に設定した。磁性微粒子の懸濁液のサンプリングは、ノズル吸引位置の左端(Left)、右端(Right)の液面下約5mmからディスポーザブルチップを用いて60μL採取し、あらかじめ1mLの100mM NaCl、0.05% Tween20、0.1%アジ化ナトリウムを含む10mMトリス塩酸緩衝液(pH8.0)を分注した試験管に添加し、ボルテックスミキサーにて均一に攪拌した。均一攪拌された磁性微粒子の懸濁液500μLを石英セルに採取し、分光光度計を用いて800nmにおける吸光度を測定した。
(Evaluation of dispersibility)
A suspension prepared to 0.08% with a diluted solution containing 5% bovine serum albumin using magnetic fine particles (particle size 2.5 μm) was prepared under each liquid volume condition (Example 1: 4.8 L, 2. The dispersibility of the magnetic fine particles was evaluated when the mixture was stirred at 0 L, 1.0 L, Example 2: 2.0 L, 1.0 L, 0.5 L) for 4 hours. A centrifugal stirrer (M-Revo, φ48 mm, Example 1: thickness 35 mm, Example 2: thickness 19 mm) was used as the stirrer, and the stirrer was mounted on a commercially available stirrer (manufactured by AS ONE Corporation) for rotary stirring. The stirring condition was rotation speed 600 rpm, inversion every 1 minute (normal rotation-inversion is repeated every 1 minute). The distance of the stirrer from the liquid level is
Example 1 10 mm (when stirring 4.8 L and 2.0 L), 3 mm (when stirring 1.0 L)
Example 2 10 mm (at the time of stirring 2.0 L and 1.0 L), 2 mm (at the time of stirring 0.5 L)
Set to. For sampling of the suspension of magnetic fine particles, 60 μL was collected from about 5 mm below the liquid surface at the left end (Left) and right end (Right) of the nozzle suction position using a disposable tip, and 1 mL of 100 mM NaCl, 0.05% Tween 20 was prepared in advance. , 10 mM Tris-hydrochloric acid buffer (pH 8.0) containing 0.1% sodium azide was added to a dispensed test tube, and the mixture was uniformly stirred with a vortex mixer. 500 μL of a suspension of uniformly stirred magnetic fine particles was collected in a quartz cell, and the absorbance at 800 nm was measured using a spectrophotometer.

実施例1
図1に示す攪拌容器10(最大容量4.8L)を、エポキシ樹脂を用いて光造形方式3Dプリント法により作製し、アクリルウレタン樹脂コートした。容器の外寸は縦196mm、横454mm、高さ131mmとし、直径48mmの攪拌子(厚さ35mm)の1.2倍の直径57mmの略円形平面状である深さ35mmの凹部と、縦15mm、横315mmの略トラック形状のノズル下降部内底面(縦2本×横10本のノズルに対応)を設けた。
Example 1
The stirring container 10 (maximum capacity 4.8 L) shown in FIG. 1 was prepared by a stereolithography 3D printing method using an epoxy resin, and coated with an acrylic urethane resin. The outer dimensions of the container are 196 mm in length, 454 mm in width, and 131 mm in height. , A substantially track-shaped inner bottom surface of a nozzle lowering portion (corresponding to 2 vertical × 10 horizontal nozzles) having a width of 315 mm was provided.

凹部の側壁部は30°の傾斜状となっており、85°の角度(台形における二つの脚の延長線の交差角)で末広がりに形成される略台形状の傾斜部と、ノズル下降部の内底面の周縁から外筒部まで11°及び17°の斜め上外方の勾配で接続した略V字形状の(又は略V字形状の一部を含む)内底面と、攪拌容器内底面の周縁から上方に、ノズル下降部内底面から開口部までの高さが93mmになるように延びた外筒部と、天面全体が開口した開口部と、略V字形状の(又は略V字形状の一部を含む)内底面の周縁から下方に58mm延びた容器スカートを一体に設けている。 The side wall of the recess is inclined at 30 °, and the substantially trapezoidal inclined part formed at an angle of 85 ° (the intersection angle of the extension lines of the two legs in the trapezoid) and the nozzle lowering part. Approximately V-shaped (or including a part of the approximately V-shaped) inner bottom surface connected from the peripheral edge of the inner bottom surface to the outer cylinder portion at diagonally upward and outer slopes of 11 ° and 17 °, and the inner bottom surface of the stirring container. An outer cylinder extending upward from the peripheral edge so that the height from the inner bottom surface of the nozzle lowering portion to the opening is 93 mm, an opening with the entire top surface open, and a substantially V-shaped (or substantially V-shaped) shape. A container skirt extending 58 mm downward from the peripheral edge of the inner bottom surface (including a part of) is integrally provided.

図2は、図1の攪拌容器を(a)上面図、(b)A−A面での正面断面図、(c)B−B面での正面断面図、(d)C−C面での側面断面図,(e)D−D面での側面断面図で表示したものである。 2A and 2B show the stirring container of FIG. 1 in (a) top view, (b) front sectional view on AA plane, (c) front sectional view on BB plane, and (d) CC plane. It is displayed by the side sectional view of (e) and the side sectional view of (e) DD plane.

ノズル下降部内底面からノズル先端までの距離を10mmとした場合(この条件において攪拌子上端は液面から露出しない)の残液量とデッドボリュームと規定すると、攪拌容器に入れた水の体積の測定結果から520mLであった。一方、攪拌容器10と同じ投影底面積をもつ平底容器の底面積を計算すると690cmとなった。平底容器の場合のデッドボリュームは、容器にセットした攪拌子(厚さ35mm、内底面から攪拌子底面までの距離7mm)の上端が露出しない残液量と規定すると2,898mLとなる。 When the distance from the inner bottom surface of the nozzle lowering part to the tip of the nozzle is 10 mm (the upper end of the stirrer is not exposed from the liquid surface under this condition), the amount of residual liquid and the dead volume are defined as the measurement of the volume of water in the stirring container. From the result, it was 520 mL. On the other hand, the bottom area of the flat bottom container having the same projected bottom area as the stirring container 10 was calculated to be 690 cm 2 . In the case of a flat-bottomed container, the dead volume is 2,898 mL, which is defined as the amount of residual liquid in which the upper end of the stirrer (thickness 35 mm, distance from the inner bottom surface to the stirrer bottom surface is 7 mm) set in the container is not exposed.

したがって、デッドボリュームをDV、最大投入液量をVmaxとしたとき、
デッドボリューム率 (DV(mL)/Vmax(mL))は、
攪拌容器10が、520mL/4800mL=0.108
攪拌容器10と投影底面積、および容器内底面から開口部までの高さが同じ128mmの平底容器の場合は、2,898mL/7066mL=0.410となり、約26%に低減することがわかった。(ただし、最大投入液量は全容積の80%と規定した。)
分散性の評価結果を図5に示した。いずれの液量においてもサンプリング箇所間で磁性微粒子濃度に有意差はなく、内底面に高低差を設けている本発明の攪拌容器においても良好な分散性が得られることがわかった。
Therefore, when the dead volume is DV and the maximum liquid input amount is Vmax,
The dead volume rate (DV (mL) / Vmax (mL)) is
Stirring container 10 is 520 mL / 4800 mL = 0.108
In the case of a flat-bottomed container having the same projected bottom area as the stirring container 10 and the height from the inner bottom surface of the container to the opening, it was 2,898 mL / 7066 mL = 0.410, which was found to be reduced to about 26%. .. (However, the maximum input liquid amount is specified as 80% of the total volume.)
The evaluation result of dispersibility is shown in FIG. It was found that there was no significant difference in the concentration of magnetic fine particles between the sampling points at any of the liquid amounts, and that good dispersibility could be obtained even in the stirring container of the present invention in which the height difference was provided on the inner bottom surface.

実施例2
図3に示す攪拌容器20(最大容量2.0L)は、実施例1と同様にエポキシ樹脂を用いた光造形方式3Dプリント法により作製し、アクリルウレタン樹脂コートした。攪拌容器20は、攪拌分注装置に搭載されている攪拌子の位置及びノズル駆動域が、図1に示す攪拌容器10を使用する攪拌分注装置の攪拌子の位置及びノズル駆動域と重なるように、凹部内底面及びノズル(縦2本×横5本に対応)下降部内底面を設計している。すなわち、攪拌容器の外寸を縦196mm、横197mm、高さ112mmとし、直径48mmの攪拌子(厚さ19mm)の1.2倍の直径57mmを有する略円形平面状である深さ16mmの凹部と、縦15mm、横158mmの長方形のノズル下降部内底面と、凹部の側壁部は13°の傾斜状となっており、15°の角度(台形における二つの脚の延長線の交差角)で末広がりに形成される略台形状の傾斜部と、ノズル下降部内底面周縁から外筒部まで11°及び18°の斜め上外方の勾配で接続した略V字形状の(又は略V字形状の一部を含む)と、攪拌容器内底面の周縁から上方に、ノズル下降部内底面からの高さが93mmになるように延びた外筒部と、天面全体が開口した開口部と、略V字形状の(又は略V字形状の一部を含む)ノズル下降部の内底面の周縁から下方に40mm延びた容器スカートを一体に設けている。
Example 2
The stirring container 20 (maximum capacity 2.0 L) shown in FIG. 3 was produced by a stereolithography 3D printing method using an epoxy resin in the same manner as in Example 1, and was coated with an acrylic urethane resin. In the stirring container 20, the position of the stirrer mounted on the stirring dispenser and the nozzle drive range overlap with the position of the stirrer and the nozzle drive range of the stirring dispenser using the stirring container 10 shown in FIG. In addition, the inner bottom surface of the recess and the inner bottom surface of the lowering part of the nozzle (corresponding to 2 vertical × 5 horizontal) are designed. That is, the outer dimensions of the stirring container are 196 mm in length, 197 mm in width, and 112 mm in height, and a concave portion having a diameter of 57 mm, which is 1.2 times the diameter of a stirrer (thickness 19 mm) having a diameter of 48 mm, and a depth of 16 mm, which is a substantially circular flat surface. The inner bottom surface of the rectangular nozzle lowering part with a length of 15 mm and a width of 158 mm and the side wall part of the recess are inclined at 13 °, and spread out at an angle of 15 ° (the intersection angle of the extension lines of the two legs in the trapezoid). One of the approximately V-shaped (or approximately V-shaped) portions connected to the substantially trapezoidal inclined portion formed in the nozzle from the inner bottom peripheral edge of the nozzle lowering portion to the outer cylinder portion at diagonally upward and outward gradients of 11 ° and 18 °. (Including the part), the outer cylinder part extending upward from the peripheral edge of the inner bottom surface of the stirring container so that the height from the inner bottom surface of the nozzle lowering part is 93 mm, the opening with the entire top surface open, and a substantially V shape. A container skirt extending 40 mm downward from the peripheral edge of the inner bottom surface of the nozzle lowering portion having a shape (or including a part of a substantially V-shape) is integrally provided.

図4は、図3の攪拌容器を(a)上面図、(b)A−A面での正面断面図、(c)B−B面での正面断面図、(d)C−C面での側面断面図,(e)D−D面での側面断面図で表示したものである。 4A and 4B show the stirring container of FIG. 3 in (a) top view, (b) front sectional view on AA plane, (c) front sectional view on BB plane, and (d) CC plane. It is displayed by the side sectional view of (e) and the side sectional view of (e) DD plane.

ノズル下降部内底面からノズル先端までの距離を10mmとした場合(この条件において攪拌子天面は液面から露出しない)の残液量とデッドボリュームと規定すると、攪拌容器に入れた水の残液量の測定結果から200mLであった。一方、容器20と同じ投影底面積をもつ平底容器の底面積を計算すると283cmとなった。平底容器の場合のデッドボリュームは、容器にセットした攪拌子(厚さ19mm、内底面から攪拌子底面までの距離7mm)の天面が露出しない残液量と規定すると735mLとなる。 When the distance from the inner bottom surface of the nozzle lowering part to the tip of the nozzle is 10 mm (the top surface of the stirrer is not exposed from the liquid surface under this condition), the residual liquid amount and dead volume are defined as the residual liquid of water in the stirring container. From the measurement result of the amount, it was 200 mL. On the other hand, the bottom area of the flat-bottomed container having the same projected bottom area as the container 20 was calculated to be 283 cm 2 . In the case of a flat-bottomed container, the dead volume is 735 mL if the top surface of the stirrer (thickness 19 mm, distance from the inner bottom surface to the stirrer bottom surface is 7 mm) set in the container is not exposed.

したがって、デッドボリュームをDV、最大投入液量をVmaxとしたとき、
デッドボリューム率 (DV(mL)/Vmax(mL))は、
攪拌容器20が、200mL/2000mL=0.100、
攪拌容器20と投影底面積、および容器内底面から開口部までの高さが同じ109mmの平底容器の場合は、735mL/2467mL=0.280となり、
約36%に低減することがわかった。(ただし、最大投入液量は全容積の80%と規定した。)
分散性の評価結果を図6に示した。いずれの液量においてもサンプリング箇所間で磁性微粒子濃度に有意差はなく、内底面に高低差を設けている本発明の攪拌容器においても良好な分散性が得られることがわかった。
Therefore, when the dead volume is DV and the maximum liquid input amount is Vmax,
The dead volume rate (DV (mL) / Vmax (mL)) is
The stirring container 20 has 200 mL / 2000 mL = 0.100,
In the case of a flat-bottomed container of 109 mm, which has the same projected bottom area as the stirring container 20 and the height from the inner bottom surface of the container to the opening, 735 mL / 2467 mL = 0.280.
It was found to be reduced to about 36%. (However, the maximum input liquid amount is specified as 80% of the total volume.)
The evaluation result of dispersibility is shown in FIG. It was found that there was no significant difference in the concentration of magnetic fine particles between the sampling points at any of the liquid amounts, and that good dispersibility could be obtained even in the stirring container of the present invention in which the height difference was provided on the inner bottom surface.

実施例3
図1の攪拌容器10を用いて図7のような態様の攪拌分注装置を作製した。
Example 3
Using the stirring container 10 of FIG. 1, a stirring dispensing device having the embodiment shown in FIG. 7 was produced.

攪拌容器10は駆動手段44による昇降動作を可能にした保持座41により位置決めし、保持する。 The stirring container 10 is positioned and held by the holding seat 41 that enables the raising and lowering operation by the driving means 44.

凹部に浸漬した攪拌子31aは、攪拌手段42により正転―反転の回転動作、及び攪拌子と深槽部内底面との距離を調整する。 The stirrer 31a immersed in the recess adjusts the forward-reverse rotation operation and the distance between the stirrer and the inner bottom surface of the deep tank portion by the stirring means 42.

ノズル32(合計20本、縦2本×横10本)は、吸引吐出手段43(X−Z軸移動)にセットし、超音波式の液面検知手段45から得られる液面高さ情報にもとづいて液面下深度を調整する。 The nozzles 32 (20 in total, 2 in length x 10 in width) are set in the suction / discharge means 43 (XZ axis movement), and the liquid level information obtained from the ultrasonic type liquid level detection means 45 is used. Based on this, adjust the depth below the liquid level.

磁性微粒子懸濁液の減少に伴う液面低下に対応して、攪拌子31aの上端が液面から所定の深度に位置するように駆動手段44により攪拌容器10を上昇させる。 In response to the decrease in the liquid level due to the decrease in the magnetic fine particle suspension, the stirring container 10 is raised by the driving means 44 so that the upper end of the stirrer 31a is located at a predetermined depth from the liquid surface.

攪拌容器10の保持座41を昇降させる駆動手段44は、攪拌容器10のデッドボリュームに相当する上昇位置にセンサーを設けて強制的にデッドボリュームの警報を出す設定とする。 The driving means 44 for raising and lowering the holding seat 41 of the stirring container 10 is set to provide a sensor at an ascending position corresponding to the dead volume of the stirring container 10 to forcibly issue a dead volume alarm.

一連の吸引吐出基本動作を以下に示す。
1)吸引吐出手段43によりノズル32が攪拌容器10の位置に移動し、吸引吐出手段43のノズル吸引動作により磁性微粒子懸濁液を吸引する。
2)吸引吐出手段43によりコンベア48に搭載した容器ラック47上の分注容器46上に移動し、磁性微粒子懸濁液を吐出する。
3)吸引吐出手段43によりノズル32を廃棄ポート49上に移動し、ノズル32に残留する磁性微粒子懸濁液を廃棄する。
A series of basic suction and discharge operations are shown below.
1) The nozzle 32 is moved to the position of the stirring container 10 by the suction / discharge means 43, and the magnetic fine particle suspension is sucked by the nozzle suction operation of the suction / discharge means 43.
2) The suction / discharge means 43 moves onto the dispensing container 46 on the container rack 47 mounted on the conveyor 48, and discharges the magnetic fine particle suspension.
3) The nozzle 32 is moved onto the disposal port 49 by the suction / discharging means 43, and the magnetic fine particle suspension remaining in the nozzle 32 is discarded.

10、20: 攪拌容器
11、21: 凹部内底面
12、22: ノズル下降部内底面
13,23: 外筒部
14,24: 開口部
15、25: 傾斜部
16、26: 容器スカート
31a、31b: 攪拌子
32: ノズル
41: 保持座
42: 攪拌手段
43: 吸引吐出手段
44: 駆動手段
45: 液面検知手段
46: 分注容器
47: 容器ラック
48: コンベア
49: 廃棄ポート
10, 20: Stirring container 11, 21: Recessed inner bottom surface 12, 22: Nozzle lowering portion inner bottom surface 13, 23: Outer cylinder portion 14, 24: Opening portion 15, 25: Inclined portion 16, 26: Container skirt 31a, 31b: Stirrer 32: Nozzle 41: Holding seat 42: Stirring means 43: Suction / discharging means 44: Driving means 45: Liquid level detecting means 46: Dispensing container 47: Container rack 48: Conveyor 49: Disposal port

Claims (3)

攪拌子(刃部材を除く)で回転攪拌された懸濁液を収容する攪拌容器を備えた攪拌分注装置であって、
前記攪拌容器の内底面に、前記攪拌子の攪拌時に形成する回転体の水平投影面を内包する水平投影面をもつ凹部であって前記攪拌子の厚み以上の深さを有する前記凹部と、前記凹部の内底面より高い位置に、略方形又は略トラック形の内底面と、が設けられている前記攪拌容器において、
前記凹部に前記攪拌子が設置され、
前記略方形又は略トラック形の内底面から前記懸濁液を吸引する一以上のノズルを移動自在に設けた吸引吐出手段と
を備えた攪拌分注装置。
A stirring and dispensing device equipped with a stirring container for accommodating a suspension that has been rotationally stirred by a stirrer (excluding blade members) .
The inner bottom surface of the stirring vessel, said recess having a rotating body horizontal projection surface recess is a by thickness or depth of the stirring bar with which encloses the horizontal projection plane to form during stirring of the stirrer, the In the stirring container provided with a substantially square or substantially track-shaped inner bottom surface at a position higher than the inner bottom surface of the recess.
The stirrer is installed in the recess,
With a suction / discharge means in which one or more nozzles for sucking the suspension from the inner bottom surface of the substantially square or substantially truck shape are movably provided.
A stirring dispenser equipped with.
前記懸濁液の液面を検知する液面検知手段をさらに備えた、請求項に記載の攪拌分注装置。 Further comprising a liquid level sensing means for sensing the liquid level of the suspension, stirred dispensing device according to claim 1. 前記液面検知手段から得られた情報にもとづいて、前記攪拌子の上端が液面から所定の深度に位置するように前記攪拌子を移動させる駆動手段をさらに備えた、請求項に記載の攪拌分注装置。 Based on the information obtained from the liquid level sensing means, the upper end of the stirring bar, further comprising a driving means for moving the stirrer so as to be positioned at a predetermined depth from the liquid surface, according to claim 2 Stir bar dispenser.
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