JP3410314B2 - Chromatographic separation apparatus and method for filling packing material into column - Google Patents
Chromatographic separation apparatus and method for filling packing material into columnInfo
- Publication number
- JP3410314B2 JP3410314B2 JP01481797A JP1481797A JP3410314B2 JP 3410314 B2 JP3410314 B2 JP 3410314B2 JP 01481797 A JP01481797 A JP 01481797A JP 1481797 A JP1481797 A JP 1481797A JP 3410314 B2 JP3410314 B2 JP 3410314B2
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- JP
- Japan
- Prior art keywords
- column
- packing material
- storage tank
- pressure
- chromatographic separation
- Prior art date
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Description
【０００１】[0001]
【発明の属する技術分野】本発明は、カラムクロマトグ
ラフィーに用いられるクロマト分離装置及びカラムへの
充填材の充填方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a chromatographic separation device used for column chromatography and a method for filling a column with a packing material.
【０００２】[0002]
【従来の技術】カラムクロマトグラフィーは、カラムに
充填されている充填材に、分離対象である原液を通液
し、しかる後、溶離液を通液して、その流出液を成分や
重合度別に分取するもので、近年は工業的にも応用され
ている。例えば、重合度の異なる複数の糖類の塩酸溶液
を原液とし、充填材として強酸性カチオン交換樹脂を用
い、溶離液として原液とほぼ同濃度の塩酸溶液を用い
て、糖類を重合度別に分離することが行われている。2. Description of the Related Art In column chromatography, a stock solution to be separated is passed through a packing material packed in a column, and then an eluent is passed through, and the effluent is separated according to a component or a degree of polymerization. It is collected separately and has been applied industrially in recent years. For example, separate saccharides by degree of polymerization by using a hydrochloric acid solution of multiple saccharides with different degrees of polymerization as stock solutions, using a strongly acidic cation exchange resin as the packing material, and using a hydrochloric acid solution of approximately the same concentration as the stock solution as the eluent. Is being done.
【０００３】[0003]
【発明が解決しようとする課題】ところで、このような
場合、充填材である強酸性カチオン交換樹脂が、塩酸等
の強電解質溶液中におかれることになり、その性質上か
なりの収縮を生じる。しかしながら、クロマト分離を効
率的に行うためには、原液の希釈を防ぐため、一般にク
ロマトカラム内に充填材を満杯に充填しておくことが好
ましい。従って、上記したような場合には、強酸性カチ
オン交換樹脂をカラム内に収縮状態で満杯に充填してお
くことが好ましい。By the way, in such a case, the strong acid cation exchange resin as a filler is placed in a strong electrolyte solution such as hydrochloric acid, which causes considerable shrinkage. However, in order to efficiently perform chromatographic separation, it is generally preferable to fully fill the packing material in the chromatographic column in order to prevent dilution of the stock solution. Therefore, in the above case, it is preferable to fill the column with the strongly acidic cation exchange resin in a contracted state.
【０００４】その一方、このようにして強酸性カチオン
交換樹脂を満杯に充填した状態で、原液の濃度調整系に
おける故障などにより、水、あるいは濃度の低い塩酸が
混入した場合には、強酸性カチオン交換樹脂が膨潤し、
その膨潤圧によりカラムが破裂するおそれがある。On the other hand, when water or low-concentration hydrochloric acid is mixed in due to a failure in the concentration adjusting system of the stock solution in the state where the strong acid cation exchange resin is filled up in this way, the strong acidic cation exchange resin is used. The exchange resin swells,
The swelling pressure may cause the column to burst.
【０００５】これを防止するため、従来、設計の際にこ
の膨潤圧も考慮した高強度のカラムを用いている。しか
しながら、カラムの設計圧力の決定に当たっては、文献
上のデータ（例えば、Helfferch‘Ion Exchange’McGra
w-Hill New York 1962によれば、ゲル型の強酸性カチオ
ン交換樹脂のＨ形の膨潤圧は、ＤＶＢ４％で４１atm）
や、強電解質溶液による収縮等の諸条件を考慮して、実
験を経て決定していた。従って、この実験のために相当
の手間、コストを要していた。また、上記した糖類の分
離に当たっては、膨潤圧を加味すると、例えば、約４０
kgf/cm2・Gの耐圧を有するカラムが必要となるが、これ
ほど高強度になると、カラムはもとより、目板や覗き窓
用ガラス等の付属品にも過剰な製作コストがかかるとい
う問題があった。In order to prevent this, a high-strength column is conventionally used in consideration of this swelling pressure in the design. However, in determining the column design pressure, literature data (eg, Helfferch'Ion Exchange'McGra
According to w-Hill New York 1962, the swelling pressure of gel type strongly acidic cation exchange resin is 41 atm at 4% DVB)
In addition, it was decided through an experiment in consideration of various conditions such as contraction due to a strong electrolyte solution. Therefore, this experiment required considerable labor and cost. In addition, in separating the saccharides described above, when swelling pressure is added, for example, about 40
A column with a pressure resistance of kgf / cm 2 · G is required, but with such high strength, there is a problem that not only the column, but also the accessories such as the eye plate and the glass for the viewing window will have an excessive manufacturing cost. there were.
【０００６】一方、上記した強酸性カチオン交換樹脂
等、強電解質溶液中におくと収縮する充填材をカラム内
に収縮状態で満杯に充填するに当たっては、従来、次の
ような方法が採られている。すなわち、配管によって接
続されているカラムと充填材を収容するための充填材貯
槽とを強電解質溶液、例えば塩酸で満たし、充填材貯槽
内に充填材を投入し、さらに、充填材貯槽にポンプを用
いて所定の流入圧で塩酸を圧送して、収縮した充填材を
この流入圧を利用してカラム内に移送している。また、
カラム内が充填材によって満たされたことは、ポンプの
流出側に付設した圧力計の値上昇で感知し、その時点で
充填作業を終了している。On the other hand, in order to fill the column with a packing material such as the above-mentioned strongly acidic cation exchange resin, which contracts when placed in a strong electrolyte solution, in the contracted state, the following method has been conventionally adopted. There is. That is, a column connected by a pipe and a packing material storage tank for containing the packing material are filled with a strong electrolyte solution, for example, hydrochloric acid, the packing material is charged into the packing material storage tank, and a pump is further installed in the packing material tank. Hydrochloric acid is pressure-fed at a predetermined inflow pressure, and the contracted packing material is transferred into the column by using this inflow pressure. Also,
The fact that the column is filled with the packing material is detected by the increase in the value of the pressure gauge attached to the outflow side of the pump, and the packing operation is completed at that point.
【０００７】しかしながら、上記した方法で充填材貯槽
内に充填材を投入する場合、充填材貯槽の上部に設けら
れたマンホールを開け、そこから塩酸が張り込まれた充
填材貯送内に充填材を投入することが行われている。こ
のため、投入時に、作業者に塩酸の飛沫が付着したり、
塩酸のヒュームが周囲環境に飛散して環境を汚染すると
いう問題があった。However, when the filler is charged into the filler storage tank by the above method, the manhole provided in the upper portion of the filler storage tank is opened, and the filler is stored in the filler storage filled with hydrochloric acid. Is being done. For this reason, when it is thrown in, splashes of hydrochloric acid adhere to workers,
There was a problem that the fume of hydrochloric acid scatters in the surrounding environment and pollutes the environment.
【０００８】本発明は上記事情に鑑みなされたものであ
り、充填材の膨潤圧によるカラムの破壊を防止できると
共に、低コストで製作できるクロマト分離装置を提供す
ることを課題とする。また、安全で環境汚染も防止でき
るカラムへの充填材の充填方法を提供することを課題と
する。The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a chromatographic separation device which can prevent the column from being broken by the swelling pressure of the packing material and can be manufactured at low cost. Another object is to provide a method for packing a packing material into a column, which is safe and can prevent environmental pollution.
【０００９】[0009]
【課題を解決するための手段】上記課題を達成するた
め、本発明のクロマト分離装置は、カラム内に充填され
た充填材の膨潤圧を測定する圧力計と、カラムに接続さ
れ、充填材の膨潤圧が所定値以上になると、該圧力計か
らの電気信号に基づき開弁する充填材逃がし弁と、を有
することを特徴とする。In order to achieve the above object, the chromatographic separation device of the present invention is equipped with a pressure gauge for measuring the swelling pressure of the packing material packed in the column and a packing material connected to the column. A filling material relief valve that opens when the swelling pressure exceeds a predetermined value based on an electric signal from the pressure gauge.
【００１０】なお、前記圧力計としては、隔膜式圧力計
が好ましく、さらには二接点付きであって、低接点で原
液のカラムへの流入を停止させる電気信号を出力し、高
接点で前記充填材逃がし弁を開弁する電気信号を出力す
るものが好ましい。As the pressure gauge, a diaphragm type pressure gauge is preferable, and further, it has two contacts and outputs an electric signal for stopping the inflow of the undiluted solution into the column at a low contact, and the filling at the high contact. It is preferable to output an electric signal for opening the material release valve.
【００１１】また、本発明のカラムへの充填材の充填方
法は、充填材を、クロマト分離装置を構成するカラム内
に強電解質溶液によって収縮させた状態で満杯に充填す
る方法であって、カラム及び該カラムに対し配管により
接続された充填材貯槽に水を張り込む工程と、充填材貯
槽内に充填材を投入する工程と、該水をクロマト分離を
行う強電解質溶液と近似する濃度の強電解質溶液と置換
する工程と、当該強電解質溶液と同じ強電解質溶液又は
気体を充填材貯槽に流入させ、そのときの流入圧によ
り、該充填材貯槽内で収縮した充填材を、その状態で配
管を経由させてカラム内に満杯になるまで移送する工程
とを有することを特徴とする。Further, the method of filling the packing material in the column of the present invention is a method of filling the packing material in the column constituting the chromatographic separation device while the column is contracted by the strong electrolyte solution. And a step of pouring water into a packing material storage tank connected to the column by a pipe, a step of charging the packing material into the packing material storage tank, and a strong electrolyte solution having a concentration similar to that of a strong electrolyte solution for chromatographic separation. The step of substituting with the electrolyte solution and the same strong electrolyte solution or gas as the strong electrolyte solution is caused to flow into the filling material storage tank, and the filling material contracted in the filling material storage tank due to the inflow pressure at that time is piped in that state. And a step of transferring the same to the column until it becomes full.
【００１２】[0012]
【発明の実施の形態】次に、本発明の実施の形態を図面
に基づいて説明する。図１において符号１は本実施の形
態に係るクロマト分離装置を示し、カラム２、圧力計３
及び充填材逃がし弁４を有して構成されている。DESCRIPTION OF THE PREFERRED EMBODIMENTS Next, embodiments of the present invention will be described with reference to the drawings. In FIG. 1, reference numeral 1 indicates a chromatographic separation device according to the present embodiment, including a column 2, a pressure gauge 3
And a filler escape valve 4.
【００１３】カラム２は、後述のように、本実施の形態
ではカラム２自体が充填材の膨潤圧に耐え得るだけの耐
圧を有している必要はない。従って、カラム２へ原液又
は溶離液を供給する一次側のポンプの最大圧力に対応し
た耐圧を有すればよい。例えば、糖類の分離に当たっ
て、充填材として強酸性カチオン交換樹脂を用い、溶離
液として塩酸等の強電解質溶液を用いる場合、充填材の
膨潤圧に耐え得る設計圧力とするには、上記したよう
に、例えば、約４０kgf/cm2・Gの耐圧を有するように設
計する必要があるが、本実施の形態によれば、例えばそ
の半分以下の耐圧で設計することができる。As will be described later, the column 2 need not have a pressure resistance sufficient to withstand the swelling pressure of the packing material in the present embodiment. Therefore, it is sufficient that the column 2 has a pressure resistance corresponding to the maximum pressure of the primary-side pump that supplies the stock solution or the eluting solution. For example, in separating saccharides, when a strong acid cation exchange resin is used as the packing material and a strong electrolyte solution such as hydrochloric acid is used as the eluent, the design pressure that can withstand the swelling pressure of the packing material is as described above. For example, it is necessary to design to have a withstand voltage of about 40 kgf / cm 2 · G, but according to the present embodiment, it is possible to design with a withstand voltage of, for example, half or less of that.
【００１４】圧力計３の取り付け位置は、次の実験から
明らかなように、充填材の膨潤圧が配管部では測定でき
ないことから、カラム２に直接取り付ける必要がある。
但し、カラム２であれば、そのいずれの部分に取り付け
ても構わない。また、膨潤圧を測定するに当たって、充
填材及び強電解質溶液に直接接触するため、隔膜式圧力
計が好ましい。また、この圧力計３は、隔膜式圧力計で
あって、さらに、二接点付きのものがより好ましい。こ
れにより、樹脂が膨潤して、例えば、圧力値が低い方の
接点（低接点）に至ったときには、その電気信号によ
り、原液及び溶離液の供給を停止すると共に、警報機を
動作させ、さらに、膨潤圧が高くなって圧力値が高い方
の接点（高接点）に至ったときには、その電気信号を後
述の充填材逃がし弁に送って充填材を排出するという制
御ができ、カラム２の破裂防止の確実性を高めることが
できる。As will be apparent from the following experiment, the mounting position of the pressure gauge 3 must be directly mounted on the column 2 because the swelling pressure of the packing material cannot be measured in the pipe section.
However, the column 2 may be attached to any part thereof. Further, in measuring the swelling pressure, a diaphragm type pressure gauge is preferable because it is in direct contact with the filler and the strong electrolyte solution. Further, the pressure gauge 3 is preferably a diaphragm type pressure gauge, and more preferably has two contacts. As a result, when the resin swells and reaches, for example, the contact (low contact) with the lower pressure value, the electric signal stops the supply of the stock solution and the eluting solution, and activates the alarm. When the swelling pressure is high and the contact point has a higher pressure value (high contact point), it is possible to control the electric signal to be sent to the filling material relief valve described later to discharge the filling material, and the column 2 is ruptured. The certainty of prevention can be increased.
【００１５】ここで、充填材の膨潤圧を調べるために行
った実験について説明する。すなわち、カラム２（容
量：３２２ml、層高：１００cm、断面積：３．２２c
m2、内径：２．０２５cm、材質：５mm厚パイレックスガ
ラス（耐圧１５kg/cm2）、エンドキャップ材質：７mm厚
ポリアセタール共重合体）に、濃度２．５Ｎの塩酸で収
縮させた充填材（強酸性カチオン交換樹脂）を満杯に充
填し、高速液体クロマトグラフ用プランジャーポンプ
（ポンプ出口圧の上限１０kg/cm2）を用いて、脱塩水を
流速ＳＶ０．３３９（１．８２ml/min）で供給し、塩酸
を脱塩水に置換した。Here, an experiment conducted for investigating the swelling pressure of the filler will be described. That is, column 2 (volume: 322 ml, bed height: 100 cm, cross-sectional area: 3.22 c
m 2 , inner diameter: 2.025 cm, material: 5 mm thick Pyrex glass (pressure resistance 15 kg / cm 2 ), end cap material: 7 mm thick polyacetal copolymer, a filler (contracted with strong acid) contracted with hydrochloric acid with a concentration of 2.5 N (Cationic cation exchange resin) is filled up and demineralized water is supplied at a flow rate of SV 0.339 (1.82 ml / min) using a plunger pump for high performance liquid chromatography (upper limit of pump outlet pressure is 10 kg / cm 2 ). Then, the hydrochloric acid was replaced with demineralized water.
【００１６】その結果、６０分経過後、流速が落ち始
め、ポンプの出口圧が１kg/cm2上昇した。そして、１１
２分後にカラム２のエンドキャップ２ａ，２ｂが上下と
も同時に破損した。実験終了後、充填材を抜き出してタ
ッピング法で充填材量を測定したところ４１０mlであっ
た。As a result, after 60 minutes, the flow rate started to drop and the outlet pressure of the pump increased by 1 kg / cm 2 . And 11
After 2 minutes, the end caps 2a and 2b of the column 2 were broken at the same time in both upper and lower parts. After the end of the experiment, the filler was taken out and the amount of the filler was measured by the tapping method, and it was 410 ml.
【００１７】このことから、ポンプの出口圧の上昇が僅
か１kg/cm2であるにも拘わらず、充填材量が４１０mlに
膨潤し、カラム２を構成するエンドキャップ２ａ，２ｂ
が破損したことから、膨潤圧が主にカラム２のみに作用
することがわかる。従って、ポンプの出口圧の上昇を検
出して、カラム２の耐圧の範囲内で装置を停止すること
は困難であり、換言すれば膨潤圧を配管部で正確に測定
することは困難であり、上記したように、膨潤圧を測定
する圧力計３としては、充填材に直接接触できる隔膜式
圧力計をカラム２に取り付けることが好ましい。また、
この実験において、エンドキャップ２ａ，２ｂが上下と
も同時に破損したことから、膨潤圧がカラム２全体に均
一にかかっていると考えられ、圧力計３はカラム２であ
ればいずれの位置に取り付けてもよいことがわかる。From this, the end caps 2a, 2b constituting the column 2 swelled up to 410 ml of the packing material even though the rise in the outlet pressure of the pump was only 1 kg / cm 2.
It was found that the swelling pressure mainly acts only on the column 2 from the fact that the column was broken. Therefore, it is difficult to detect an increase in the outlet pressure of the pump and stop the apparatus within the range of the pressure resistance of the column 2, in other words, it is difficult to accurately measure the swelling pressure in the pipe section. As described above, as the pressure gauge 3 for measuring the swelling pressure, it is preferable to attach the diaphragm type pressure gauge that can directly contact the packing material to the column 2. Also,
In this experiment, since the end caps 2a and 2b were broken at the same time in the upper and lower sides, it is considered that the swelling pressure is evenly applied to the entire column 2, and the pressure gauge 3 may be attached at any position in the column 2. I know it's good.
【００１８】充填材逃がし弁４は、圧力計３からの電気
信号に基づき作動する自動弁からなり、カラム２に接続
された逃がし管４ａ中に介在配設されている。そして、
上記したように圧力計３が高接点に至った時点で開弁
し、該逃がし管４ａを通じて充填材を外部に排出する機
能を担う。The filling material relief valve 4 is an automatic valve which operates based on an electric signal from the pressure gauge 3, and is disposed in a relief pipe 4 a connected to the column 2. And
As described above, it has a function of opening the valve when the pressure gauge 3 reaches the high contact point and discharging the filler to the outside through the relief pipe 4a.
【００１９】次に、上記したクロマト分離装置１を含む
クロマト分離システムにおける、カラム１への充填材の
充填方法について図２に基づき説明する。なお、図２に
おいて１０はクロマト分離システム全体を示し、クロマ
ト分離装置１のほかに、充填材貯槽１１、溶離液貯槽１
２、原液貯槽１３、該充填材貯槽１１と溶離液貯槽１２
との間に配設された溶離液流入本管１４、該溶離液流入
本管１４から枝分かれした２本の溶離液流入枝管１４
ａ，１４ｂ、該溶離液流入本管１４中に介在配設された
ポンプ１５、一方の溶離液流入枝管１４ｂとカラム２と
を連通する連通管１６、充填材貯槽１１とカラム２との
間に配設された充填材移送管１７、カラム２に接続され
て設けられた流出管１８、原液貯槽１３とカラム２とを
結ぶ原液供給管１９を有している。Next, a method of filling the column 1 with the packing material in the chromatographic separation system including the chromatographic separation device 1 will be described with reference to FIG. In FIG. 2, reference numeral 10 denotes the entire chromatographic separation system, and in addition to the chromatographic separation device 1, a packing material storage tank 11 and an eluent storage tank 1 are provided.
2, stock solution storage tank 13, the filling material storage tank 11 and the eluent storage tank 12
And an eluent inflow main pipe 14 disposed between the eluent and the two eluent inflow main pipes 14 branched from the eluent inflow main pipe 14.
a, 14b, a pump 15 disposed in the eluent inflow main pipe 14, a communication pipe 16 for communicating one eluent inflow branch pipe 14b with the column 2, and a space between the packing material storage tank 11 and the column 2. And a stock solution feed pipe 19 connecting the stock solution storage tank 13 and the column 2.
【００２０】充填材を充填するに当たっては、まず、図
示しない水供給源から溶離液流入本管１４、溶離液流入
枝管１４ａ，１４ｂ、連通管１６を介して、充填材貯槽
１１及びカラム２共に水で満たす。次に、充填材貯槽１
１のマンホールを開けて充填材１１ａを投入する。な
お、投入量は、カラム２に収縮状態で充填したときに満
杯となる量よりも多めにしておく。In filling the packing material, first, both the packing material storage tank 11 and the column 2 are supplied from a water supply source (not shown) through the eluent inflow main tube 14, the eluent solution inflow branch tubes 14a and 14b, and the communication tube 16. Fill with water. Next, the filler storage tank 1
The manhole 1 is opened and the filling material 11a is introduced. It should be noted that the input amount is set to be larger than the full amount when the column 2 is packed in a contracted state.
【００２１】次に、ポンプ１５を起動して、溶離液貯槽
１２から、溶離液流入本管１４、溶離液流入枝管１４
ａ，１４ｂを介して充填材貯槽１１へ強電解質溶液であ
る塩酸等の溶離液（実際にクロマト分離する際の濃度と
同じか近似した濃度）を供給し、さらに、連通管１６を
介してカラム２へも溶離液を供給することにより、水を
溶離液と置換する。この置換作業は、流出管１８から流
出する溶離液の濃度が溶離液貯槽１２の溶離液の濃度と
同じになった時点で終了する。これにより、充填材貯槽
１１内の充填材は溶離液の濃度に応じて収縮する。Next, the pump 15 is started to drive the eluent inflow main pipe 14 and the eluent inflow branch pipe 14 from the eluent storage tank 12.
An eluent such as hydrochloric acid, which is a strong electrolyte solution (concentration that is the same as or close to that in actual chromatographic separation), is supplied to the packing material storage tank 11 via a and 14b, and further, the column is connected via a communication pipe 16. Water is replaced by eluent by also supplying eluent to 2. This replacement operation ends when the concentration of the eluent flowing out of the outflow pipe 18 becomes the same as the concentration of the eluent in the eluent storage tank 12. As a result, the packing material in the packing material storage tank 11 contracts according to the concentration of the eluent.
【００２２】このような状態で、再びポンプ１５を起動
して所定の圧力で溶離液貯槽１２から溶離液を充填材貯
槽１１に供給し、このときの溶離液の流入圧により充填
材貯槽１１内で既に収縮している充填材１１ａを移送管
１７を経由させてカラム２内へ満杯となるまで移送す
る。なお、溶離液によって収縮した充填材貯槽１１内の
充填材をカラム２に移送させる際、ポンプ１５の流入圧
力を用いるのに代えて、充填材貯槽１１に連通した空気
等の気体の流入管（図示せず）からの流入圧力を用いて
移送しても差し支えない。In such a state, the pump 15 is started again to supply the eluent from the eluent storage tank 12 to the filling material storage tank 11 at a predetermined pressure, and the inside pressure of the eluent at this time causes the inside of the filling material storage tank 11 to flow. Then, the packing material 11a which has already contracted is transferred into the column 2 through the transfer pipe 17 until it becomes full. When the packing material in the packing material storage tank 11 contracted by the eluent is transferred to the column 2, instead of using the inflow pressure of the pump 15, a gas inflow pipe (such as air) communicating with the packing material storage tank 11 ( Transfer may be performed using the inflow pressure from (not shown).
【００２３】その後は、分離対象である原液を、原液供
給管１９に介在配設されるポンプ１９ａを起動して、原
液貯槽１３から原液供給管１９を介してカラム２内へ導
入すると共に、ポンプ１５により溶離液貯槽１２から溶
離液を流入させ、クロマト分離を行う。After that, the stock solution to be separated is introduced into the column 2 from the stock solution storage tank 13 through the stock solution supply pipe 19 by activating the pump 19a provided in the stock solution supply pipe 19. The eluent is caused to flow from the eluent storage tank 12 by means of 15 for chromatographic separation.
【００２４】[0024]
【発明の効果】本発明のクロマト分離装置によれば、カ
ラムに圧力計が取り付けられているため、充填材の膨潤
圧を確実に測定でき、所定の設定圧力で装置の停止、充
填材のカラムからの排出を行うことができる。従って、
充填材の膨潤圧に合わせた高い耐圧を有するカラムを用
いる必要がなく、材料コストの削減に資する。また、充
填材の膨潤圧は、充填材の種類、あるいは溶離液の種類
や濃度等によって異なるため、従来、カラムの耐圧をこ
の膨潤圧に合わせるよう、耐圧を決定するための実験を
行う必要があったが、本発明によれば、このような実験
を行う必要がないため、実験に伴う手間及びコストの削
減にも資する。According to the chromatographic separation apparatus of the present invention, since the pressure gauge is attached to the column, the swelling pressure of the packing material can be reliably measured, the apparatus is stopped at a predetermined set pressure, and the packing material column is stopped. Can be discharged from. Therefore,
It is not necessary to use a column having a high pressure resistance according to the swelling pressure of the packing material, which contributes to material cost reduction. In addition, since the swelling pressure of the packing material varies depending on the type of packing material, the type and concentration of the eluent, etc., conventionally, it is necessary to perform an experiment for determining the pressure resistance so that the pressure resistance of the column is adjusted to this swelling pressure. However, according to the present invention, since it is not necessary to perform such an experiment, it also contributes to the reduction of labor and cost involved in the experiment.
【００２５】また、本発明のカラムへの充填材の充填方
法によれば、充填材貯槽に充填材を投入する際は、充填
材貯槽内には水が張られているだけであるため、作業者
にとって安全である。また、強電解質溶液からなる溶離
液あるいは原液を使用する際には、既にクロマト分離シ
ステム内が密閉系になっているため、ヒュームによる環
境汚染もない。Further, according to the method of filling the packing material into the column of the present invention, when the packing material is charged into the packing material storage tank, only water is filled in the packing material storage tank, so It is safe for the person. Further, when using an eluent or a stock solution composed of a strong electrolyte solution, there is no environmental pollution due to fumes because the chromatographic separation system is already closed.
【図１】本発明に係るクロマト分離装置の一の実施の形
態を示す模式図である。FIG. 1 is a schematic diagram showing an embodiment of a chromatographic separation device according to the present invention.
【図２】本発明に係るクロマト分離装置を構成するカラ
ムへ充填材を充填する方法の一の実施の形態を説明する
ための図である。FIG. 2 is a diagram for explaining one embodiment of a method of packing a packing material into a column constituting the chromatographic separation device according to the present invention.
１ クロマト分離装置 ２ カラム ３ 圧力計 ４ 充填材逃がし弁 １０ クロマト分離システム １１ 充填材貯槽 １２ 溶離液貯槽 １３ 原液貯槽 1 Chromatographic separation device 2 columns 3 pressure gauge 4 Filler relief valve 10 Chromatographic separation system 11 Filling material storage tank 12 Eluent storage tank 13 Stock solution storage tank
フロントページの続き (56)参考文献 特開 平８−50123（ＪＰ，Ａ) 特開 昭53−114779（ＪＰ，Ａ) 特開 昭52−17089（ＪＰ，Ａ) 特開 昭53−87294（ＪＰ，Ａ) 特表 平４−502276（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 30/56 Continuation of the front page (56) Reference JP-A-8-50123 (JP, A) JP-A-53-114779 (JP, A) JP-A-52-17089 (JP, A) JP-A-53-87294 (JP , A) Tokuyohei 4-502276 (JP, A) (58) Fields investigated (Int.Cl. 7 , DB name) G01N 30/56
Claims (4)
測定する圧力計と、カラムに接続され、充填材の膨潤圧
が所定値以上になると、該圧力計からの電気信号に基づ
き開弁する充填材逃がし弁と、を有することを特徴とす
るクロマト分離装置。1. A pressure gauge for measuring the swelling pressure of a packing material packed in a column, and a pressure gauge connected to the column, which opens based on an electric signal from the pressure gauge when the swelling pressure of the packing material reaches or exceeds a predetermined value. A chromatographic separation device comprising: a filling material relief valve that is valved.
項１記載のクロマト分離装置。2. The chromatographic separation device according to claim 1, wherein the pressure gauge is a diaphragm pressure gauge.
り、低接点で原液のカラムへの流入を停止させる電気信
号を出力し、高接点で前記充填材逃がし弁を開弁する電
気信号を出力する請求項２記載のクロマト分離装置。3. The diaphragm type pressure gauge has two contacts, and outputs an electric signal for stopping the flow of the stock solution into the column at a low contact, and an electric signal for opening the packing material relief valve at a high contact. The chromatographic separation device according to claim 2, which outputs.
記載のクロマト分離装置を構成するカラム内に強電解質
溶液によって収縮させた状態で満杯に充填する方法であ
って、 カラム及び該カラムに対し配管により接続された充填材
貯槽に水を張り込む工程と、充填材貯槽内に充填材を投
入する工程と、該水をクロマト分離を行う強電解質溶液
と近似する濃度の強電解質溶液と置換する工程と、当該
強電解質溶液と同じ強電解質溶液又は気体を充填材貯槽
に流入させ、そのときの流入圧により、該充填材貯槽内
で収縮した充填材を、その状態で配管を経由させてカラ
ム内に満杯になるまで移送する工程とを有することを特
徴とする、請求項１〜３のいずれか１項記載のクロマト
分離装置を構成するカラムへの充填材の充填方法。4. The filler as claimed in any one of claims 1 to 3.
A method of filling a column constituting the chromatographic separation device described above in a state in which the column is contracted by a strong electrolyte solution and filling the column and a filling material storage tank connected by piping to the column with water. , A step of introducing the filler into the filler storage tank, a step of replacing the water with a strong electrolyte solution having a concentration similar to the strong electrolyte solution for performing chromatographic separation, and a strong electrolyte solution or gas that is the same as the strong electrolyte solution. A step of causing the packing material to flow into the packing material storage tank and transferring the packing material contracted in the packing material storage tank through the pipe in that state until the column is full by the inflow pressure at that time. The chromatograph according to any one of claims 1 to 3,
A method for packing a packing material into a column constituting a separation device .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP01481797A JP3410314B2 (en) | 1997-01-13 | 1997-01-13 | Chromatographic separation apparatus and method for filling packing material into column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP01481797A JP3410314B2 (en) | 1997-01-13 | 1997-01-13 | Chromatographic separation apparatus and method for filling packing material into column |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10197507A JPH10197507A (en) | 1998-07-31 |
| JP3410314B2 true JP3410314B2 (en) | 2003-05-26 |
Family
ID=11871603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP01481797A Expired - Fee Related JP3410314B2 (en) | 1997-01-13 | 1997-01-13 | Chromatographic separation apparatus and method for filling packing material into column |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3410314B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4626745B2 (en) * | 2004-05-10 | 2011-02-09 | 栗田工業株式会社 | Chromatographic packing method |
| JP5023775B2 (en) * | 2007-04-05 | 2012-09-12 | 栗田工業株式会社 | Extraction method of chromatographic packed bed |
| JP4968489B2 (en) * | 2010-03-29 | 2012-07-04 | 栗田工業株式会社 | Chromatographic packing device |
-
1997
- 1997-01-13 JP JP01481797A patent/JP3410314B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10197507A (en) | 1998-07-31 |
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