JPS62108155A - Liquid chromatographic device - Google Patents

Liquid chromatographic device

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Publication number
JPS62108155A
JPS62108155A JP60249709A JP24970985A JPS62108155A JP S62108155 A JPS62108155 A JP S62108155A JP 60249709 A JP60249709 A JP 60249709A JP 24970985 A JP24970985 A JP 24970985A JP S62108155 A JPS62108155 A JP S62108155A
Authority
JP
Japan
Prior art keywords
sample
flow path
filter
section
flow passage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP60249709A
Other languages
Japanese (ja)
Inventor
Akira Nakamoto
中本 晃
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP60249709A priority Critical patent/JPS62108155A/en
Publication of JPS62108155A publication Critical patent/JPS62108155A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To increase the number of usable times of a piece of filter and to reduce a running cost by constituting a filter section provided to the 1st flow passage in such a manner that many filters can be successively and automatically changed over and used and constituting a flow passage in such a manner that a cleaning solvent flows backward at every one use of each filter. CONSTITUTION:A pipeline for sample transmission is first connected between the filter section 3 of the 1st flow passage A and drain a and a diluted and filtered sample is stored therein. The flow passage is then changed over and the pipeline for sample transfer is connected between a mobile phase solvent reservoir 4 of the 2nd flow passage B and an analyzing column 6 so that the sample stored in the pipeline is transported together with the mobile phase solvent to the column 6. The sample is thus analyzed. The cleaning solvent flows backward from a cleaning solvent resevoir 16 to clean, for example, a filter F1 when 3-way valves 11, 12 in the 1st flow passage A is thereafter changed over. The selector valves 17, 18 are successively changed over to the pipelines including another filters by the command from a controller 19 when the filter F1 is used at the set number of times in the above-mentioned manner.

Description

【発明の詳細な説明】 (イ)産業上の利用分野 この発明は液体クロマトグラフ装置に関Vる。[Detailed description of the invention] (b) Industrial application fields This invention relates to a liquid chromatography device.

さらに詳しくは製造ラインなどから試料を採取し、それ
を高速液体クロマトグラフに注入して分析を行い、製造
ラインのモニタ、制御などを行うノステムにおいてその
採取した試料のろ過機構に関する。
More specifically, it relates to a filtration mechanism for the collected sample in Nostem, which collects a sample from a production line, injects it into a high-performance liquid chromatograph, analyzes it, and monitors and controls the production line.

(ロ)従来の技術 ある製造ラインから試料を自動採取し、それを自動的に
前処理してから高速液体クロマトグラフに自動注入して
分析を行い、製造ラインのモニタをする、あるいはその
分析結果に基づいて製造ラインにフィー ドパツクする
ということがよく行われるようになってきている。
(b) Conventional technology Automatically collects a sample from a certain manufacturing line, automatically pre-processes it, and then automatically injects it into a high-performance liquid chromatograph to perform analysis and monitor the manufacturing line, or the results of the analysis It is becoming common practice to feed and pack products into production lines based on

(ハ)発明が解決しようとする間麗点 しかしながら、高速液体クロマトグラフの分析カラムは
、数μmの微粒子充填剤が充填されているため、試料の
前処理においては0.5μm程度のメツシュのメンブレ
ンフィルタを使用してのろ過が必要である。しかし0.
5μmと大変メツシュが小さいため数回(3〜5回)の
使用でそれを交換する必要があり、ラニングコストのア
ップ及び自動運転ノステムにおける効果の低下をもたら
している。
(c) Problems to be solved by the present invention However, since the analysis column of a high performance liquid chromatograph is filled with a fine particle packing material of several micrometers, it is necessary to use a mesh membrane of about 0.5 micrometers during sample pretreatment. Filtration using a filter is required. But 0.
Since the mesh is very small at 5 μm, it is necessary to replace it after several uses (3 to 5 times), resulting in an increase in running costs and a decrease in effectiveness in automatic driving systems.

(ニ)問題点を解決するための手段 かくしてこの発明によれば、試料導入部から試料希釈部
及びろ過部を介してドレインに延設される第一流路と、 移動相溶媒供給部から分析用カラム及び検出器を介して
ドレインに延設される第二流路と、切り換えバルブによ
り、第一流路のろ過部とドレインの間及び第二流路の移
動相供給部と分析用カラムの間のいずれかに接続される
試料転送用管路とから構成されてなり、第一流路のろ過
部を、フィルタを有する管路を複数本並設しかつこの両
端にこれらの管路のいずれかを選択して第一流路に接続
する二つの切り換えバルブで構成すると共に、第一流路
の下流に三方弁を介して洗浄溶媒を試料のろ過方向と逆
方向に切り換え導入しうる洗浄溶媒供給手段を設け、か
つ試料希釈部とろ過部の間に、上記逆方向への切り換え
導入時に第一流路を逆流する洗浄溶媒をドレインへ排出
しうる三方弁を設けたことを特徴とする液体クロマトグ
ラフ装置が提供される。
(d) Means for Solving the Problems Thus, according to the present invention, the first flow path extends from the sample introduction section to the drain via the sample dilution section and the filtration section, and the mobile phase solvent supply section for analysis. A second flow path that extends to the drain via the column and the detector, and a switching valve between the filtration part and the drain in the first flow path and between the mobile phase supply part and the analytical column in the second flow path. The filtration section of the first flow path has multiple pipes with filters installed in parallel, and one of these pipes is selected at both ends. and a cleaning solvent supply means that can switch and introduce the cleaning solvent in the opposite direction to the filtration direction of the sample through a three-way valve downstream of the first flow path. There is also provided a liquid chromatograph apparatus, characterized in that a three-way valve is provided between the sample diluting section and the filtration section, which can discharge the cleaning solvent flowing backward through the first flow path to the drain when switching to the reverse direction. Ru.

この発明によれば、上記第一流路に付設されたろ過部は
、多数のフィルタを順次自動的に切り換えて使用できる
よう構成され、かつ各フィルタは一回の使用毎に洗浄溶
媒が逆流するよう流路構成されている。
According to this invention, the filtration section attached to the first flow path is configured so that a large number of filters can be automatically switched and used in sequence, and each filter is configured so that the cleaning solvent flows back through each filter each time it is used. The flow path is configured.

上記ろ過部は、多数のポートを有する二つの切り換えバ
ルブ間に、フィルタを介在した管(フィルタ管路)が該
ボートに対応して複数個並設され、それらの両端の切り
換えバルブにより10図する管のみ第一流路に設定して
使用できるよう管路構成されており、一つの管に予め設
定された使用回数終了後、別のフィルタを含む管路に切
り換え接続されるよう設定されている。この切り換えバ
ルブは、どちらも一つのボートに対して複数の切り換え
可能なポートを有する切り換えバルブ、ことに中心から
回転してボート切り換えが出来るものが適しおり、該切
り換えバルブは後述するフィルタ管路数と同数のポジン
ジン(ポート対)を有するものが好ましい。該バルブに
おけるポートの切り換えは両者同時に同一の管路に接続
するよう切り換えられる。
In the above-mentioned filtration section, a plurality of pipes (filter pipe lines) with filters interposed between two switching valves having a large number of ports are arranged in parallel corresponding to the boat, and the switching valves at both ends of the pipes are arranged in parallel. The pipe is configured so that only the pipe can be set and used in the first flow path, and after a preset number of uses for one pipe is completed, it is set to be switched and connected to a pipe containing another filter. A suitable switching valve is a switching valve that has a plurality of switching ports for one boat, especially one that can be rotated from the center to switch boats. It is preferable to have the same number of ports (pairs of ports). The ports in the valve are switched so that both ports are connected to the same line at the same time.

上記フィルタ管路は、フィルタを管路の途中にフィルタ
ホルダ等により介在させたものであり、フィルタを交換
可能にした構造のものが好ましい。
The filter conduit has a filter interposed in the middle of the conduit by a filter holder or the like, and preferably has a structure in which the filter is replaceable.

該フィルタ管路数は目的に応じて適宜設定される。The number of filter pipes is appropriately set depending on the purpose.

上記管路に用いるフィルタは、市販のろ紙でもよく目の
細かいもの(例えば0.5μm程度)が好ましい。
The filter used for the above-mentioned conduit may be commercially available filter paper, but preferably has a fine mesh (for example, about 0.5 μm).

と記洗浄溶媒供給手段には、洗浄溶媒リザーバと大流量
送液が可能なポンプを備えていることが好ましい。大流
量送液とは例えば0.5μm程度のろ紙目を]Oml/
min程度に送液することをいう。
It is preferable that the cleaning solvent supply means is equipped with a cleaning solvent reservoir and a pump capable of feeding a large amount of liquid. Large flow rate liquid delivery is, for example, filter paper grain size of about 0.5 μm] Oml/
This means to send liquid at a rate of about min.

上記第一流路における試料ろ過部へは通常の送液ポンプ
が用いられ、製造ラインから試料を採取し以降の流路に
該試料を輸送する。
A normal liquid pump is used in the sample filtration section in the first flow path to collect a sample from the production line and transport the sample to the subsequent flow path.

この発明の装置の爾二流路に設けられた移動相溶媒供給
部には、移動相溶媒リザーバと送液ポンプを備えたもの
が適しており、該ポンプには通常の送液ポンプが用いら
れる。
The mobile phase solvent supply section provided in the second flow path of the apparatus of the present invention is suitably equipped with a mobile phase solvent reservoir and a liquid feeding pump, and a normal liquid feeding pump is used as the pump.

上記第一流路または第二流路いずれかへの試料転送用管
路の選択接続は、切り換えバルブを用いて行われるが、
この例では高圧六方バルブを用いるのが好ましい。該切
り換えバルブの切り換えのタイミングは、上記第一流路
のドレインの手前に試料計量ユニットを付設して、そこ
への溶液流入量により制御するのが好ましい。
Selective connection of the sample transfer pipe to either the first flow path or the second flow path is performed using a switching valve,
Preferably, a high pressure six-way valve is used in this example. The switching timing of the switching valve is preferably controlled by the amount of solution flowing into a sample measuring unit provided in front of the drain of the first channel.

この発明の装置の作動、制御等はマイクロコンピュータ
等を用いたコントローラにより操作されていてもよい。
The operation, control, etc. of the apparatus of this invention may be operated by a controller using a microcomputer or the like.

該コントローラは、試料希釈部、洗浄溶媒送液ポンプ、
切り換えバルブ及び三方弁総てに電気接続され、試料計
量ユニットからの信号に基づいて作動を制御するよう構
成されているものが好ましい。
The controller includes a sample dilution section, a cleaning solvent delivery pump,
Preferably, the switching valve and the three-way valve are electrically connected to each other and configured to control their operation based on signals from the sample metering unit.

(ホ)作用 この発明によれば、まず第一流路のろ過部とドレインと
の間に試料転送用管路が接続されて、希釈、ろ過された
試料が貯留され、次ぎに流路が切り換えられて第二流路
の移動相溶媒供給部と分析用カラムとの間に上記試料転
送用管路が接続され、該管路に貯留されていた試料か移
動相溶媒と共に分析カラムに輸送されそこで分析が行わ
れる。この後第一流路における二つの三方弁を切り換え
ることにより、洗浄溶媒供給手段から洗浄溶媒が逆流し
てフィルタを洗浄する。上記作動を所定の回数繰り返し
た後、ろ過部に設けた両端の切り換えバルブが同時に他
の同一のフィルタ管路に切り換わり以降上記と同様の操
作を繰り返すことになる。
(E) Function According to the present invention, first, a sample transfer pipe is connected between the filtration part of the first flow path and the drain, and the diluted and filtered sample is stored, and then the flow path is switched. The sample transfer pipe is connected between the mobile phase solvent supply section of the second channel and the analytical column, and the sample stored in the pipe is transported to the analytical column together with the mobile phase solvent and analyzed there. will be held. Thereafter, by switching the two three-way valves in the first flow path, the cleaning solvent flows back from the cleaning solvent supply means to clean the filter. After repeating the above operation a predetermined number of times, the switching valves at both ends of the filtration section are simultaneously switched to another same filter line, and the same operation as above is repeated thereafter.

以下実施例によりこの発明の詳細な説明するが、これに
よりこの発明は限定されるものではない。
The present invention will be described in detail below with reference to Examples, but the present invention is not limited thereby.

(へ)実施例 第1図には、この発明の装置の一例を示しである。図に
おいて液体クロマトグラフ装置(21)は、製造ライン
(20)から試料を採取する試料導入部(1)、試料希
釈部(2)及びろ過部(3)がこの順に管路接続されて
、さらにドレイン(a)へ延設される第一流路(A)と
、移動相溶媒リザーバ(4)、送液ポンプ(5)、分析
カラム(6)及び検出器(7)がこの順に管路接続され
てざらにドレイン(c)へ延設される第二流路(B)と
、試料を貯留し、次いで移動相溶媒と共に分析カラム(
6)に転送する試料転送用管路としてのサンプルループ
(8)とがそれぞれ6ボートバルブ(9)を介して接続
されている。
(F) Embodiment FIG. 1 shows an example of the apparatus of the present invention. In the figure, a liquid chromatograph device (21) includes a sample introduction section (1) for collecting a sample from a production line (20), a sample dilution section (2), and a filtration section (3) connected in this order through pipes. A first flow path (A) extending to the drain (a), a mobile phase solvent reservoir (4), a liquid feeding pump (5), an analytical column (6), and a detector (7) are connected in this order by piping. A second flow path (B) that extends to the drain (c) and a second flow path (B) where the sample is stored and then transferred to the analysis column (
A sample loop (8) serving as a sample transfer conduit for transferring the sample to 6) is connected to each sample via a 6-boat valve (9).

第一流路(A)において、試料希釈部(1)とろ過部(
3)との間にはラインフィルタ(1o)及び三方弁(1
1)が管路接続されており、該三方弁(11)からはド
レイン(b)への管路が設けられている。
In the first channel (A), the sample dilution section (1) and the filtration section (
3) and a line filter (1o) and three-way valve (1o).
1) is connected by a pipe line, and a pipe line is provided from the three-way valve (11) to a drain (b).

一方6ポートバルブ(9)とドレイン(a)との間には
、三方弁(12)及び試料計量ユニット(13)が管路
接続されており、上記三方弁(12)からはラインフィ
ルタ(14)、送液ポンプ(15)及び洗浄溶媒リザー
バ(16)がこの順で管路接続されている。
On the other hand, a three-way valve (12) and a sample measuring unit (13) are connected via a pipe line between the six-port valve (9) and the drain (a), and a line filter (14) is connected to the three-way valve (12). ), a liquid feeding pump (15), and a cleaning solvent reservoir (16) are connected in this order by pipes.

上記ろ過fJS(3)は、 この実施例では約0.5μ
mメツシュのメンブレンフィルタを6個(P、−F、)
使用し、フィルタを介在させた6本の管路のそれぞれの
両端に、7ボート6ポジシヨンの切り換えバルブ(17
)及び(18)により並列に管路接続されたものからな
り、意図する一本の管路を両端の切り換えバルブ(17
)及び(18)の切り換えにより選択可能となっている
The above filtration fJS (3) is approximately 0.5μ in this example.
6 m mesh membrane filters (P, -F,)
A 7-boat, 6-position switching valve (17
) and (18) are connected in parallel, and one intended pipe can be connected by switching valves (17) at both ends.
) and (18) can be selected.

コントローラ(19)はマイクロコンピュータからなり
、試料希釈部(2)、切り換えバルブ(17)及び(1
8)、6ポートバルブ(9)、三方弁(11)及び(1
2)並びに送液ポンプ(15)それぞれに電気接続され
、試料計量ユニット(13)からの信号等に基づいて上
記各接続部を制御する。
The controller (19) consists of a microcomputer, and includes a sample dilution section (2), a switching valve (17) and a
8), 6-port valve (9), 3-way valve (11) and (1
2) and the liquid feeding pump (15), and controls each of the above-mentioned connections based on signals from the sample measuring unit (13).

上記装置(21)において、まずコントローフう(19
)からの指令で、切り換えバルブ(17)及び(I8)
が図中の結線位置のポートに、かつ三方弁(11)、 
(12)及び6ポートバルブ(9)が実線側とされ、試
料導入部(1)より採取された試料は、約0.5〜bの
流量で試料希釈部(2)から三方弁(11)、切り換え
バルブ(17)、フィルタF5、切り換えバルブ(18
)、6ボートバルブ(9)の順に通ってサンプルループ
(8)にロードされ、 この際サンプルループ(8)内
の残留液(先の分析で残留する移動相溶媒等)は三方弁
(12)及び試料計量ユニット(13)を介してドレイ
ン(a)へ排出される。ここで試料計量ユニット(13
)は液面センサを内蔵し、サンプルループ(8)からド
レイン(a)に排出される液体の量を一時的にモニタし
うるような貯槽から構成されてなる。そして液面センサ
は前記サンプルループ(8)内の残留液が希釈試料で充
分に置換されるに必要なドレイン(a)への排出液体量
に相当する高さに位置されている。なお、この液面セン
サの位置を変化させることにより、サンプルループ(8
)内への希釈試料の導入量ひいては試料の第二流路(B
)・\の転送量を適宜制御することができる。
In the above device (21), first the controller (19)
), the switching valves (17) and (I8)
is connected to the port at the connection position in the figure, and the three-way valve (11),
(12) and the 6-port valve (9) are on the solid line side, and the sample collected from the sample introduction part (1) is passed from the sample dilution part (2) to the three-way valve (11) at a flow rate of about 0.5 to b. , switching valve (17), filter F5, switching valve (18)
), 6 boat valves (9), and loaded into the sample loop (8). At this time, residual liquid in the sample loop (8) (such as mobile phase solvent remaining from the previous analysis) is removed through the three-way valve (12). and is discharged to the drain (a) via the sample measuring unit (13). Here, the sample weighing unit (13
) consists of a storage tank with a built-in liquid level sensor that can temporarily monitor the amount of liquid discharged from the sample loop (8) to the drain (a). The liquid level sensor is positioned at a height corresponding to the amount of liquid discharged into the drain (a) necessary to sufficiently replace the residual liquid in the sample loop (8) with the diluted sample. In addition, by changing the position of this liquid level sensor, the sample loop (8
), and the amount of the diluted sample introduced into the second flow path (B
) and \ transfer amount can be controlled as appropriate.

またこのとき、第二流路(B)側では移動相溶媒が移動
相溶媒リザーバ(4)から送液ポンプ(5)により約0
.5〜2ml/minの流量で分析カラム(6)、検出
器(7)を通ってドレイン(c)へ排出されている。
At this time, on the second flow path (B) side, the mobile phase solvent is transferred from the mobile phase solvent reservoir (4) to the liquid feed pump (5) to approximately zero.
.. It passes through the analytical column (6) and the detector (7) and is discharged to the drain (c) at a flow rate of 5 to 2 ml/min.

所定債の試料がサンプルループ(8)にロードされると
、上記試料計量ユニット(13)内の液面セノサからの
信号に基づいてコントローラ(19)が作動し、試料導
入部(1)の吸引ポンプ及び試料希釈部(2)の吸引ポ
ンプが停止し、試料希釈部(2)からの試料の流れはと
まり、6ボートバルブ(9)は点線側流路に切り換わり
サンプルループ(8)にロードされていた試料が移動相
溶媒と共に分析カラム(6)に注入され分析が開始され
る。
When a predetermined amount of sample is loaded into the sample loop (8), the controller (19) is activated based on the signal from the liquid level sensor in the sample measuring unit (13), and the sample introduction section (1) is suctioned. The pump and the suction pump of the sample dilution section (2) stop, the flow of the sample from the sample dilution section (2) stops, and the 6-boat valve (9) switches to the dotted line side flow path and loads it into the sample loop (8). The sample that has been analyzed is injected into the analytical column (6) together with the mobile phase solvent, and analysis is started.

分析か開始されると、三方弁(11)及び(12)は点
線側流路に切り換わり送液ポンプ(15)から洗浄溶媒
が10m1/min程度のかなり大きな流量で三方弁(
12)、6ボートバルブ(9)、切り換えバルブ(18
)、フィルタF、、切り換えバルブ(17)、三方弁(
11)の順に逆流してフィルタF、に詰まっている粒子
を洗い落とし、該液はドレイン(b)へ排出される。
When analysis starts, the three-way valves (11) and (12) are switched to the dotted line side flow path, and the cleaning solvent is fed from the liquid feed pump (15) at a fairly large flow rate of about 10 ml/min to the three-way valve (11) and (12).
12), 6-boat valve (9), switching valve (18)
), filter F,, switching valve (17), three-way valve (
The liquid flows backward in the order of step 11) to wash away particles clogging the filter F, and the liquid is discharged to the drain (b).

一定時間の洗浄後、コントローラ(19)の指令により
、送液ポンプ(15)の動作は停止し、三方弁(+1)
及び(12)はそれぞれ図中の実線側流路の接続状態に
復帰し、−分析終了後6ボートバルブ(9)も実線側流
路に復帰する。そして再び製造ライン(20)からの試
料採取が行われ上記操作が繰り返される。
After cleaning for a certain period of time, the operation of the liquid pump (15) is stopped according to the command from the controller (19), and the three-way valve (+1)
and (12) respectively return to the connection state of the flow path on the solid line side in the figure, and - after the analysis is completed, the 6 boat valve (9) also returns to the flow path on the solid line side. Then, a sample is taken from the production line (20) again and the above operation is repeated.

一つのフィルタは設定回数使用後(例えば30回程度)
、コントローラ(19)からの指令により切り換えバル
ブ(17)及び(18〕は、別のフィルタ(例えばF、
 )を含む管路に切り換わる。このようにして順次、予
め並列に設定されたフィルタ管路が使用される。
One filter is used after a set number of times (for example, about 30 times)
, the switching valves (17) and (18) are switched to another filter (for example, F,
). In this way, filter lines previously set in parallel are used one after another.

(ト)発明の効果 一回の使用毎にフィルタを逆方向から洗浄するため、−
個のフィルタの使用可能回数が大幅に増加し、ラニング
コストを下げることができる。また意図する数のフィル
タを設置でき、これら複数個のフィルタを切り換えバル
ブによって自動的に使用できるため、自動運転に適した
構成とすることができる。さらに一つのフィルタの使用
中に他のフィルタを取り替えることが出来るため、フィ
ルタ交換中も装置を止めずに連続で作動できる。
(G) Effect of the invention Since the filter is cleaned from the reverse direction after each use, -
This greatly increases the number of times each filter can be used and reduces running costs. Further, since the intended number of filters can be installed and a plurality of filters can be automatically used by switching valves, a configuration suitable for automatic operation can be achieved. Furthermore, since one filter can be replaced while another filter is in use, the device can continue to operate without stopping even during filter replacement.

また、フィルタの代わりに試料前処理用のカラムを用い
るような流路構成も可能である。
Furthermore, a flow path configuration in which a column for sample pretreatment is used instead of a filter is also possible.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は、この発明の装置の一例の構成説明図である。 (1)・・・・試料導入部、   (2)・・・・・・
試料希釈部、(3)・・−・・ろ過部、  (4)・・
・・・・移動相溶媒リザーバ、(5)、(15)・・・
・・・送液ポンプ、  (6)・・・・・・分析カラム
、(7)・・・・検出部、    (8)・・・・・・
サンプルループ、(9)・・・・・・6ボートバルブ、 (10)、(+4)・−・・・・ラインフィルタ、(I
I)、(12)−・・・・三方弁、(13)・・−・・
試料計量ユニット、(16)・・・・・洗浄溶媒リザー
バ、(17)、(18)・・・・・切り換えバルブ、(
+9)・・・・・コントローラ、   (20)・・・
・・・製造ライン、(21)・・・この発明の装置、 (A)・・・・第一流路、       (B)・・・
・・第二流路、(F、)〜(F6)・・・・・・メンブ
レンフィルタ、(a) 、 (b) 、 (c)・・・
・・−ドレイン。
FIG. 1 is an explanatory diagram of the configuration of an example of the apparatus of the present invention. (1)...Sample introduction section, (2)...
Sample dilution section, (3)...Filtration section, (4)...
...Mobile phase solvent reservoir, (5), (15)...
... Liquid pump, (6) ... Analysis column, (7) ... Detection section, (8) ...
Sample loop, (9)... 6 boat valves, (10), (+4)... Line filter, (I
I), (12)---three-way valve, (13)------
Sample weighing unit, (16)...Washing solvent reservoir, (17), (18)...Switching valve, (
+9)...Controller, (20)...
...Production line, (21) ...Apparatus of the present invention, (A) ...First flow path, (B) ...
...Second flow path, (F,) to (F6)...Membrane filter, (a), (b), (c)...
...-Drain.

Claims (1)

【特許請求の範囲】 1、試料導入部から試料希釈部及びろ過部を介してドレ
インに延設される第一流路と、 移動相溶媒供給部から分析用カラム及び検出器を介して
ドレインに延設される第二流路と、切り換えバルブによ
り、第一流路のろ過部とドレインの間及び第二流路の移
動相供給部と分析用カラムの間のいずれかに接続される
試料転送用管路とから構成されてなり、第一流路のろ過
部を、フィルタを有する管路を複数本並設しかつこの両
端にこれらの管路のいずれかを選択して第一流路に接続
する二つの切り換えバルブで構成すると共に、第一流路
の下流に三方弁を介して洗浄溶媒を試料のろ過方向と逆
方向に切り換え導入しうる洗浄溶媒供給手段を設け、か
つ試料希釈部とろ過部の間に、上記逆方向への切り換え
導入時に第一流路を逆流する洗浄溶媒をドレインへ排出
しうる三方弁を設けたことを特徴とする液体クロマトグ
ラフ装置。
[Claims] 1. A first channel extending from the sample introduction section to the drain via the sample dilution section and the filtration section, and a first channel extending from the mobile phase solvent supply section to the drain via the analytical column and the detector. A sample transfer tube connected either between the filtration part and the drain in the first flow path or between the mobile phase supply part and the analytical column in the second flow path by means of a second flow path provided and a switching valve. The filtration section of the first flow path has a plurality of pipes each having a filter installed in parallel, and one of these pipes is connected to the first flow path by selecting one of these pipes at both ends. In addition to comprising a switching valve, a cleaning solvent supply means is provided downstream of the first flow path through a three-way valve to switch and introduce the cleaning solvent in a direction opposite to the filtration direction of the sample, and between the sample dilution section and the filtration section. . A liquid chromatograph apparatus, characterized in that a three-way valve is provided that can discharge the cleaning solvent flowing backward through the first flow path to the drain when the cleaning solvent is switched in the reverse direction.
JP60249709A 1985-11-06 1985-11-06 Liquid chromatographic device Pending JPS62108155A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60249709A JPS62108155A (en) 1985-11-06 1985-11-06 Liquid chromatographic device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60249709A JPS62108155A (en) 1985-11-06 1985-11-06 Liquid chromatographic device

Publications (1)

Publication Number Publication Date
JPS62108155A true JPS62108155A (en) 1987-05-19

Family

ID=17197034

Family Applications (1)

Application Number Title Priority Date Filing Date
JP60249709A Pending JPS62108155A (en) 1985-11-06 1985-11-06 Liquid chromatographic device

Country Status (1)

Country Link
JP (1) JPS62108155A (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01142458A (en) * 1987-11-30 1989-06-05 Yokogawa Electric Corp Measurement of cation with very low density
JPH0373847A (en) * 1989-03-18 1991-03-28 Hitachi Ltd Method and apparatus for analysis utilizing liquid chromatography
JPH04359148A (en) * 1991-06-05 1992-12-11 Eisai Co Ltd Liquid chromatograph
JPH05180822A (en) * 1991-12-20 1993-07-23 Shimadzu Corp Gas chromatograph analysis system of argon
JPH06138112A (en) * 1991-06-05 1994-05-20 G L Sci Kk Apparatus for removing impurity eluent
JPH06242094A (en) * 1993-02-15 1994-09-02 Tosoh Corp Filter incorporating column for liquid
JPH09178719A (en) * 1987-07-14 1997-07-11 Kdk Corp Automatic measuring method for glycohemoglobin
JP2012047633A (en) * 2010-08-27 2012-03-08 Toshiba Plant Systems & Services Corp Preprocessing apparatus for online type sample analyzer and method of controlling preprocessing apparatus for online type sample analyzer
EP2526396A1 (en) * 2010-01-19 2012-11-28 Bio-Rad Laboratories, Inc. Automated analyzer with low-pressure in-line filtration

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5124314U (en) * 1974-08-07 1976-02-23
JPS5633561B2 (en) * 1978-11-10 1981-08-04
JPS59157563A (en) * 1983-02-28 1984-09-06 Shimizu Constr Co Ltd Molecular sieve type liquid chromatograph

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5124314U (en) * 1974-08-07 1976-02-23
JPS5633561B2 (en) * 1978-11-10 1981-08-04
JPS59157563A (en) * 1983-02-28 1984-09-06 Shimizu Constr Co Ltd Molecular sieve type liquid chromatograph

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09178719A (en) * 1987-07-14 1997-07-11 Kdk Corp Automatic measuring method for glycohemoglobin
JPH01142458A (en) * 1987-11-30 1989-06-05 Yokogawa Electric Corp Measurement of cation with very low density
JPH0373847A (en) * 1989-03-18 1991-03-28 Hitachi Ltd Method and apparatus for analysis utilizing liquid chromatography
JPH04359148A (en) * 1991-06-05 1992-12-11 Eisai Co Ltd Liquid chromatograph
JPH06138112A (en) * 1991-06-05 1994-05-20 G L Sci Kk Apparatus for removing impurity eluent
JPH05180822A (en) * 1991-12-20 1993-07-23 Shimadzu Corp Gas chromatograph analysis system of argon
JPH06242094A (en) * 1993-02-15 1994-09-02 Tosoh Corp Filter incorporating column for liquid
EP2526396A1 (en) * 2010-01-19 2012-11-28 Bio-Rad Laboratories, Inc. Automated analyzer with low-pressure in-line filtration
JP2013517484A (en) * 2010-01-19 2013-05-16 バイオ−ラッド ラボラトリーズ,インコーポレイティド Automatic analyzer with low-pressure in-line filter action
US8733152B2 (en) 2010-01-19 2014-05-27 Bio-Rad Laboratories, Inc. Automated analyzer with low-pressure in-line filtration
EP2526396A4 (en) * 2010-01-19 2014-07-23 Bio Rad Laboratories Automated analyzer with low-pressure in-line filtration
JP2012047633A (en) * 2010-08-27 2012-03-08 Toshiba Plant Systems & Services Corp Preprocessing apparatus for online type sample analyzer and method of controlling preprocessing apparatus for online type sample analyzer

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