JPS6385356A - Liquid feed apparatus for chromatography - Google Patents

Liquid feed apparatus for chromatography

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Publication number
JPS6385356A
JPS6385356A JP23099986A JP23099986A JPS6385356A JP S6385356 A JPS6385356 A JP S6385356A JP 23099986 A JP23099986 A JP 23099986A JP 23099986 A JP23099986 A JP 23099986A JP S6385356 A JPS6385356 A JP S6385356A
Authority
JP
Japan
Prior art keywords
pressure
flow rate
liquid
pump
discharge
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
JP23099986A
Other languages
Japanese (ja)
Inventor
Akinori Kiyofuji
章典 清藤
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 JP23099986A priority Critical patent/JPS6385356A/en
Publication of JPS6385356A publication Critical patent/JPS6385356A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To feed a liquid with high flow rate accuracy, by providing a pressure detection means for detecting the discharge pressure of a pump and operating the variation rate of the discharge pressure to control the rotational speed of the drive means of the pump. CONSTITUTION:A pressure detector 10 is connected to the pipe 8 connecting a plunger pump 1 and an analytic column 9. When a liquid is received in a carrier liquid tank 7 and the flow rate of the liquid is set by a flow rate setting device 17, a flow rate control circuit 16 drives a motor 3 and the liquid is discharged at a flow rate coinciding with a set flow rate. The pressure at the time when the discharge pressure rises by the resistance of the fluid of the column 9 to reach a steady state and the pressure at the time when said discharge pressure becomes the min. pressure are detected by detection circuits 12, 13 and a pressure variation rate is calculated by a divider circuit 15. The set value of the setting device 17 is corrected on the basis of said pressure variation rate by the flow rate control circuit 16 and the number of rotations of the motor 3 are altered to hold the discharge flow rate of the pump 1 to a set value.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、高圧力により液体をカラムに圧送するクロマ
トグラフィ用送液装フにおける流量補正技術に関する。
DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a flow rate correction technique in a liquid feeding device for chromatography that pumps liquid to a column under high pressure.

(従来技術) 液体クロマトグラフやイオンクロマトグラフにおいては
、流体抵抗が極めて大きな分析用カラムにキャリア液を
供給するため通常数百に9/am2程度の吐出圧をもつ
ポンプが使用されている。
(Prior Art) In liquid chromatographs and ion chromatographs, pumps with a discharge pressure of about several hundred to 9/am2 are usually used to supply carrier liquid to analytical columns with extremely high fluid resistance.

ところで、このような数百に9/cm”という高い圧力
を受けると、水のように圧縮率の小さな液体でも2%程
度体積の収縮か生じ、またクロマトグラムのキャリア液
に多用されるノルマへキサンにあっては5%以上もの収
縮が生じるため、カラムへのキャリア液の供給】が圧力
に左右されて分析結果に誤差を生じることになる。
By the way, when subjected to such a high pressure of several hundred to 9/cm", even a liquid with a small compressibility such as water will shrink by about 2% in volume, and the norm, which is often used as a carrier liquid in chromatograms, will shrink by about 2%. Since xane shrinks by more than 5%, the supply of carrier liquid to the column depends on the pressure, causing errors in analysis results.

すなわち、ブラシジャポンプは、プランジャ径rとスト
ローク長ρIこよって決る容積3%1工程の吐出量とす
るが、液体の収縮が無視できない場合(こは、圧縮率を
β、吐出圧をPとすると、実際には5(1−βP)L/
か吐出されず、89分か誤差となる。このため、流1f
flfモニターしながらポンプの動作速度を制御するこ
とも考えられるが、高圧用流量計は極めて高価であるば
かりでなく、高々lcc/分程度の微小な流量を高い精
度で測定することは極めて困難で実用的な装=は存在し
ない。
In other words, the brush jar pump has a volume of 3% and a discharge amount per process determined by the plunger diameter r and stroke length ρI, but if the contraction of the liquid cannot be ignored (in this case, the compression ratio is β and the discharge pressure is P). Then, actually 5(1-βP)L/
However, the liquid was not discharged, resulting in an error of 89 minutes. For this reason, the flow 1f
It is possible to control the pump operating speed while monitoring flf, but high-pressure flowmeters are not only extremely expensive, but also extremely difficult to measure minute flow rates of at most lcc/min with high accuracy. There is no practical outfit.

このような問題を解消するため、送液圧と液体の収縮特
性を予め加味してポンプの駆動速度を設定して、収縮に
よる供給量の変化分BPを補正する方法も提案されてい
るが、キャリア液毎に補正量を変更する必要があって手
間を要するばかりでなく、2種類の溶媒の混合率を時間
的に変化させながら分析を行なうグラシュエンド法にあ
っては補正が極めて困難であるという問題があった。
In order to solve this problem, a method has been proposed in which the pump drive speed is set in advance by considering the liquid delivery pressure and the contraction characteristics of the liquid, and the change in supply amount BP due to contraction is corrected. Not only is it necessary to change the correction amount for each carrier liquid, which is time-consuming, but it is also extremely difficult to make corrections in the Grass-end method, which performs analysis while changing the mixing ratio of two types of solvent over time. There was a problem.

(目的) 本発明はこのような問題に鑑みてなされたものであって
、その目的とするところは移送すべき液体の収縮度を常
時検出してポンプの送液能力を自動的に補正することが
できる新規なりロマトグラフ用送液装置を提供すること
を目的とする。
(Purpose) The present invention has been made in view of these problems, and its purpose is to constantly detect the degree of contraction of the liquid to be transferred and automatically correct the liquid feeding capacity of the pump. The purpose of the present invention is to provide a novel liquid feeding device for romatographs that can perform the following steps.

(実施例) そこで、以下に本発明の詳細を図示した実施例に基づい
て説明する。
(Example) The details of the present invention will be described below based on illustrated examples.

第1図は、本発明の一実施例を示すものであって、図中
符号1は、偏心カム2を介して可変速モータ3により1
80度の機械的位相差をもって駆動されるプランジャ4
a、5aと、これに共働するシリンダ4b、5bを備え
たプランジャポンプで、それぞれの吸引口4C15Cは
バイブロによりキャリア液槽7が、また吐出口4d、5
dにはバイブ8により分析用カラム9を接続してなる従
来の高速液体クロマトグラフ装置の送液システムにおい
て、ポンプ1の吐出口4d、5dと高速液体クロマトグ
ラフ用カラム9を結ぶバイブ8には、例えば液圧を受け
るダイヤフラムに10aにストレインゲージ10111
1取付けてなる圧力検出器10を接続して、カラム9へ
の送液圧を電気信号に変換して検出するように構成され
ている。
FIG. 1 shows an embodiment of the present invention, in which reference numeral 1 indicates a motor driven by a variable speed motor 3 via an eccentric cam 2.
Plunger 4 driven with a mechanical phase difference of 80 degrees
a, 5a and cylinders 4b, 5b working together, each suction port 4C15C is connected to the carrier liquid tank 7 by vibro, and the discharge ports 4d, 5
In a conventional liquid delivery system of a high-performance liquid chromatograph apparatus, in which an analytical column 9 is connected to the column 9 by a vibrator 8, the vibrator 8 that connects the discharge ports 4d and 5d of the pump 1 and the column 9 for high-performance liquid chromatograph is connected to the column 9 for analysis by a vibrator 8. For example, a strain gauge 10111 is attached to the diaphragm 10a that receives hydraulic pressure.
A pressure detector 10 attached to the column 9 is connected to the column 9 to convert the liquid feeding pressure to the column 9 into an electric signal and detect it.

11は、圧力変動率演算回路で、圧力検出器1oの出力
から定常圧力Ps (第2図)を検出する定常圧力検出
回路12と、最低圧力PL1Fr検出する最低圧力検出
回路13と、これら両回路12.13からの信号の差分
から圧力変動幅ΔPを検出する圧力変動幅検出回路14
と、圧力変動幅ΔPと定常圧力Psの比を求める割算回
路15かうなり、圧力検出器1oの出力に基づいて圧力
変動率信号を出力するように構成されている。
Reference numeral 11 denotes a pressure fluctuation rate calculation circuit, which includes a steady pressure detection circuit 12 that detects the steady pressure Ps (Fig. 2) from the output of the pressure detector 1o, a minimum pressure detection circuit 13 that detects the minimum pressure PL1Fr, and both of these circuits. 12. Pressure fluctuation width detection circuit 14 that detects the pressure fluctuation width ΔP from the difference in signals from 13.
Then, a division circuit 15 for determining the ratio between the pressure fluctuation range ΔP and the steady pressure Ps is configured to output a pressure fluctuation rate signal based on the output of the pressure detector 1o.

16は、流量制御回路で、流量設定器17からの出力信
号を圧力変動率信号に基づいて補正し、この結果に対応
してモータの回転数を決定するように構成されている。
16 is a flow control circuit configured to correct the output signal from the flow rate setting device 17 based on the pressure fluctuation rate signal, and determine the rotation speed of the motor in accordance with this result.

なお、図中符号18は、流量制御回路16からの信号に
一致した回転速度でモータ3を駆動させるモータ駆動回
路を示す。
Note that reference numeral 18 in the figure indicates a motor drive circuit that drives the motor 3 at a rotational speed that matches the signal from the flow rate control circuit 16.

この実施例において、キャリア液槽7に液体を収容して
流量設定器17により所望流量を設定すると、流量制御
回路16は、流量設定器17からの信号に一致した回転
数によつモータ2を駆動して、ポンプ1から設定量に一
敗した流量の流体を吐出せしめようとする。しかしなが
ら、前述したようにクロマトグラフ用カラム9の流体抵
抗が極めて大きいため、ポンプ1からの吐出圧力が上昇
する。このため、ポンプ1に吸込まれたキャリア液は、
ポンプの吐出工程において、その液体の圧縮率と圧力に
より定まる比率でもって圧縮を受け、前述したように圧
縮率VB、吐出圧をPとすると、実際には収縮度βP分
少なくなって(1−βP)だけが吐出される。
In this embodiment, when the carrier liquid tank 7 is filled with liquid and the desired flow rate is set by the flow rate setting device 17, the flow rate control circuit 16 controls the motor 2 at a rotation speed that matches the signal from the flow rate setting device 17. The pump 1 attempts to drive the pump 1 to discharge fluid at a flow rate that is slightly below the set amount. However, as described above, the fluid resistance of the chromatographic column 9 is extremely large, so the discharge pressure from the pump 1 increases. Therefore, the carrier liquid sucked into pump 1 is
In the discharge process of the pump, the liquid is compressed at a ratio determined by the compressibility and pressure, and as mentioned above, if the compression ratio is VB and the discharge pressure is P, the actual contraction rate is reduced by the degree of contraction βP (1- Only βP) is discharged.

一方、プランジャポンプ1は、各プランジャの行程位相
、’1180’ずらせて吸引行程と吐出行程を交互に組
合わせて可及的に圧力変動率を小さくするように構成さ
れている。この圧力変動率は通常ポンプ自体の機構的要
因によって一義的に決まるものであるが、送液すべき流
体の収縮が無視できない場合1こは、ポンプの吐出工程
の開始によりシリンダ内において圧縮を受けて徐々に吐
出可能な圧力に至るため、この期間が無吐出状態となっ
て、圧力変動率が流体の収縮度BPに比例して大きくな
る(第2図口、ハ)。
On the other hand, the plunger pump 1 is configured to shift the stroke phase of each plunger by '1180' and alternately combine suction strokes and discharge strokes to reduce the rate of pressure fluctuation as much as possible. This rate of pressure fluctuation is usually uniquely determined by the mechanical factors of the pump itself, but if the contraction of the fluid to be pumped cannot be ignored (1), the pressure fluctuation rate may be compressed in the cylinder by the start of the pump's discharge stroke. Since the pressure gradually reaches a level at which discharge is possible, there is no discharge during this period, and the rate of pressure fluctuation increases in proportion to the degree of contraction BP of the fluid (Figure 2, Part 3).

この吐出行程において、吐出圧が定常状態となった時点
の圧力Psを定常圧力検出回路12が、また最低圧PL
を最低圧検出回路13が検出する。これら各検出信号は
、圧力変動幅検出回路14において圧力変動幅ΔPを演
算され、ついで割算回路15においてΔP / P s
、つ走り圧力変動率を計算される。流量制御回路16は
、この収縮層演算回路11からの信号を受けて設定器1
7の設定値を圧力変動率に基づいて補正してモータ3の
回転数を変更古せ、ポンプ1の駆動速度、つまりポンプ
]のストローク速度を変更させて吐出する液体の流量を
設定値に維持きせる。
In this discharge stroke, the steady pressure detection circuit 12 detects the pressure Ps at the time when the discharge pressure reaches a steady state, and also detects the lowest pressure PL.
is detected by the lowest pressure detection circuit 13. For each of these detection signals, a pressure fluctuation width ΔP is calculated in a pressure fluctuation width detection circuit 14, and then a pressure fluctuation width ΔP is calculated in a division circuit 15.
, the pressure fluctuation rate is calculated. The flow rate control circuit 16 receives the signal from the contraction layer calculation circuit 11 and controls the setting device 1.
7 is corrected based on the pressure fluctuation rate to change the rotation speed of motor 3, and the drive speed of pump 1, that is, the stroke speed of the pump, is changed to maintain the flow rate of the discharged liquid at the set value. I can make it.

以下、このような過程を繰返しながら送給すべき液体の
収縮度に追従しながらポンプの駆動速度を調整して、流
量を設定値に維持する。
Thereafter, while repeating such a process, the drive speed of the pump is adjusted while following the degree of contraction of the liquid to be delivered, and the flow rate is maintained at the set value.

なお、この実施例においては、説明を簡素化するため、
流体の圧縮率が一定である合を例に採って説明したが、
温度変化により圧縮率が時間的に変動した場合や、複数
の液体の混合率を時間的に変化させながら分析を行なう
グラディエンド分析のキャリア液の送給においても、時
々刻々の圧縮率が検出できるため、その収縮度の変化に
間わりなく設定流量を維持して送液することができる。
In addition, in this example, in order to simplify the explanation,
The explanation was given using an example where the compressibility of the fluid is constant.
The moment-to-moment compressibility can be detected even when the compressibility changes over time due to temperature changes, or when feeding the carrier liquid for gradient-end analysis, where analysis is performed while changing the mixing ratio of multiple liquids over time. Therefore, the liquid can be fed while maintaining the set flow rate regardless of changes in the degree of contraction.

また、本発明においては2シリンダ型のプランジャポン
プに例を採って説明したが、3シリンダ以上のものであ
っても同様に適用でき、ざらには翼車型のものにも適用
できることは明らかである。
In addition, although the present invention has been explained by taking an example of a two-cylinder plunger pump, it is obvious that it can be similarly applied to a plunger pump with three or more cylinders, and in general, it can also be applied to a blade-type plunger pump. .

(効果) 以上、説明したように本発明によれば、ポンプの圧力変
動率が液体の収縮度に依存することを積極的に利用して
圧力変動率に基づいてポンプの駆動速度を補正するよう
にしたので、高耐圧像量流量計を不要としで、高圧力で
かつ微小な流体を高い流量精度で送液することができ、
特に移送すべき流体が多種に亘るクロマトグラフ装置に
あっては多大な効果を奏する。
(Effects) As described above, according to the present invention, the fact that the pressure fluctuation rate of the pump depends on the degree of contraction of the liquid is actively utilized to correct the pump drive speed based on the pressure fluctuation rate. This eliminates the need for a high-pressure image volume flowmeter, and enables the delivery of high-pressure, minute fluids with high flow rate accuracy.
This is particularly effective in chromatographic apparatuses in which a wide variety of fluids are to be transferred.

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

第1図は、本発明の一実施例を示す装置の構成図、第2
図は、同上装置の動作を示す説明図である。 1・・・・プランジャポンプ  2・・・・偏心カム3
・・・・可変速度型モータ  7・・・・キャリア液槽
9・・・・分析用カラム    10・・・・圧力検出
器11・・・・圧力変動率検出回路 17・・・・流量設定器 出願人  株式会社 島津製作所 代理人 弁理士 西 川 贋 治 同 木村勝彦 第1図 /′ 第2図 (イ) ρ。
FIG. 1 is a configuration diagram of an apparatus showing one embodiment of the present invention, and FIG.
The figure is an explanatory diagram showing the operation of the same device. 1... Plunger pump 2... Eccentric cam 3
... Variable speed motor 7 ... Carrier liquid tank 9 ... Analysis column 10 ... Pressure detector 11 ... Pressure fluctuation rate detection circuit 17 ... Flow rate setting device Applicant Shimadzu Corporation Representative Patent Attorney Haruto Nishikawa Katsuhiko Kimura Figure 1/' Figure 2 (A) ρ.

Claims (1)

【特許請求の範囲】[Claims] 変速可能な駆動手段に接続されたポンプ手段と、該手段
の吐出圧を検出する圧力検出手段と、吐出圧の圧力変動
率を演算する手段と、前記圧力変動率により流量設定値
を補正して前記駆動手段の回転速度を制御する手段を備
えてなるクロマトグラフィ用送液装置。
A pump means connected to a variable speed driving means, a pressure detection means for detecting the discharge pressure of the means, a means for calculating a pressure fluctuation rate of the discharge pressure, and a flow rate setting value corrected by the pressure fluctuation rate. A liquid feeding device for chromatography, comprising means for controlling the rotational speed of the driving means.
JP23099986A 1986-09-29 1986-09-29 Liquid feed apparatus for chromatography Pending JPS6385356A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP23099986A JPS6385356A (en) 1986-09-29 1986-09-29 Liquid feed apparatus for chromatography

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP23099986A JPS6385356A (en) 1986-09-29 1986-09-29 Liquid feed apparatus for chromatography

Publications (1)

Publication Number Publication Date
JPS6385356A true JPS6385356A (en) 1988-04-15

Family

ID=16916645

Family Applications (1)

Application Number Title Priority Date Filing Date
JP23099986A Pending JPS6385356A (en) 1986-09-29 1986-09-29 Liquid feed apparatus for chromatography

Country Status (1)

Country Link
JP (1) JPS6385356A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0255886A (en) * 1988-08-15 1990-02-26 Viking Pump Inc Terminal-element
JP2015502843A (en) * 2011-11-09 2015-01-29 ユーオーピー エルエルシー Improving energy efficiency in adsorptive separations.

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0255886A (en) * 1988-08-15 1990-02-26 Viking Pump Inc Terminal-element
JP2015502843A (en) * 2011-11-09 2015-01-29 ユーオーピー エルエルシー Improving energy efficiency in adsorptive separations.

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