JPH0249762B2 - - Google Patents
Info
- Publication number
- JPH0249762B2 JPH0249762B2 JP59112586A JP11258684A JPH0249762B2 JP H0249762 B2 JPH0249762 B2 JP H0249762B2 JP 59112586 A JP59112586 A JP 59112586A JP 11258684 A JP11258684 A JP 11258684A JP H0249762 B2 JPH0249762 B2 JP H0249762B2
- Authority
- JP
- Japan
- Prior art keywords
- vacuum chamber
- polymer membrane
- eluent
- temperature
- liquid chromatograph
- 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.)
- Expired - Lifetime
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0063—Regulation, control including valves and floats
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Degasification And Air Bubble Elimination (AREA)
Description
【発明の詳細な説明】
技術分野
本発明は、液体クロマトグラフによる分析にお
いて、溶離液中に溶存する空気を除去する液体ク
ロマトグラフ用脱気装置に関する。DETAILED DESCRIPTION OF THE INVENTION Technical Field The present invention relates to a deaerator for a liquid chromatograph that removes air dissolved in an eluent during analysis using a liquid chromatograph.
従来技術
液体クロマトグラフにより分離、分析を行なう
場合、その分析性能を向上させるため、溶離液中
の溶存空気を除去する液体クロマトグラフ用脱気
装置（以下脱気装置という）が使用されるように
なつてきた。Prior Art When performing separation and analysis using a liquid chromatograph, a deaerator for liquid chromatographs (hereinafter referred to as a deaerator) has been used to remove dissolved air in the eluent in order to improve the analytical performance. I'm getting old.
一般に上記脱気装置Ａは、第２図にそのフロー
を示すように、スパイラルチユーブ状高分子膜１
が内蔵された真空チヤンバ２と、この真空度を検
出して、制御回路３を介して、上記真空チヤンバ
２の内圧を低下させる真空ポンプ４を始動或いは
停止させる圧力センサ５によつて構成されてい
る。 In general, the degassing device A has a spiral tube-shaped polymer membrane 1, as shown in FIG.
It is composed of a vacuum chamber 2 with a built-in vacuum chamber 2, and a pressure sensor 5 that detects the degree of vacuum and starts or stops a vacuum pump 4 that lowers the internal pressure of the vacuum chamber 2 via a control circuit 3. There is.
上記脱気装置Ａによつて溶離液６中に溶存する
空気を除去する場合には、真空チヤンバ２の内圧
を所定の範囲の減圧状態に保持しながら、溶離液
６をチユーブ状高分子膜内を所定速度で通過させ
ることにより溶存空気をチユーブ状高分子膜１を
通して真空チヤンバ２内にに拡散させ除去し、空
気の除去された溶離液６を液体クロマトグラフ７
に供給している。 When removing air dissolved in the eluent 6 using the deaerator A, the eluent 6 is pumped into the tube-shaped polymer membrane while maintaining the internal pressure of the vacuum chamber 2 within a predetermined range of reduced pressure. Dissolved air is diffused and removed through the tubular polymer membrane 1 into the vacuum chamber 2 by passing through it at a predetermined speed, and the eluent 6 from which the air has been removed is transferred to the liquid chromatograph 7.
is supplied to.
従来技術の問題点
ところで、上記脱気装置によつて溶存する空気
を除去する速度は相当の幅で変動し、残存空気濃
度は一定せず、そのため液体クロマトグラフの性
能が安定しないばかりでなく、十分な除去が行な
われないことがあつた。Problems with the Prior Art By the way, the speed at which dissolved air is removed by the deaerator described above fluctuates over a considerable range, and the residual air concentration is not constant, which not only makes the performance of the liquid chromatograph unstable; In some cases, sufficient removal was not carried out.
本発明の目的および構成
本発明は、上記の事情に鑑み、鋭意研究した結
果、上記チユーブ状高分子膜内に溶離液を通過さ
せて溶存する空気を高分子膜を透過させて除去す
る際の除去速度は、真空チヤンバ内の温度によつ
ても、大幅に変ることを知見した。Object and Structure of the Present Invention In view of the above circumstances, the present invention has been developed as a result of intensive research, and has been developed to provide a method for removing dissolved air by passing an eluent through the tubular polymer membrane and removing dissolved air through the polymer membrane. It has been found that the removal rate also varies significantly depending on the temperature within the vacuum chamber.
本発明は上記の知見に基づいてなされたもの
で、安定な性能を有する脱気装置を提供すること
を目的とするもので、その要旨は、液体クロマト
グラフへ供給する、気体を溶存した溶離液を、真
空チヤンバ内に設けたチユーブ状高分子膜内を通
過させて、溶存する気体を除去する液体クロマト
グラフ用脱気装置において、前記真空チヤンバの
外側底部に、前記チユーブ状高分子膜を所定の温
度に保持する自己制御型面ヒータを設けている脱
気装置にある。 The present invention has been made based on the above findings, and aims to provide a degassing device with stable performance. In a deaerator for liquid chromatography in which dissolved gas is removed by passing through a tubular polymer membrane provided in a vacuum chamber, the tubular polymer membrane is placed in a predetermined position on the outer bottom of the vacuum chamber. The degassing device is equipped with a self-regulating surface heater that maintains the temperature at .
本発明の具体的構成、効果
第１図は、本発明に係る脱気装置の一実施例を
示すもので、第２図と同一部分には同一符号を付
してその説明を省略する。図中符号１１は、チユ
ーブ状高分子膜１が内蔵された真空チヤンバ２外
側底部に設けられ、その内部を所定の温度に加温
する公知の自己制御型面ヒータである。また、本
発明において用いられる高分子膜としては、通常
ポリ四フツ化エチレン、等が用いられる。Specific Structure and Effects of the Present Invention FIG. 1 shows an embodiment of a degassing device according to the present invention, and the same parts as those in FIG. 2 are given the same reference numerals, and the explanation thereof will be omitted. Reference numeral 11 in the figure is a known self-control type surface heater that is provided at the outer bottom of the vacuum chamber 2 in which the tubular polymer membrane 1 is built-in, and that heats the inside of the vacuum chamber 2 to a predetermined temperature. Further, as the polymer membrane used in the present invention, polytetrafluoroethylene or the like is usually used.
上記脱気装置Ａの真空チヤンバ２内部を所定の
温度、圧に保持して、空気を溶存した溶離液を一
定速度で通過させると、溶離液６中の溶存空気
は、ほぼ同じ量が除去され、通過した溶離液中の
溶存空気はほぼ一定濃度に低下され、液体クロマ
トグラフに好適に使用される。 When the inside of the vacuum chamber 2 of the deaerator A is maintained at a predetermined temperature and pressure and the eluent containing dissolved air is passed through at a constant speed, approximately the same amount of dissolved air in the eluent 6 is removed. , the dissolved air in the eluent that has passed through the eluent is reduced to a nearly constant concentration, and is suitably used in liquid chromatography.
この場合、温度が高い方が、空気の残存濃度が
低下する。これは、高分子膜１の気体拡散速度が
高くなるためである。しかし、温度が高すぎる
と、液体の蒸気も透過するようになるので、40℃
以下の温度に保持するのが好ましい。 In this case, the higher the temperature, the lower the residual concentration of air. This is because the gas diffusion rate of the polymer membrane 1 increases. However, if the temperature is too high, liquid vapor will also pass through, so 40℃
It is preferable to maintain the temperature at the following temperature.
なお、真空チヤンバ２内部を所定温度に加温す
るとともに、チユーブ状高分子膜１に導入する溶
離液６を上記温度に加温しても、真空チヤンバ２
のみを加温した場合と差が認められない。これ
は、上記チユーブ状高分子膜１内に導入された溶
離液６が、比較的早く昇温し、真空チヤンバ１内
部と同じ温度となるためと思料する。また、上記
説明では、加熱手段として自己制御型面ヒータを
用いたがこれに限るものでなく、所定温度に真空
チヤンバ２内を加熱出来るものであればよい。 Note that even if the inside of the vacuum chamber 2 is heated to a predetermined temperature and the eluent 6 introduced into the tubular polymer membrane 1 is heated to the above temperature, the vacuum chamber 2
No difference was observed compared to when only the sample was heated. This is thought to be because the temperature of the eluent 6 introduced into the tubular polymer membrane 1 rises relatively quickly to reach the same temperature as the inside of the vacuum chamber 1. Further, in the above description, a self-controlled surface heater is used as the heating means, but the heating means is not limited to this, and any device that can heat the inside of the vacuum chamber 2 to a predetermined temperature may be used.
実施例 次に実施例を示して本発明を説明する。Example Next, the present invention will be explained with reference to Examples.
真空チヤンバ２内に内径：1.8mm、外径：2.2
mm、長さ：10mのパイプ状ポリ四フツ化エチレン
膜を設け、真空チヤンバ２内を圧力：50Torr、
温度：10、20、30℃の温度で、酸素：10ppm溶存
する蒸溜水を通過させ、通過した蒸溜水中の溶存
酸素濃度を測定した。 Inside vacuum chamber 2: Inner diameter: 1.8mm, Outer diameter: 2.2
A pipe-shaped polytetrafluoroethylene membrane with a length of 10 m was installed, and the pressure inside the vacuum chamber 2 was 50 Torr.
Distilled water containing 10 ppm dissolved oxygen was passed through the tube at temperatures of 10, 20, and 30°C, and the dissolved oxygen concentration in the passing distilled water was measured.
その結果、真空チヤンバ２内部が一定温度で通
過した蒸溜水中の酸素濃度はほぼ一定であり、温
度を変えた場合の、通過した蒸溜水中の酸素濃度
は、10℃：5.2ppm、20℃：3.7ppm、30℃：
3.2ppmであつた。10℃の場合と30℃の場合とで
は、30℃の方が除去率が大幅によくなることわか
る。 As a result, the oxygen concentration in the distilled water that passed inside the vacuum chamber 2 at a constant temperature was almost constant, and when the temperature was changed, the oxygen concentration in the distilled water that passed through the vacuum chamber 2 was 5.2ppm at 10℃ and 3.7ppm at 20℃. ppm, 30℃:
It was 3.2ppm. It can be seen that the removal rate is significantly better at 30°C than at 10°C.
本発明の効果
以上述べたように本発明に係る脱気装置は、真
空チヤンバ内の温度を上昇せしめて一定範囲に保
持することにより、大幅、かつ一定の脱気が可能
となり、液体クロマトグラフ分離性能を安定して
向上せしめるものである。Effects of the Present Invention As described above, the deaerator according to the present invention enables significant and constant degassing by increasing the temperature inside the vacuum chamber and maintaining it within a certain range, thereby making it possible to perform liquid chromatography separation. This improves performance stably.
第１図は本発明に係る脱気装置の一実施例を示
すフロー図、第２図は、従来の脱気用装置のフロ
ー図である。
１……チユーブ状高分子膜、２……真空チヤン
バ、３……制御回路、４……真空ポンプ、５……
圧力センサ、６……溶離液、７……液体クロマト
グラフ、１１……自己制御型面ヒータ（加熱手
段）、Ａ……脱気装置。
FIG. 1 is a flow diagram showing an embodiment of a degassing device according to the present invention, and FIG. 2 is a flow diagram of a conventional degassing device. 1...Tubular polymer membrane, 2...Vacuum chamber, 3...Control circuit, 4...Vacuum pump, 5...
Pressure sensor, 6... Eluent, 7... Liquid chromatograph, 11... Self-controlled surface heater (heating means), A... Deaerator.
Claims (1)
した溶離液を、真空チヤンバ内に設けたチユーブ
状高分子膜内を通過させて、溶存する気体を除去
する液体クロマトグラフ用脱気装置において、前
記真空チヤンバの外側底部に、前記チユーブ状高
分子膜を所定の温度に保持する自己制御型面ヒー
タを設けていることを特徴とする液体クロマトグ
ラフ用脱気装置。1. In a degassing device for a liquid chromatograph, which removes the dissolved gas by passing an eluent containing dissolved gas to the liquid chromatograph through a tubular polymer membrane provided in a vacuum chamber, the vacuum 1. A degassing device for a liquid chromatograph, characterized in that a self-controlled surface heater for maintaining the tubular polymer membrane at a predetermined temperature is provided at the outer bottom of the chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11258684A JPS60255120A (en) | 1984-06-01 | 1984-06-01 | Deaeration apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11258684A JPS60255120A (en) | 1984-06-01 | 1984-06-01 | Deaeration apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60255120A JPS60255120A (en) | 1985-12-16 |
| JPH0249762B2 true JPH0249762B2 (en) | 1990-10-31 |
Family
ID=14590435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11258684A Granted JPS60255120A (en) | 1984-06-01 | 1984-06-01 | Deaeration apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60255120A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62204086A (en) * | 1986-03-04 | 1987-09-08 | 株式会社エルマ、シーアール | Pipe |
| JPH01215312A (en) * | 1988-02-22 | 1989-08-29 | Takuma Co Ltd | Method for removing dissolved gas in liquid |
| JPH09162118A (en) * | 1995-12-11 | 1997-06-20 | Dainippon Screen Mfg Co Ltd | Degassing device for processing liquid for substrates |
| JP5260967B2 (en) * | 2006-02-09 | 2013-08-14 | アークレイ株式会社 | Liquid chromatography device |
| US20250387733A1 (en) * | 2022-06-27 | 2025-12-25 | Dic Corporation | Deaerator |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2907188A1 (en) * | 1978-02-24 | 1979-08-30 | Du Pont | DEGASSING DEVICE |
| JPS615928Y2 (en) * | 1980-06-04 | 1986-02-22 |
-
1984
- 1984-06-01 JP JP11258684A patent/JPS60255120A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60255120A (en) | 1985-12-16 |
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