JPS61223555A - Analysis of ion species and apparatus using the same - Google Patents
Analysis of ion species and apparatus using the sameInfo
- Publication number
- JPS61223555A JPS61223555A JP6463285A JP6463285A JPS61223555A JP S61223555 A JPS61223555 A JP S61223555A JP 6463285 A JP6463285 A JP 6463285A JP 6463285 A JP6463285 A JP 6463285A JP S61223555 A JPS61223555 A JP S61223555A
- Authority
- JP
- Japan
- Prior art keywords
- eluent
- liquid
- ion species
- column
- detector
- 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.)
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Links
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- Treatment Of Liquids With Adsorbents In General (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は、被測定液中のイオン種をクロマトグラフィ、
りに分析するイオン種分析方法およびその装置に関する
。[Detailed Description of the Invention] <Industrial Application Field> The present invention is a method of analyzing ionic species in a liquid to be measured using chromatography,
This invention relates to a method for analyzing ion species and an apparatus for the same.
〈従来の技術〉
イオンクロマトグラフを用いて、被測定液中のイオン種
を分離分析する場合、通常、一種類の溶離液を使用して
クロマトグラムを得ることが多い。<Prior Art> When using an ion chromatograph to separate and analyze ion species in a liquid to be measured, a chromatogram is usually obtained using one type of eluent.
このクロマトグラムにおいて、分離が不十分なイオン種
のピークがあると、そのイオンの定量尋が困難になる６
このため、溶離液を交換し、上記被測定液を再度所定量
株数して、分離が不十分な上記イオン種を分離させ、良
好な分離状態を示すクロマトグラムを得るようにしてい
た。In this chromatogram, if there is a peak of an ion species that is insufficiently separated, it becomes difficult to quantify that ion6.
For this reason, the eluent was exchanged and the sample liquid was added again in a predetermined amount to separate the insufficiently separated ion species and obtain a chromatogram showing a good separation state.
然し乍ら、上記従来例においては、被測定液を２回採取
する必要があるため、分析に必要な被測定液が多くなる
という欠点があった。また、溶離液の交換を行なうため
、との溶離液交換に例えば３０分以上もの長時間を必要
とし、究極的に分析に要する時間（分析時間）が長くな
るという欠点かのコンタミネーションが生じ晶いという
欠点もあった。However, in the conventional example described above, it is necessary to sample the liquid to be measured twice, which has the disadvantage that a large amount of the liquid to be measured is required for analysis. In addition, in order to exchange the eluent, it takes a long time, for example, 30 minutes or more, to exchange the eluent, which ultimately increases the time required for analysis (analysis time), which can lead to contamination. There was also a drawback.
〈発明が解決しようとする問題点〉
本発明は、上述のような従来例の欠点に鑑みてなされた
ものであり、その目的は、被測定液を１回計量採取する
だけで被測定液中のイオン種を容易かつ短時間に分析で
きるような方法およびその方法を用いた分析装置を提供
することにある。<Problems to be Solved by the Invention> The present invention has been made in view of the above-mentioned drawbacks of the conventional examples, and its purpose is to measure and sample the liquid to be measured only once. It is an object of the present invention to provide a method that can easily and quickly analyze ion species, and an analyzer using the method.
〈問題点を解決するための手段〉
上記問題点を解決する本発明の特徴は、被測定液中のイ
オン種をクロマトグラフィ、りに分析スるイオン種分析
方法およびその装置において、被測定液を所定量採取し
第１の溶離液を用いてイオンクロマトグラフィックに分
析し、この分析で得られたイオン種のうち分離が不十分
な部分を第２の溶離液を用いて再度イオンクジマドグラ
フィックに分析することにある。<Means for Solving the Problems> A feature of the present invention that solves the above problems is that in an ion species analysis method and apparatus for analyzing ion species in a liquid to be measured using chromatography, A predetermined amount is collected and analyzed using ion chromatography using the first eluent, and the portions of the ion species obtained in this analysis that are insufficiently separated are analyzed again using ion chromatography using the second eluent. It's about analyzing.
〈実施例〉
以下、本発明について図を用いて詳細に説明する。第１
図は本発明実施例の構成説明図であり、この図において
、檜１ｍには例えば４ ｍ ｍｏｌ／ｊＮａ２ＣＯ３／
４ ｍ ｍｏｌ／ＬＮａ）ｉｃＯ３で々る第１溶離液
が貯留され、檜１ｂＫは例えば１０ｍ ｍｏｌ／１Ｎａ
２Ｂ４０７でなる第２溶離液が貯留され、槽１ｃには例
えば０．０３規定のＨ２Ｓｏ４溶液でなる除去液が貯留
されている。<Example> Hereinafter, the present invention will be described in detail using the drawings. 1st
The figure is an explanatory diagram of the configuration of the embodiment of the present invention, and in this figure, 1 m of cypress contains, for example, 4 m mol/jNa2CO3/
The first eluent at 4 m mol/LNa)icO3 is stored, and Hinoki 1bK has a concentration of, for example, 10 m mol/1Na.
A second eluent made of 2B407 is stored, and a removal liquid made of, for example, a 0.03N H2So4 solution is stored in the tank 1c.
また、第１切換弁３．第１試料採取弁４．第２試料採取
弁５．および第２切換弁１２ ａ 、その内部流路がい
ずれも実線接続状態と破線接続状態が交互に切換えられ
るようになっている。更に、第１切換弁３の第１接続口
３１には第２溶離液を送液するポンプ２ｂが接続され、
第３接続口３３には第１溶離液を送液するポンプ２ａが
接続されている。第１切換弁３の第４接続口３４に接続
されているカラム１３には例えば陰イオン交換樹脂が充
填されておシ、後述のカラム８とほぼ同じ流体抵抗値を
示すようになっている。第１試料採取弁４の第３および
第６接続口４３．４６には計量管４７が接続され、第２
試料採取弁５の第３および１ｓ６接続口５３．５６には
計量管５７が接続されている。カラム８はブレカラム８
ａと分離カラム８ｂからなシ、いずれも例えば陰イオン
交換樹脂が充填されている。サブレ、す９は例えば陽イ
オン交換膜でなるチューブ９ａによって内部が内室９ｂ
と外室９ｃに仕切られておシ、該内室９ｂには分離カラ
ム８ｂの溶出液が導びかれ外室９ｃにはポンプ２ｃで送
液される除去液が導ひかれて流れるようになっている。Also, the first switching valve 3. First sampling valve4. Second sampling valve5. and the second switching valve 12a, the internal flow paths thereof are alternately switched between a solid line connection state and a broken line connection state. Further, a pump 2b for feeding the second eluent is connected to the first connection port 31 of the first switching valve 3,
A pump 2a for feeding the first eluent is connected to the third connection port 33. The column 13 connected to the fourth connection port 34 of the first switching valve 3 is filled with, for example, an anion exchange resin, and exhibits approximately the same fluid resistance value as the column 8, which will be described later. A metering pipe 47 is connected to the third and sixth connection ports 43.46 of the first sampling valve 4, and the second
A metering tube 57 is connected to the third and 1s6 connection ports 53,56 of the sampling valve 5. Column 8 is Brecolumn 8
A and separation column 8b are both filled with, for example, an anion exchange resin. For example, the sublet 9 has an inner chamber 9b formed by a tube 9a made of a cation exchange membrane.
The eluate from the separation column 8b is guided into the inner chamber 9b, and the removal solution sent by the pump 2c is guided into the outer chamber 9c. There is.
検出器１０は例えば導電率計でなり、上記内室９ｂから
τ配出する液体の物理量（例えば導電率）を検出し、そ
の検出信号を図示しない記録計等に送出し上記イオン種
に対応したクロマドグ２ム等を描かせるようになってい
る。The detector 10 is, for example, a conductivity meter, which detects the physical quantity (for example, conductivity) of the liquid τ distributed from the inner chamber 9b, and sends the detection signal to a recorder (not shown) or the like, which corresponds to the ion type. It is designed to allow you to draw chroma dogs, etc.
このような構成から々る本発明の実施例において、最初
、切換弁３．１２や試料採取弁４，５が全てオフにされ
、それらの内部流路は全て実線接続状態となりている。In the embodiment of the present invention having such a configuration, the switching valves 3, 12 and the sampling valves 4, 5 are all turned off at first, and all of their internal flow paths are in a solid line connection state.
この状態で、槽ｌａ内の第１溶離液はポンプ２ａにより
て例えば２ｍｔ／ｍｉｎ、の流量で送液されて、第１切
換弁３の第３および第２接続口３３．３！−１１Ｅ１試
料採取弁４の第１および第２接続口４１．４２→第２試
料採取弁５の第１および第２接続口５１．５２→プレ力
ラム８ａ→分離カラム８ｂ→サブレ、す９の内室９ｂ→
検出器ｌＯ→槽１ｅの経路で流れる。槽１ｂ内の第２溶
離液は、ポンプ２ｂによって例えば２ ｍ ｔ／ｎｉ
ｎ、の流量で送液されて、第１切換弁３の第１および第
４接続口３１，３４→カラム１３→槽１ｆの経路で流れ
、槽ｌｃ内の除去液は、ポンプ２ｃによって例えば２
ｎｌ １７ｍ Ｉｎ ａの流量で送液されて、サブレ、
す９の外室９ｃを経て槽１ｄに導びかれる。In this state, the first eluent in the tank la is fed by the pump 2a at a flow rate of, for example, 2 mt/min, and the third and second connection ports 33.3 of the first switching valve 3! -11E1 First and second connection ports 41.42 of the sampling valve 4 → First and second connection ports 51.52 of the second sampling valve 5 → Pre-force ram 8a → Separation column 8b → Sable, step 9 Inner room 9b→
It flows along the path from detector lO to tank 1e. The second eluent in tank 1b is pumped by pump 2b at a rate of, for example, 2 mt/ni.
n, and flows through the path of the first and fourth connection ports 31, 34 of the first switching valve 3→column 13→tank 1f, and the removed liquid in the tank lc is pumped by the pump 2c to, for example, 2
The liquid is pumped at a flow rate of nl 17m Ina, and the sable,
It is led to the tank 1d through the outer chamber 9c of the tank 9.
この状態で、被測定液が第１試料採取弁４の第４接続口
４４から注入され計量管４７を満たしてのち接続口４５
かも排出される０次に、第１試料採取弁４がオンにされ
その内部流路が実線接続状態から破線接続状態に切換え
られる。計量管４７内の被測定液は、溶離液に搬送され
てカラム８に至〕、分離カラム８ｂで被測定液中のイオ
ン種がクロマトグラフィ、りに分離される。このカラム
８ｂからの溶出液は、サブレ、す９の内室９ｂＫ至シ、
チューブ９ａを介して外室９ｃ内の除去液と接し、これ
ら両液に含まれている例えば陽イオンの交換が行なわれ
る。In this state, the liquid to be measured is injected from the fourth connection port 44 of the first sample sampling valve 4, fills the measuring tube 47, and then enters the connection port 45.
After the water is discharged, the first sampling valve 4 is turned on and its internal flow path is switched from the solid line connection state to the dashed line connection state. The liquid to be measured in the measuring tube 47 is carried by the eluent to the column 8], where the ionic species in the liquid to be measured are separated by chromatography in the separation column 8b. The eluate from this column 8b is sent to the inner chamber 9bK of the sublet 9.
It comes into contact with the removal liquid in the outer chamber 9c via the tube 9a, and exchanges of, for example, cations contained in these two liquids.
この内室９ｂから排出される液体は検出器１Ｇに導びか
れて例えば導電率が検出され、この検出信号に応じたク
ロマトグラムを上記記録針等に描くようになる。このク
ロマトグラムにおいて分離不十分なイオン種群の部分だ
けが、第２切換弁１２の切換操作で第２試料採取弁５の
計量管５７に導びかれる。The liquid discharged from the inner chamber 9b is guided to the detector 1G, where its conductivity, for example, is detected, and a chromatogram corresponding to this detection signal is drawn on the recording needle or the like. In this chromatogram, only the portion of the ion species group that is insufficiently separated is guided to the metering tube 57 of the second sampling valve 5 by the switching operation of the second switching valve 12.
次に、第１切換弁３をオンにしその内部流路を実線接続
状態から破線接続状態に切換える。この状態では、上記
第１溶離液に代わり第２溶離液が、第１切換弁３から槽
１ｅに至る流路に流れるようになる。その後、第２試料
採取弁５をオンしその内部流路を切換えて、計量管５７
内の液体を第２溶離液でもってカラム８に搬送する。こ
のため１分離カラム８ｂでは、上述の分離不十分なイオ
ン種群が第２溶離液の作用で良好な分離を行なうように
なる。このようＫして分離されたイオン種は再び溶離液
に搬送され、サブレ、す９の内室９ｂを経て検出器ｌＯ
に至シ、鋏イオン種に対応するクロマトグラムを上記記
録計等に描かせる。Next, the first switching valve 3 is turned on and its internal flow path is switched from the solid line connection state to the broken line connection state. In this state, the second eluent instead of the first eluent flows into the channel from the first switching valve 3 to the tank 1e. After that, the second sampling valve 5 is turned on and its internal flow path is switched, and the measuring tube 57 is turned on.
The liquid inside is transported to column 8 with a second eluent. Therefore, in the first separation column 8b, the above-mentioned group of insufficiently separated ion species is effectively separated by the action of the second eluent. The ion species separated in this way are transported to the eluent again, and pass through the interior chamber 9b of the sublet 9 to the detector 1O.
Finally, draw a chromatogram corresponding to the scissor ion species on the recorder or the like.
第２図は１本発明実施例を用い、例えば５ ｐｐｍ１０
ｐｐｍの酢酸イオン（Ａｃｅｔｉｃ Ｉｏｎ） ＃お
よび１０ｐｐｍの蟻酸イオン（Ｆｏｒｍｉｃ Ｉｏｎ
）を含む試料（以下「標準液」という）を分析した結果
を示すクロマトグラムである。このクロマトグラムによ
れば、第１溶離液を用いるイオン種分析（第２図の左側
部分）では分離不十分なイオン種群（Ｆ″″、 ＩＰｏ
ｒｍｉｃ Ｉｏｎ、およびＡｃｅｔｉｃ Ｉｏｎ ）が
現われるが、このイオン種群を第２試料採取弁５（詳し
くは計量管５７内）Ｋ保持してのち第２溶離液を用いて
分析すると良好な分離（第２図の中央部分）を示すよう
になることが分る。尚、第１切換弁３を切換えて数分後
にクロマドグ２ムのベースラインが変動しているのは、
第１切換弁３で切換えられた溶離液が検出器ｌＯに至る
まで数分間もの時間がかかシ、且つ、これら溶離液の物
理量（例えば導電率）が異なるととに起因するものであ
る。FIG. 2 uses one embodiment of the present invention, for example, 5 ppm 10
ppm Acetic Ion # and 10 ppm Formic Ion #
) (hereinafter referred to as "standard solution") is a chromatogram showing the results of analyzing a sample containing (hereinafter referred to as "standard solution"). According to this chromatogram, ion species analysis using the first eluent (left part of Figure 2) results in a group of ion species (F'''', IPo
rmic ion, and acetic ion), but if this ion species group is held in the second sampling valve 5 (more specifically, in the measuring tube 57) and then analyzed using the second eluent, a good separation can be achieved (see Fig. 2). It can be seen that the central part of The baseline of the chroma dog 2 is fluctuating several minutes after switching the first switching valve 3 because
This is due to the fact that it takes several minutes for the eluent switched by the first switching valve 3 to reach the detector IO, and the physical quantities (eg, electrical conductivity) of these eluents are different.
〈効果〉
以上詳しく説明したような本発明によれば、分離不十分
なイオン種群に相肩する部分だけを検出器の後方で分取
して再分析するような構成であるため、被測定液の採取
が１回で済むという利点がある。また、第１切換弁３の
切換えによって第１溶離液と第２溶離液を交互に切換え
るような構成であるため、前記従来例に比し、溶離液交
換が容易且つ短時間で済み、しかも溶離液のコンタミ・
ネーシ、ンも生じないという利点がある。<Effects> According to the present invention as described in detail above, only the portion corresponding to the insufficiently separated ion species group is fractionated behind the detector and reanalyzed. It has the advantage that it only needs to be collected once. Furthermore, since the structure is such that the first eluent and the second eluent are alternately switched by switching the first switching valve 3, the eluent can be replaced more easily and in a shorter time than in the conventional example. Liquid contamination/
It has the advantage that no leakage occurs.
第１図は本発明実施例の構成説明図であシ、第２図は本
発明実施例を用いて作成したクロマトグラムである。
１ａ＝１ｆ・・・槽、２ａ〜２ｃ・・・送液ポンプ、３
，１２・・・切換弁、４，５・・・試料採取弁、８．１
３・・・カラム、９・・・サプレッサ、１０・・・検出
器。FIG. 1 is an explanatory diagram of the configuration of an embodiment of the present invention, and FIG. 2 is a chromatogram prepared using the embodiment of the present invention. 1a=1f...tank, 2a-2c...liquid pump, 3
, 12... switching valve, 4, 5... sample collection valve, 8.1
3... Column, 9... Suppressor, 10... Detector.
Claims (4)
オンクロマトグラフィックに分析し、この分析で得られ
るイオン種のうち分離が不十分な部分を第２の溶離液を
用いて再度イオンクロマトグラフィックに分析すること
を特徴とするイオン種分析方法。(1) Collect a predetermined amount of the liquid to be measured and analyze it by ion chromatography using the first eluent, and remove the insufficiently separated portions of the ionic species obtained in this analysis using the second eluent. An ion species analysis method characterized by performing ion chromatographic analysis again.
Ｏ＿３と４ｍ ｍｏｌ／ｌのＮａＨＣＯ＿３の混合液で
なり、前記第２溶離液は１０ｍ ｍｏｌ／ｌのＮａ＿２
Ｂ＿４Ｏ＿７溶液でなる特許請求範囲第（１）項記載の
イオン種分析方法。(2) The first eluent is 4 mmol/l Na_2C
The second eluent is a mixture of O_3 and 4 mmol/l NaHCO_3, and the second eluent is a mixture of 10 mmol/l NaHCO_3.
The ion species analysis method according to claim (1), which comprises a B_4O_7 solution.
の採取弁で採取された被測定液中のイオン種を分離する
カラムと、このカラムから溶出するイオン種を検出する
検出器と、この検出器から排出される液体の一部を計量
して採取する第２試料採取弁と、この採取弁と前記検出
器を断続的に接続せしめる第１流路切換弁と、前記第１
および第２の試料採取弁を介して前記カラムに第１溶離
液と第２溶離液とを交互に切換えて送液せしめる第２流
路切換弁とを具備してなるイオン種分析装置。(3) A first sample sampling valve that collects a predetermined amount of the liquid to be measured, a column that separates the ionic species in the liquid that is sampled by this sampling valve, and a detector that detects the ionic species eluted from this column. a second sample sampling valve that measures and samples a portion of the liquid discharged from the detector; a first flow path switching valve that connects the sampling valve and the detector intermittently;
and a second flow path switching valve that alternately switches and sends a first eluent and a second eluent to the column via a second sample collection valve.
列接続されてなる特許請求範囲第（３）項記載のイオン
種分析装置。(4) The ion species analyzer according to claim (3), wherein the column includes a precolumn and a separation column connected in series.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6463285A JPS61223555A (en) | 1985-03-28 | 1985-03-28 | Analysis of ion species and apparatus using the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6463285A JPS61223555A (en) | 1985-03-28 | 1985-03-28 | Analysis of ion species and apparatus using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61223555A true JPS61223555A (en) | 1986-10-04 |
| JPH0465980B2 JPH0465980B2 (en) | 1992-10-21 |
Family
ID=13263833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6463285A Granted JPS61223555A (en) | 1985-03-28 | 1985-03-28 | Analysis of ion species and apparatus using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61223555A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06510607A (en) * | 1992-07-27 | 1994-11-24 | ダイオネックス コーポレイション | Electrochemical pretreatment device for liquid sample analysis |
| CN106404980A (en) * | 2016-08-26 | 2017-02-15 | 广州京诚检测技术有限公司 | Detection method for nitric acid fog in atmosphere |
| CN106885865A (en) * | 2017-04-06 | 2017-06-23 | 天津师范大学 | Nitrate anion, the method for nitrite anions content and application in a kind of detection broccoli |
| CN107703250A (en) * | 2017-10-24 | 2018-02-16 | 上海上药第生化药业有限公司 | The assay method of Pericarpium Trichosanthis injection ions content |
| CN109828077A (en) * | 2018-12-27 | 2019-05-31 | 河海大学 | The method that ion chromatography detects Ordinary ion in the pore water of ocean |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51104893A (en) * | 1975-03-12 | 1976-09-17 | Hitachi Ltd | SAIJUNKANKUROMATOGURAFUIIHOHOOYOBISOCHI |
-
1985
- 1985-03-28 JP JP6463285A patent/JPS61223555A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51104893A (en) * | 1975-03-12 | 1976-09-17 | Hitachi Ltd | SAIJUNKANKUROMATOGURAFUIIHOHOOYOBISOCHI |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06510607A (en) * | 1992-07-27 | 1994-11-24 | ダイオネックス コーポレイション | Electrochemical pretreatment device for liquid sample analysis |
| CN106404980A (en) * | 2016-08-26 | 2017-02-15 | 广州京诚检测技术有限公司 | Detection method for nitric acid fog in atmosphere |
| CN106885865A (en) * | 2017-04-06 | 2017-06-23 | 天津师范大学 | Nitrate anion, the method for nitrite anions content and application in a kind of detection broccoli |
| CN107703250A (en) * | 2017-10-24 | 2018-02-16 | 上海上药第生化药业有限公司 | The assay method of Pericarpium Trichosanthis injection ions content |
| CN109828077A (en) * | 2018-12-27 | 2019-05-31 | 河海大学 | The method that ion chromatography detects Ordinary ion in the pore water of ocean |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0465980B2 (en) | 1992-10-21 |
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