JPS6311859A - Liquid chromatography analytical method and apparatus - Google Patents
Liquid chromatography analytical method and apparatusInfo
- Publication number
- JPS6311859A JPS6311859A JP15401086A JP15401086A JPS6311859A JP S6311859 A JPS6311859 A JP S6311859A JP 15401086 A JP15401086 A JP 15401086A JP 15401086 A JP15401086 A JP 15401086A JP S6311859 A JPS6311859 A JP S6311859A
- Authority
- JP
- Japan
- Prior art keywords
- eluate
- dichloroethane
- layer
- liquid chromatography
- section
- 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
Links
- 238000004811 liquid chromatography Methods 0.000 title claims abstract description 14
- 238000004458 analytical method Methods 0.000 title claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract 2
- 239000013626 chemical specie Substances 0.000 claims description 7
- 238000002835 absorbance Methods 0.000 claims description 4
- 238000011481 absorbance measurement Methods 0.000 claims description 2
- 239000003480 eluent Substances 0.000 abstract description 13
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 abstract description 10
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 5
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 5
- 238000002347 injection Methods 0.000 abstract description 4
- 239000007924 injection Substances 0.000 abstract description 4
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- 238000000034 method Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 description 5
- 239000003957 anion exchange resin Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010828 elution Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、液体クロマトグラフィー分析方法および装置
に関する。更に詳しくは、高癲択的、高感度分析に好適
な液体クロマトグラフィー分析方法および装置に関する
。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a liquid chromatography analysis method and apparatus. More specifically, the present invention relates to a liquid chromatography analysis method and apparatus suitable for highly selective and sensitive analysis.
イオン交換樹脂を用いてイオン種の分離を行い、導電率
計で検出する従来の液体クロマトグラフィ二は、溶離液
中の電解質によるパックグラウンド導電率を徒＜子るた
めに、低交換容量のイオン交換樹脂カラムを用いて低濃
度の溶離液で分離する必要がある。この場合、試料中の
高濃度イオン種のクロマトグラムはブロードになり、近
接して溶出する微景イオン種の分析を妨害することが有
った。また、検出感度を上げるためには当量型導度の低
い溶離液を用い宛り、Ｃ′０２−塩基溶離液で分離後の
溶出液をサプレッサに通して導電率の低いＨ２ＣＯ，＊
変換するなど、溶離液の種類が限定されるという問題点
があった。なおこの種の装置として関連するものには例
えば、アナリテ斗カル・ケミストリー（”Ａｎａｌｙｔ
ｉｃａｌ Ｃｈｅｍｉｓｔｒｙ）、４７巻、１８０１頁
〜１８０９頁（１９７５）において論じられているイオ
ンクロマトグラフィー、およびジャーナル・オプ・クロ
マトグラフィー（Ｊｏｕｒｎａｌ ｏｆＣｈｒｏｍａｔ
ｏｇｒａｐｈｙ）、 １８６巻、５０９頁（１９７９）
において論じられている液体クロマトグラフィー等が挙
げられる。Conventional liquid chromatography, which separates ionic species using an ion exchange resin and detects them with a conductivity meter, uses ion exchange with a low exchange capacity to reduce the background conductivity caused by the electrolyte in the eluent. It is necessary to separate using a resin column with a low concentration eluent. In this case, the chromatogram of high-concentration ion species in the sample becomes broad, which may interfere with analysis of minute ion species eluting in close proximity. In addition, in order to increase the detection sensitivity, an eluent with a low conductivity of equivalent type is used, and the eluate separated with a C'02-base eluent is passed through a suppressor to collect H2CO,* which has a low conductivity.
There was a problem in that the types of eluents were limited, such as conversion. Related devices of this type include, for example, "Analyt Cal Chemistry".
47, pp. 1801-1809 (1975), and the Journal of Chromatography.
(1979), Volume 186, Page 509 (1979)
Examples include liquid chromatography, which is discussed in .
上記従来技術は溶離後の化学種を一率に導電率や吸光光
度法で検出するもので、選択性の点について配慮がされ
ておらず、近接する位置に溶出する化学種が多量に含ま
れている場合などに妨害を受は易いという問題があった
。The above conventional technology detects chemical species after elution using conductivity or spectrophotometry, but does not take into account selectivity, and a large amount of chemical species elute in nearby positions. There was a problem in that it was easily susceptible to interference when
本発明の目的は、上記のような問題点を解決し、成分検
出における選択性が高く感度の高い液体クロマトグラフ
ィー分析方法および装置を提供することにある。An object of the present invention is to solve the above-mentioned problems and provide a liquid chromatography analysis method and apparatus that have high selectivity and sensitivity in component detection.
上記目的は、液体クロマトグラフィーにおいて分離カラ
ムで分離後の試料溶出液に反応試薬及び抽出溶媒を添加
し、目的化学種との反応生成物を溶媒に抽出して抽出液
の吸光度を測定することにより達成される。その際の液
体クロマトグラフィー装置は１分離カラムの後方の溶出
液流路上に。The above purpose is achieved by adding a reaction reagent and an extraction solvent to the sample eluate after separation in a separation column in liquid chromatography, extracting the reaction product with the target chemical species into the solvent, and measuring the absorbance of the extract. achieved. At that time, the liquid chromatography device was placed on the eluate flow path behind the 1-separation column.
反応試薬添加部、抽出溶媒添加部、抽出部、分離部、フ
ローセル部および吸光光度測定部を備えたものである。It is equipped with a reaction reagent addition section, an extraction solvent addition section, an extraction section, a separation section, a flow cell section, and an absorbance measurement section.
更に詳しくは分離カラムで分離後の溶出液だ目的化生釉
と反応して溶媒層に抽出され易い物質を生成する反応試
薬と抽出溶媒を定速で添加し、抽出溶媒層の吸光度を連
続測定するのが好ましい。これによシ反応試薬と反応す
る化学種のみの測定が可能となるため、溶出位置が近似
する共存成分の妨害を受けることが無い。More specifically, it is the eluate after separation in the separation column.A reaction reagent and extraction solvent that react with the raw glaze to produce a substance that is easily extracted into the solvent layer are added at a constant rate, and the absorbance of the extraction solvent layer is continuously measured. It is preferable to do so. This makes it possible to measure only the chemical species that react with the reaction reagent, so there is no interference from coexisting components whose elution positions are close to each other.
本発明によれば、測定対象化学種に応じて分離カラム充
填剤、溶離液の種類及び反応試薬と抽出溶媒を変えるこ
とにより、種々の化学種を選択的に、高感度に分析でき
る。According to the present invention, various chemical species can be analyzed selectively and with high sensitivity by changing the separation column packing material, the type of eluent, the reaction reagent, and the extraction solvent depending on the chemical species to be measured.
また、導電率検出器を用いる場合と異り、溶離液として
当量電導度の低い溶離液を用いたり、サプレッサを用い
て溶離液の電導度を下げる必要が無く、装置の簡素化や
溶離液の選択範囲の拡大が可能となる。また高濃度の溶
離液を用いることが可能で、交換容量の大きい分離カラ
ムを用いることＫよシ、従来の低交換容量のカラムを用
いたイオンクロマトグラフでは不可能であった高濃度共
存成分中の微量成分の分析なども可能となる。In addition, unlike when using a conductivity detector, there is no need to use an eluent with low equivalent conductivity or use a suppressor to lower the conductivity of the eluent, simplifying the equipment and reducing the The selection range can be expanded. In addition, it is possible to use a highly concentrated eluent, and it is possible to use a separation column with a large exchange capacity. It also becomes possible to analyze trace components of
以下、本発明の一実施例を第１図により説明する。１は
溶離液槽、２は定量ポンプ、３はインジェクションパル
プ、４は陰イオン交換樹脂カラムで、これらで構成され
る液体クロマトグラフィーにＢＦ４−を含む試料液をイ
ンジェクションパルプ３より一定量注入する。溶離液の
流速２ｍｔ／ｍで分離後の溶出液に反応液槽５よシα０
５Ｗ／Ｗ％メチレ／ブルー溶液を定量ポンプ６を用いて
毎分α５−の流速で送入し、溶媒槽７より１．２−ジク
ロロエタンを定量ポンプ８を用いて毎分α５−の流速で
送入する。混合器９を経て抽出コイル１０を通過中にＢ
Ｆ４− のメチレンブルー錯体が１．２−ジクロロエタ
ン層に抽出され、セパレータ１１で水層と１．２−ジク
ロロエタン層が分離される。水層は排出口１２より排出
され、１．２−ジクロロエタン層が７０−セル１３に送
られ吸光光度計１４を用いて６６０ｎｍにおける吸光度
が連続測定され、レコーダ１５を用いてクロマトグラム
が描かれる。フローセル１５を通過後の１．２−ジクロ
ロエタン層は排出口１６よシ排出される。An embodiment of the present invention will be described below with reference to FIG. 1 is an eluent tank, 2 is a metering pump, 3 is an injection pulp, and 4 is an anion exchange resin column. A fixed amount of a sample solution containing BF4- is injected from the injection pulp 3 into a liquid chromatography system composed of these. The flow rate of the eluent is 2 mt/m, and the eluate after separation is passed from the reaction liquid tank 5 to α0.
A 5W/W% methylene/blue solution was delivered at a flow rate of α5- per minute using the metering pump 6, and 1,2-dichloroethane was delivered from the solvent tank 7 at a flow rate of α5- per minute using the metering pump 8. Enter. B while passing through the mixer 9 and the extraction coil 10
The methylene blue complex of F4- is extracted into the 1,2-dichloroethane layer, and the separator 11 separates the aqueous layer and the 1,2-dichloroethane layer. The aqueous layer is discharged from the discharge port 12, and the 1,2-dichloroethane layer is sent to the 70-cell 13, where the absorbance at 660 nm is continuously measured using the spectrophotometer 14, and a chromatogram is drawn using the recorder 15. The 1,2-dichloroethane layer after passing through the flow cell 15 is discharged through the discharge port 16.
本実施例によれば、メチレンブルーと錯体を作って溶媒
に抽出されるＮＯ３−や界面活性剤は陰イオン交換樹脂
カラムで分離され、またＢＦ４− と近接して溶出され
る８０４′−等はメチレンブルー錯体を作らないことか
ら、ＢＦ４− のみを高感度に測定することができる。According to this example, NO3- and surfactants that form complexes with methylene blue and are extracted into the solvent are separated using an anion exchange resin column, and 804'-, etc., which are eluted in close proximity to BF4-, are separated by methylene blue. Since no complex is formed, only BF4- can be measured with high sensitivity.
なお、本発明は上述した実施例に限定されるものではな
く、測定対象成分に応じて反応試薬、抽出溶媒を変える
ことにより、種々の成分を選択的に、高感度に分析する
ことができる。Note that the present invention is not limited to the above-described embodiments, and various components can be selectively analyzed with high sensitivity by changing the reaction reagent and extraction solvent depending on the component to be measured.
上述の如く、本発明の液体クロマトグラフィー分析方法
および装置によれば、成分検出における選択性が高く感
度の高い分析ができるという作用効果がある。As described above, the liquid chromatography analysis method and apparatus of the present invention have the effect of allowing highly selective and highly sensitive analysis in component detection.
第１図は本発明の一実施例を示すフロー図である。 １・・・溶離液槽 ２．６．８・・・定量ポンプ ３・・・インジェクションパルプ ４・・・陰イオン交換樹脂カラム ５・・・反応液槽 ７・・・抽出溶媒層 ９・・・混合器 １０・・・抽出コイル １１・・・セパレータ １２．１６・・・排出口 １３・・・フローセル １４・・・吸光光度計 １５・・・記録計。 FIG. 1 is a flow diagram showing one embodiment of the present invention. 1... Eluent tank 2.6.8...metering pump 3... Injection pulp 4...Anion exchange resin column 5...Reaction liquid tank 7...Extraction solvent layer 9...Mixer 10...Extraction coil 11...Separator 12.16...Discharge port 13...Flow cell 14... Absorption photometer 15...Recorder.
Claims (1)
離後の試料溶出液に反応試薬及び抽出溶媒を添加し、目
的化学種との反応生成物を溶媒に抽出して抽出液の吸光
度を測定する液体クロマトグラフィー分析方法。 ２、液体クロマトグラフィーにおいて、分離カラムの後
方の溶出液流路上に、反応試薬添加部、抽出溶媒添加部
、抽出部、分離部、フローセル部および吸光光度測定部
を備えたことを特徴とする液体クロマトグラフィー装置
。[Claims] 1. In liquid chromatography, a reaction reagent and an extraction solvent are added to the sample eluate after separation in a separation column, and the reaction product with the target chemical species is extracted into the solvent to determine the absorbance of the extract. A liquid chromatography analysis method for measuring. 2. In liquid chromatography, a liquid characterized by comprising a reaction reagent addition section, an extraction solvent addition section, an extraction section, a separation section, a flow cell section, and an absorbance measurement section on the eluate flow path after the separation column. Chromatography equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15401086A JPS6311859A (en) | 1986-07-02 | 1986-07-02 | Liquid chromatography analytical method and apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15401086A JPS6311859A (en) | 1986-07-02 | 1986-07-02 | Liquid chromatography analytical method and apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6311859A true JPS6311859A (en) | 1988-01-19 |
Family
ID=15574934
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15401086A Pending JPS6311859A (en) | 1986-07-02 | 1986-07-02 | Liquid chromatography analytical method and apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6311859A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111610247A (en) * | 2020-05-27 | 2020-09-01 | 中国科学院地质与地球物理研究所 | Method for quickly separating high-purity W from geological sample |
-
1986
- 1986-07-02 JP JP15401086A patent/JPS6311859A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111610247A (en) * | 2020-05-27 | 2020-09-01 | 中国科学院地质与地球物理研究所 | Method for quickly separating high-purity W from geological sample |
| CN111610247B (en) * | 2020-05-27 | 2021-03-16 | 中国科学院地质与地球物理研究所 | Method for quickly separating high-purity W from geological sample |
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