JPH0743361B2 - Capillary column - Google Patents
Capillary columnInfo
- Publication number
- JPH0743361B2 JPH0743361B2 JP63286326A JP28632688A JPH0743361B2 JP H0743361 B2 JPH0743361 B2 JP H0743361B2 JP 63286326 A JP63286326 A JP 63286326A JP 28632688 A JP28632688 A JP 28632688A JP H0743361 B2 JPH0743361 B2 JP H0743361B2
- Authority
- JP
- Japan
- Prior art keywords
- capillary column
- column
- capillary
- present
- inner diameter
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6004—Construction of the column end pieces
- G01N2030/6008—Construction of the column end pieces capillary restrictors
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Description
【発明の詳細な説明】 （イ）産業上の利用分野 この発明は、ガスクロマトグラフ用キャピラリカラムに
関する。TECHNICAL FIELD The present invention relates to a capillary column for a gas chromatograph.
（ロ）従来の技術 従来、キャピラリカラムガスクロマトグラフに用いられ
るキャピラリカラムは、その全長にわたって均一な内径
を有し、そのまま検出器に接続されて用いられている。(B) Conventional Technology Conventionally, a capillary column used in a capillary column gas chromatograph has a uniform inner diameter over its entire length and is used as it is while being connected to a detector.
（ハ）発明が解決しようとする課題 しかしながら、上記キャピラリカラムでは、そのカラム
出口に接続される検出器は大気圧下にあるため、こうし
た系で試料を分析すると、該カラムで分離される成分
は、出口に近付く程キャリアガス圧が低下するため拡散
しやすくなり、その結果ピークがブローになる。(C) Problem to be Solved by the Invention However, in the above-mentioned capillary column, the detector connected to the column outlet is under atmospheric pressure. Therefore, when a sample is analyzed by such a system, the components separated in the column are The closer to the outlet, the lower the carrier gas pressure and the more likely it is to diffuse, resulting in a peak blow.
この発明にかかる状況に鑑みなされたものであり、分離
成分の拡散を防止しうるガスクロマトグラフ用キャピラ
リカラムを提供しようとするものである。The present invention has been made in view of the circumstances of the present invention, and an object of the present invention is to provide a capillary column for a gas chromatograph capable of preventing the diffusion of separated components.
（ニ）課題を解決するための手段 かくしてこの発明によれば、ガスクロマトグラフ用キャ
ピラリカラムであって、該カラムの検出器接続側出口端
部またはその近傍に、流路断面を縮小して流束を絞りう
る内径変更部を有するキャピラリカラムが提供される。(D) Means for Solving the Problems Thus, according to the present invention, there is provided a capillary column for a gas chromatograph, in which the flow passage cross-section is reduced at the detector connection side outlet end of the column or in the vicinity thereof. There is provided a capillary column having an inner diameter changing portion capable of squeezing.
この発明は、ガスクロマトグラフ用キャピラリカラムに
おいて、そのカラム流路の下流で流路抵抗を増大し、上
流部で分離された各分離成分の拡散を防止しつつ検出器
に移送しうるよう構成したことを特徴とする。According to the present invention, a capillary column for a gas chromatograph is configured so that the flow passage resistance is increased downstream of the column flow passage and each separated component separated in the upstream portion can be transferred to a detector while preventing diffusion. Is characterized by.
この発明において、キャピラリカラムの検出器接続側出
口端部またはその近傍に、内径変更部が設けられる。上
記近傍とは該カラム出口端部からカラム側であってもよ
く、検出器接続側であってもよい。上記内径変更部は、
流路断面を縮小して流束を絞りうる構造に形成される。
上記縮小は分離成分の拡散を防止しうるに足る程度に設
定される。従ってキャピラリカラムの本体部の流路抵抗
の２倍以上となるよう設定されることが好ましい。（例
えば分離用キャピラリカラムの出口直前圧が、1kg/cm2
（ゲージ圧）以上が好ましい。）上記流束の絞りうる構
造としては、キャピラリカラム出口端部周囲のカラム壁
の肉厚を大きくして流路を絞る構成、出口端部またはそ
の近傍のカラム壁を引き伸ばして流路を絞る構成、キャ
ピラリカラム出口端部に断面の小さいチューブを接続す
る構成等を挙げることができる。In the present invention, the inner diameter changing portion is provided at or near the outlet end of the capillary column on the detector connection side. The vicinity may be the column side from the column outlet end or the detector connection side. The inner diameter changing part is
It is formed in a structure that can reduce the flow flux by reducing the cross section of the flow channel.
The reduction is set to such an extent that diffusion of separated components can be prevented. Therefore, it is preferable that the flow path resistance of the main body of the capillary column is set to twice or more. (For example, the pressure immediately before the exit of the separation capillary column is 1 kg / cm 2
(Gauge pressure) or higher is preferable. ) As a structure capable of restricting the above-mentioned flux, a structure in which the wall thickness around the outlet end of the capillary column is increased to restrict the flow passage, and a structure in which the outlet end or the column wall in the vicinity thereof is expanded to restrict the flow passage A configuration in which a tube having a small cross section is connected to the outlet end of the capillary column can be used.
この発明において、上記内径変更部に加圧用流路を設け
ることにより、流路抵抗の増大度を調節できるように構
成することが好ましい。このため好ましい構成例として
は、例えばキャピラリカラム出口端部に三方ジョイント
を用いて、第２のキャリアガス流入路を設け、このキャ
リアガス流入路に調圧器を設ける等が挙げられる。In the present invention, it is preferable that the inner diameter changing portion is provided with a pressurizing channel so that the degree of increase in the channel resistance can be adjusted. Therefore, as a preferable configuration example, for example, a three-way joint is used at the exit end of the capillary column to provide a second carrier gas inflow path, and a pressure regulator is provided in this carrier gas inflow path.
この発明のキャピラリカラムにおいて、その下流部で流
路抵抗を増大させる構成とする以外は、当該分野で公知
の構成とすることができる。The capillary column of the present invention may have a configuration known in the art, except that the flow path resistance is increased at the downstream portion thereof.
（ホ）作用 この発明によれば、キャピラリカラムは検出器に接続さ
れる出口端部またはその近傍が、流束が絞られる内径変
更部を有しており、キャピラリカラム出口部付近でのキ
ャリアガス圧の減衰が防止され、その結果上流部で分離
された分離成分は、その分離状態を保持したまま検出器
に導入されることとなる。(E) Action According to the present invention, the capillary column has the inner diameter changing portion for narrowing the flux at or near the outlet end connected to the detector, and the carrier gas near the outlet of the capillary column is The pressure decay is prevented, and as a result, the separated components separated in the upstream portion are introduced into the detector while maintaining the separated state.
以下実施例によりこの発明を詳細に説明するが、これに
よりこの発明は限定されるものではない。Hereinafter, the present invention will be described in detail with reference to Examples, but the present invention is not limited thereto.
（ヘ）実施例 実施例１ 第１図はこの発明のキャピラリカラムの一実施例の部分
構成説明図である。同図にはキャピラリカラムの検出器
接続側の端部構造が示されている。すなわちこのキャピ
ラリカラムは、化学結合型メチルシリコン（長さ25m,内
径0.32mm、膜厚５μｍ）でできた通常のガスクロマトグ
ラフ用キャピラリカラム（１）を、カラム内に不活性ガ
スを微量流しながら、出口端部を溶融して封じた後、ヤ
スリで切削して内径（d1:10μｍ）の細孔（イ）を形成
したものである。このカラム本体ロ部の流路断面と細孔
（イ）での流路断面との比は1/1024であった。(F) Embodiments Embodiment 1 FIG. 1 is a partial configuration explanatory view of an embodiment of a capillary column of the present invention. The drawing shows the structure of the end of the capillary column on the detector connection side. That is, this capillary column is a normal gas chromatograph capillary column (1) made of chemically bonded methyl silicon (length 25 m, inner diameter 0.32 mm, film thickness 5 μm), while flowing a small amount of inert gas into the column. The outlet end is melted and sealed, and then cut with a file to form pores (a) having an inner diameter (d 1 : 10 μm). The ratio of the flow passage cross section of the column main body to the flow passage cross section in the pore (a) was 1/1024.
実施例２ 第２図に、この発明のキャピラリカラムの他の実施例の
部分構成説明図を示す。同図のキャピラリカラムは、実
施例１で用いたものと同様のキャピラリカラム（１）
を、カラム内に不活性ガスを流しながら出口端部を溶融
し引き伸ばして細管に形成した後、切断したものであ
る。得られたキャピラリカラム出口端部の細管部（ハ）
先端の内径（d2）は８μｍであった。このとき該カラム
本体ロ部の流路断面とハの先端細孔での流路断面との比
は1/1600であった。Embodiment 2 FIG. 2 is a partial structural explanatory view of another embodiment of the capillary column of the present invention. The capillary column shown in the figure is the same as the one used in Example 1 (1).
While the inert gas was allowed to flow into the column, the outlet end was melted and stretched to form a thin tube, which was then cut. Capillary column outlet end of the resulting capillary (c)
The inner diameter (d 2 ) of the tip was 8 μm. At this time, the ratio of the flow passage cross section of the column main body to the flow passage cross section at the tip end pores of C was 1/1600.
実施例３ 第３図に、この発明のキャピラリカラムの他の実施例部
分構成説明図を示す。同図のキャピラリカラムは、実施
例１で用いたものと同様のキャピラリカラム（１）の出
口端部に、ユニオン（２）を介して内径（d3:50μ
ｍ）、長さ0.25mのキャピラリチューブ（３）を接続し
たものである。キャピラリチューブ（３）はその内面が
不活性処理された石英製チューブであり、ユニオン
（２）はその内部にキャピラリカラム（１）出口端とキ
ャピラリチューブ（３）端を接続保持するベスペルフェ
ルール（４）等を有して構成されている。このとき該カ
ラム本体ロ部の流路断面とキャピラリチューブ（３）の
流路断面との比は1/41であった。Embodiment 3 FIG. 3 is a partial structural explanatory view of another embodiment of the capillary column of the present invention. Capillary column of the figure, the outlet end of the same capillary column as used in Example 1 (1), an inner diameter through the union (2) (d 3: 50.mu.
m), a capillary tube (3) having a length of 0.25 m is connected. The capillary tube (3) is a quartz tube whose inner surface is inactivated, and the union (2) has a Vespel ferrule (4) connecting and holding the outlet end of the capillary column (1) and the end of the capillary tube (3) inside. ) And the like. At this time, the ratio of the flow passage cross section of the column main body to the flow passage cross section of the capillary tube (3) was 1/41.
上記実施例３で得られたキャピラリカラムについて、そ
の分離能を現す指標の１つとして理論段高さ（HETP）： HETP＝L/N （L:カラム長,N:総理論段数） を検討した。すなわち、実施例３のキャピラリカラムを
ガスクロマトグラフに用いて下記条件で分析し、HETP
（mm）と線速度（cm/sec）との関係を調べたところ、第
４図に示すHETP曲線（ａ）が得られた。このとき比較例
として通常のキャピラリカラム（１）を上記と同様の条
件で用いて得られたHETP曲線（ｂ）を併せて示す。Regarding the capillary column obtained in Example 3 above, theoretical plate height (HETP): HETP = L / N (L: column length, N: total number of theoretical plates) was examined as one of the indexes showing the resolution. . That is, the capillary column of Example 3 was used in a gas chromatograph and analyzed under the following conditions to obtain HETP
When the relationship between (mm) and linear velocity (cm / sec) was investigated, the HETP curve (a) shown in FIG. 4 was obtained. At this time, as a comparative example, the HETP curve (b) obtained by using the ordinary capillary column (1) under the same conditions as above is also shown.
カラム温度:180℃ キャリアガス：ヘリウム スプリット比:30:1 試料:n−C12化合物（ｎ−ペンタン中） 上記第４図の結果から、前者のHETP値は、後者のそれに
比べて低くなり、分離能が向上していることがわかる。Column temperature: 180 ° C. Carrier gas: Helium Split ratio: 30: 1 Sample: nC 12 compound (in n-pentane) From the results of FIG. 4 above, the HETP value of the former becomes lower than that of the latter, It can be seen that the resolution is improved.
実施例４ 第５図に、この発明のキャピラリカラムの他の実施例の
部分構成説明図を示す。同図のキャピラリカラムは、実
施例１で用いたものと同様のキャピラリカラム（１）
と、実施例３で用いたキャピラリチューブ（３）とを、
三方ジョイント（５）で接続し、この三方ジョイント
（５）に図示しないキャリアガス供給部からのキャリア
ガス供給路（ｃ）を、調圧器（６）および圧力計（７）
を介して接続したものである。このものは、キャリアガ
ス供給路（ｃ）のキャリアガス圧を調整することによ
り、任意の比率でキャピラリカラムの流路抵抗を増大で
きるものである。Embodiment 4 FIG. 5 is a partial structural explanatory view of another embodiment of the capillary column of the present invention. The capillary column shown in the figure is the same as the one used in Example 1 (1).
And the capillary tube (3) used in Example 3,
A three-way joint (5) is used for connection, and a carrier gas supply path (c) from a carrier gas supply unit (not shown) is connected to the three-way joint (5) and a pressure regulator (6) and a pressure gauge (7).
It is connected through. This is capable of increasing the flow passage resistance of the capillary column at an arbitrary ratio by adjusting the carrier gas pressure in the carrier gas supply passage (c).
（ト）発明の効果 この発明によれば、キャピラリカラム内で分離された数
分の出口近傍での拡散を押さえることができ、分離能を
向上することができる。(G) Effect of the Invention According to the present invention, it is possible to suppress the diffusion in the vicinity of the outlet for several minutes separated in the capillary column, and it is possible to improve the resolution.
第１図はこの発明のキャピラリカラムの一実施例の部分
構成説明図、第２図および第３図はそれぞれこの発明の
キャピラリカラムの他の例の部分構成説明図、第４図は
この発明のキャピラリカラムの一例の分離能の向上を比
較例と共に示すHETP曲線図、第５図はこの発明のキャピ
ラリカラムの他の実施例の部分構成説明図である。 （１）……キャピラリカラム、 （２）……ユニオン、 （３）……キャピラリチューブ、 （５）……三方ジョイント、 （６）……調圧器、（７）……圧力計。FIG. 1 is a partial structural explanatory view of an embodiment of the capillary column of the present invention, FIGS. 2 and 3 are partial structural explanatory views of other examples of the capillary column of the present invention, and FIG. FIG. 5 is a HETP curve diagram showing the improvement of the resolution of an example of a capillary column together with a comparative example, and FIG. 5 is a partial configuration explanatory diagram of another example of the capillary column of the present invention. (1) ... capillary column, (2) ... union, (3) ... capillary tube, (5) ... three-way joint, (6) ... pressure regulator, (7) ... pressure gauge.
Claims (2)
あって、該カラムの検出器接続側出口端部またはその近
傍に、流路断面を縮小して流束を絞りうる内径変更部を
有するキャピラリカラム。1. A capillary column for a gas chromatograph, the capillary column having an inner diameter changing portion capable of reducing a flow flux by narrowing a cross section of a flow passage, at or near an outlet end of a detector connecting side of the column.
続されてなる請求項１のキャピラリカラム。2. The capillary column according to claim 1, wherein a pressurizing carrier gas channel is connected to the inner diameter changing portion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63286326A JPH0743361B2 (en) | 1988-11-11 | 1988-11-11 | Capillary column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63286326A JPH0743361B2 (en) | 1988-11-11 | 1988-11-11 | Capillary column |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02132371A JPH02132371A (en) | 1990-05-21 |
| JPH0743361B2 true JPH0743361B2 (en) | 1995-05-15 |
Family
ID=17702938
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63286326A Expired - Lifetime JPH0743361B2 (en) | 1988-11-11 | 1988-11-11 | Capillary column |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0743361B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230280314A1 (en) * | 2022-03-02 | 2023-09-07 | Thermo Finnigan Llc | Ferrule sleeve for preventing excessive ferrule deformation causing leaks and stuck ferrules |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5114054B2 (en) * | 2003-02-04 | 2013-01-09 | ウオーターズ・テクノロジーズ・コーポレイシヨン | Capillary loop with built-in retention frit |
| JP4769792B2 (en) * | 2004-03-29 | 2011-09-07 | ウオーターズ・テクノロジーズ・コーポレイシヨン | Capillary emitter for electrospray mass spectrometry |
| DE102005055675B3 (en) * | 2005-11-23 | 2007-07-12 | Andreas Varesi | Detector device for detecting the presence of a gas |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62228159A (en) * | 1985-12-26 | 1987-10-07 | Kagakuhin Kensa Kyokai | Column for gas chromatograph |
-
1988
- 1988-11-11 JP JP63286326A patent/JPH0743361B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230280314A1 (en) * | 2022-03-02 | 2023-09-07 | Thermo Finnigan Llc | Ferrule sleeve for preventing excessive ferrule deformation causing leaks and stuck ferrules |
| US12487211B2 (en) * | 2022-03-02 | 2025-12-02 | Thermo Finnigan Llc | Ferrule sleeve for preventing excessive ferrule deformation causing leaks and stuck ferrules |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02132371A (en) | 1990-05-21 |
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