JP3158049U - Gas chromatograph - Google Patents

Gas chromatograph Download PDF

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JP3158049U
JP3158049U JP2009009289U JP2009009289U JP3158049U JP 3158049 U JP3158049 U JP 3158049U JP 2009009289 U JP2009009289 U JP 2009009289U JP 2009009289 U JP2009009289 U JP 2009009289U JP 3158049 U JP3158049 U JP 3158049U
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column
sample
detector block
vaporization chamber
detector
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古川 雅直
雅直 古川
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Shimadzu Corp
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Abstract

【課題】検出器ブロックと試料気化室に対するカラム挿入長さを仕様通り確保するガスクロマトグラフを提供する。【解決手段】検出器ブロック4および試料気化室にカラム挿入長さを規制するためにカラム1の先端を当接する係止部11を内設するとともにカラム挿入口に向かって拡大する円錐状凹部12を形成する。またカラム1と滑合するフェルール2に、外周部は先端に向かって縮小する円錐状凸部13および内周部は先端に向かって拡大する円錐状凹部17を設けることによりカラム1の先端が破損することがなく取付け作業を容易に且つ正確に行うことができる。【選択図】図1A gas chromatograph that secures a column insertion length for a detector block and a sample vaporization chamber as specified. In order to regulate the column insertion length in the detector block 4 and the sample vaporization chamber, a locking portion 11 that contacts the tip of the column 1 is provided, and a conical recess 12 that expands toward the column insertion port. Form. In addition, the ferrule 2 that slides on the column 1 is provided with a conical convex portion 13 whose outer peripheral portion is reduced toward the front end and a conical concave portion 17 that is enlarged toward the front end, whereby the front end of the column 1 is damaged. Therefore, the mounting operation can be performed easily and accurately. [Selection] Figure 1

Description

本考案は、試料分析に用いられるガスクロマトグラフに係り、特にガスクロマトグラフの検出器とカラムあるいは試料気化室とカラムを連結するための密封用フェルールにカラムを貫設したガスクロマトグラフに関する。   The present invention relates to a gas chromatograph used for sample analysis, and more particularly, to a gas chromatograph in which a column is provided in a sealing ferrule for connecting the detector and column of the gas chromatograph or the sample vaporizing chamber and the column.

分析計の一種であるガスクロマトグラフは、固定相を充填したカラムに移動相であるキャリアガスを連続的に流し、瞬間的に混合試料をカラムの入口から導入することによって、混合試料が移動相とともにカラム内を移動する間に固定相に対する各成分の吸着性(親和性)や分配係数の差異に基づく移動速度の差を利用して各成分を相互分離し、定量定性分析する装置である(特許文献1参照)。   A gas chromatograph, a type of analyzer, continuously flows a carrier gas, which is a mobile phase, into a column packed with a stationary phase, and instantaneously introduces the mixed sample from the inlet of the column. A device that separates components from each other using a difference in adsorption speed (affinity) of each component with respect to the stationary phase and a difference in partition coefficient while moving through the column, and performs quantitative qualitative analysis (patent) Reference 1).

前記カラムと、該カラムの両端にそれぞれ密封連結された試料気化室および検出器ブロックによって、ガスクロマトグラフの一部が構成される。前記混合試料が前記キャリアガスとともに、前記試料気化室、またはカラムを通り、検出器ガス導入路から導入された検出器ガスとともに前記検出器ブロックを経て検出器に導入される。   A part of the gas chromatograph is constituted by the column, the sample vaporizing chamber and the detector block that are hermetically connected to both ends of the column. The mixed sample passes through the sample vaporization chamber or column together with the carrier gas, and is introduced into the detector through the detector block together with the detector gas introduced from the detector gas introduction path.

図4は従来のガスクロマトグラフにおける検出器ブロックおよび試料気化室とカラムの密封連結状態を説明するために、検出器ブロックを例に検出器ブロックとカラムの連結状態を示している。検出器ブロック7のねじ部7Nに螺合させたナット3を締め込むことにより、カラム1を貫設したフェルール6の円錐状凸部19を検出器ブロック7の円錐状凹部18に押圧させ、検出器ブロック7とフェルール6、およびフェルール6とカラム1を連結させ、結果的に検出器ブロック7とカラム1が密封連結される。   FIG. 4 shows a detector block and a column connected to each other in the detector block as an example in order to explain a detector block and a sample vaporization chamber in a conventional gas chromatograph. By tightening the nut 3 screwed into the threaded portion 7N of the detector block 7, the conical convex portion 19 of the ferrule 6 penetrating the column 1 is pressed against the conical concave portion 18 of the detector block 7, thereby detecting The detector block 7 and the ferrule 6 and the ferrule 6 and the column 1 are connected, and as a result, the detector block 7 and the column 1 are hermetically connected.

したがって前記混合試料は前記キャリアガスとともに、連続的な流れとして試料気化室(図示せず)を経て、前記カラム1を通り、検出器ガス導入路23から導入された検出器ガスとともに前記検出器ブロック7を経て検出器(図示せず)に導入される。   Therefore, the mixed sample passes through the sample vaporization chamber (not shown) as a continuous flow together with the carrier gas, passes through the column 1 and the detector gas introduced from the detector gas introduction path 23. 7 is introduced into a detector (not shown).

カラム1をガスクロマトグラフに取付ける場合、前記検出器ブロック7および前記試料気化室(図示せず)に対するカラム挿入長さを設定することは重要で試料分析の感度や精度に重要な影響を及ぼす。   When the column 1 is attached to a gas chromatograph, it is important to set the column insertion length for the detector block 7 and the sample vaporization chamber (not shown), which has an important influence on the sensitivity and accuracy of sample analysis.

前記試料気化室(図示せず)においては前記カラム1の先端部より気化した試料が導入されるが、その位置により導入量あるいは導入タイミングが異なるために最適なカラム挿入長さが設定される。また前記検出器ブロック7においても前記カラム1の先端部の位置により検出感度や最小検出量等が左右されるために同様に最適なカラム挿入長さが設定される。   In the sample vaporizing chamber (not shown), the vaporized sample is introduced from the tip of the column 1, and the optimum column insertion length is set because the introduction amount or introduction timing differs depending on the position. Also in the detector block 7, since the detection sensitivity, the minimum detection amount, etc. are influenced by the position of the tip of the column 1, the optimum column insertion length is set similarly.

したがって通常、前記カラム挿入長さは前記検出器ブロック7または前記試料気化室(図示せず)に対して予め定められ、ガスクロマトグラフの取扱説明書にその値が記載されている。分析者はカラム取付け時に物差し等の定規を当てながらカラム挿入長さを一々確認して取付けていた。   Therefore, normally, the column insertion length is predetermined for the detector block 7 or the sample vaporizing chamber (not shown), and the value is described in an instruction manual of the gas chromatograph. The analyst checked the column insertion length one by one while applying a ruler such as a ruler when installing the column.

特開平7−20112号公報Japanese Patent Laid-Open No. 7-20112

分析者はカラム取付け時に物差し等で検出器ブロック7および試料気化室(図示せず)に対するカラム挿入長さを確認しながら、カラム1に通したフェルール6の円錐状凸部19をナット3で締め込み、検出器ブロック7の円錐状凹部18に押し進めることにより検出器ブロック7とフェルール6、およびフェルール6とカラム1を固着させ、結果的に検出器ブロック7とカラム1が密封連結される。   The analyst tightens the conical convex portion 19 of the ferrule 6 passed through the column 1 with the nut 3 while checking the column insertion length with respect to the detector block 7 and the sample vaporizing chamber (not shown) with a ruler or the like when installing the column. Then, the detector block 7 and the ferrule 6 and the ferrule 6 and the column 1 are fixed to each other by being pushed into the conical recess 18 of the detector block 7, and as a result, the detector block 7 and the column 1 are hermetically connected.

しかしながら、カラム1とフェルール6は微小な隙間を持った滑合関係にあるため、互いの位置を指定寸法に維持しながらナット3を締め込むことは非常に困難であり、カラム1とフェルール6を固着させた後一旦外して前記カラム挿入長さを計測確認し、前記カラム挿入長さが確保されていない場合には修正が必要であった。   However, since the column 1 and the ferrule 6 are in a sliding relationship with a minute gap, it is very difficult to tighten the nut 3 while maintaining the position of the column 1 and the ferrule 6 at the specified dimensions. After fixing, the column insertion length was once removed and the column insertion length was measured and confirmed. If the column insertion length was not secured, correction was necessary.

本考案は上記課題を解決するために、注入された試料を気化する試料気化室と、前記試料気化室に挿入されるとともに気化された前記試料が導入されるカラムと、前記カラムが挿入され前記カラムを通過した試料が溶出するとともに、前記試料の定量定性分析を行う検出器を取付ける検出器ブロックと、前記試料気化室および前記検出器ブロックと挿入された前記カラムを密封連結するためのフェルールを備えたガスクロマトグラフにおいて、前記試料気化室と前記検出器ブロックに対して挿入される前記カラムを係止する係止部を前記試料気化室と前記検出器ブロックに内設する。   In order to solve the above problems, the present invention provides a sample vaporization chamber for vaporizing an injected sample, a column inserted into the sample vaporization chamber and into which the vaporized sample is introduced, and the column is inserted into the column. The sample that has passed through the column elutes, and a detector block for mounting a detector for quantitative qualitative analysis of the sample, and a ferrule for hermetically connecting the sample vaporization chamber and the detector block to the inserted column In the gas chromatograph provided, the sample vaporizing chamber and the detector block are provided with locking portions for locking the column inserted into the sample vaporizing chamber and the detector block.

本考案によりカラムを検出器ブロックおよび試料気化室に取付ける際、物差し等の定規を当てながらカラム挿入長さを一々確認して取付ける必要がなく、前記係止部にカラム先端を軽く当ててナットを締め込むだけでよく、作業を容易に且つ正確に行うことができる。   When attaching the column to the detector block and the sample vaporization chamber according to the present invention, it is not necessary to check the column insertion length while applying a ruler such as a ruler. It is only necessary to tighten, and the operation can be performed easily and accurately.

本考案にかかわる実施例を示す図で、検出器ブロックとカラムを密封連結する部分を断面で示す概念図である。It is a figure which shows the Example concerning this invention, and is the conceptual diagram which shows the part which seal-connects a detector block and a column in a cross section. 本考案のガスクロマトグラフの構成を示す概念図である。It is a conceptual diagram which shows the structure of the gas chromatograph of this invention. 本考案にかかわる変形実施例を示す図で、本変形実施例にかかわるフェルールの断面図である。It is a figure which shows the modified example concerning this invention, and is sectional drawing of the ferrule concerning this modified example. 従来の検出器ブロックとカラムを密封連結する部分を断面で示す概念図である。It is a conceptual diagram which shows the part which seals and connects the conventional detector block and a column in a cross section.

試料気化室および検出器ブロックに対して、試料気化室および検出器ブロックに対するカラム挿入長さを予め定められた最適な値に規制する係止部を内設するとともに、カラム挿入口に向かって拡大する円錐状凹部を形成する。さらにフェルールに対して、外周部は試料気化室および検出器ブロックの円錐状凹部に嵌合する端部に向かって縮小する円錐状凸部および内周部は前記端部に向かって拡大する円錐状凹部を形成する。   In addition to the sample vaporization chamber and detector block, there is an internal locking section that regulates the column insertion length for the sample vaporization chamber and detector block to a predetermined optimum value, and it expands toward the column insertion port. A conical recess is formed. Further, with respect to the ferrule, the outer peripheral portion is reduced toward the end fitting into the conical concave portion of the sample vaporizing chamber and the detector block, and the conical convex portion and the inner peripheral portion are conical shapes expanding toward the end portion. A recess is formed.

図2は本考案にかかわるガスクロマトグラフの構成を示す概念図である。図2に示すとおりガスクロマトグラフの主要な構成要素は、分析すべき試料が注入される試料気化室14と、この試料気化室14からの試料をキャリアガスとともに流動させ、成分に応じて分離させる主体のカラム1と、このカラム1を試料気化室14と、検出器16の検出器ブロック4間にて接続する接続具(フェルール)等である。   FIG. 2 is a conceptual diagram showing the configuration of a gas chromatograph according to the present invention. As shown in FIG. 2, the main components of the gas chromatograph are a sample vaporization chamber 14 into which a sample to be analyzed is injected, and a main body that causes the sample from the sample vaporization chamber 14 to flow together with a carrier gas and separates according to the components. And a connecting tool (ferrule) for connecting the column 1 between the sample vaporizing chamber 14 and the detector block 4 of the detector 16.

図2にしたがって分析の流れを説明すると、試料気化室14において、キャリアガス導入口15から導入され、係止部22に設けられたガス通路21を通過したキャリアガスの流れの中に少量の試料が注入される。試料が気体であればそのままの状態で、液体試料であれば適当な温度に加熱されて試料気化室14でガス状態に気化された試料は、キャリアガスに運ばれ、係止部22に設けられた小孔20を経てカラム1を通過する間に各成分に分離される。   The flow of analysis will be described with reference to FIG. 2. In the sample vaporization chamber 14, a small amount of sample is introduced into the carrier gas flow introduced from the carrier gas inlet 15 and passed through the gas passage 21 provided in the locking portion 22. Is injected. If the sample is a gas, the sample is left as it is; if it is a liquid sample, the sample heated to an appropriate temperature and vaporized in the gas state in the sample vaporization chamber 14 is carried to the carrier gas and provided in the locking portion 22. Each component is separated while passing through the column 1 through the small holes 20.

各成分に分離された試料は、係止部11に設けられた小孔9を通って検出器ブロック4に溶出し、検出器ガス導入路8より導入され係止部11に設けられたガス通路10を通過した検出器ガスと合流した後検出器16へと流入し試料の成分と量が検出され、最後は排出路(図示せず)から大気に放出される。   The sample separated into each component elutes into the detector block 4 through the small hole 9 provided in the locking part 11 and is introduced from the detector gas introduction path 8 and is provided in the locking part 11. After joining the detector gas that has passed 10, it flows into the detector 16, where the component and amount of the sample are detected, and finally, it is released from the discharge path (not shown) to the atmosphere.

ここでカラム1は、分析したい試料が気化している必要があるので、一般的に恒温槽(図示せず)内に収められている。また、試料気化室14は試料を気体状態に保つとともに、周囲の温度変化の影響を受けないように、カラム1とは別の恒温槽(図示せず)に収められている。   Here, since the sample to be analyzed needs to be vaporized, the column 1 is generally stored in a thermostat (not shown). The sample vaporizing chamber 14 is housed in a thermostat (not shown) separate from the column 1 so that the sample is kept in a gaseous state and is not affected by ambient temperature changes.

図2に示す実施例1のガスクロマトグラフの構成に係り、図1に検出器ブロックとカラムを密封連結する部分を示す。検出器ブロック4に対するカラム挿入長さを規制するためにカラム1の先端を係止する係止部11を内設するとともに、カラム挿入口に向かって拡大する円錐状凹部12を検出器ブロック4に形成する。またカラム1と滑合する中空形状のフェルール2に、外周部は先端に向かって縮小する円錐状凸部13および内周部は先端に向かって拡大する円錐状凹部17を設ける。なお図2において、図1と同一の符号で示される部品は図1と同一の部品である。   In relation to the configuration of the gas chromatograph of Example 1 shown in FIG. 2, FIG. 1 shows a portion where the detector block and the column are hermetically connected. In order to regulate the column insertion length with respect to the detector block 4, a locking portion 11 for locking the tip of the column 1 is provided, and a conical concave portion 12 that expands toward the column insertion port is provided in the detector block 4. Form. The hollow ferrule 2 that slides on the column 1 is provided with a conical convex portion 13 whose outer peripheral portion is reduced toward the tip and a conical concave portion 17 whose inner peripheral portion is enlarged toward the tip. In FIG. 2, parts denoted by the same reference numerals as in FIG. 1 are the same parts as in FIG.

フェルール2に貫設したカラム1の先端を軽く係止部11に押し付けつつ、ナット3を締め込みながらフェルール2の円錐状凸部13を検出器ブロック4の円錐状凹部12に押し進めていくとフェルール2の円錐状凸部13が検出器ブロック4の円錐状凹部12に押し付け密着させられ、検出器ブロック4とフェルール2が密封される。さらにナット3を押し進めていくと、前記円錐状凹凸部12、13の押し付けにより発生する反力によってフェルール2を径方向に縮小させカラム1とフェルール2を固着部Bで固着密封させる。   When the tip of the column 1 penetrating the ferrule 2 is lightly pressed against the locking portion 11 and the conical convex portion 13 of the ferrule 2 is pushed into the conical concave portion 12 of the detector block 4 while tightening the nut 3, the ferrule The two conical convex portions 13 are pressed and brought into close contact with the conical concave portion 12 of the detector block 4 so that the detector block 4 and the ferrule 2 are sealed. When the nut 3 is further pushed forward, the ferrule 2 is contracted in the radial direction by the reaction force generated by the pressing of the conical concavo-convex portions 12 and 13, and the column 1 and the ferrule 2 are fixedly sealed by the fixing portion B.

さらにナット3を押し進めていくとフェルール2の円錐状凸部13と検出器ブロック4の円錐状凹部の固着密封状態を保持したまま、フェルール2が支点Aを支点として微小変形して固着部Bが支点Aから遠ざかる方向に微小移動する。この固着部Bの移動と一体にカラム1の先端も係止部11より退避するためカラム1の先端と係止部11間に微小な隙間ができ、カラム先端が破損することがなくカラム挿入長さが確保される。したがって本考案によりカラムを検出器ブロック4に取付ける際、その取付け作業を容易に且つ正確に行うことができる。   When the nut 3 is further pushed forward, the ferrule 2 is slightly deformed with the fulcrum A as a fulcrum while the conical convex portion 13 of the ferrule 2 and the conical concave portion of the detector block 4 are maintained, and the fixing portion B is formed. It moves slightly in the direction away from the fulcrum A. Since the front end of the column 1 is also retracted from the locking portion 11 together with the movement of the fixing portion B, a minute gap is formed between the front end of the column 1 and the locking portion 11, and the column front end is not damaged. Is secured. Therefore, when the column is attached to the detector block 4 according to the present invention, the attaching operation can be performed easily and accurately.

係止部11には、ガス通路10とカラム1の軸芯と一致する位置にカラム外径よりわずかに小さい小孔9が設けられている。小孔9からはカラム1を通ってきた試料ガスが通過し、ガス通路10からは検出器ガス導入路8から導入された検出器ガスが通過する。   The engaging portion 11 is provided with a small hole 9 slightly smaller than the outer diameter of the column at a position coinciding with the gas passage 10 and the axis of the column 1. The sample gas that has passed through the column 1 passes through the small hole 9, and the detector gas introduced from the detector gas introduction passage 8 passes through the gas passage 10.

試料気化室14は検出器ブロック4と同様な密封連結構造である。すなわち、試料気化室14もカラム1との密封連結構造とされており、その取付け作業を容易であり、且つ正確に行うことができる。   The sample vaporizing chamber 14 has a sealed connection structure similar to that of the detector block 4. That is, the sample vaporizing chamber 14 is also structured to be hermetically connected to the column 1 and can be easily and accurately attached.

図3に実施例2を示す。実施例2は実施例1のフェルールの形状を変形したものであり、それ以外は実施例1と全く同じであって、機能についても実施例1と全く同等である。したがって図3にはフェルール5のみを示す。ただし、カラム1の密封連結のためのナット3の締め付け力は、変形しやすい中空形状のフェルール2に対して中実形状であるフェルール5の方が大きくなるが、フェルール5の方が製作が安価で且つ容易である。   Example 2 is shown in FIG. The second embodiment is a modification of the ferrule shape of the first embodiment. Except for this, the second embodiment is exactly the same as the first embodiment, and the functions are also exactly the same as the first embodiment. Therefore, only ferrule 5 is shown in FIG. However, the tightening force of the nut 3 for hermetically connecting the column 1 is larger in the ferrule 5 which is a solid shape than the hollow ferrule 2 which is easily deformed, but the ferrule 5 is less expensive to manufacture. And easy.

1 カラム
2 フェルール
3 ナット
4 検出器ブロック
5 フェルール
6 フェルール
7 検出器ブロック
8 検出器ガス導入路
9 小孔
10 ガス通路
11 係止部
12 円錐状凹部
13 円錐状凸部
14 試料気化室
15 キャリアガス導入口
16 検出器
17 円錐状凹部
18 円錐状凹部
19 円錐状凸部
20 小孔
21 ガス通路
22 係止部
23 検出器ガス導入路
A 支点
B 固着部
7N ねじ部
DESCRIPTION OF SYMBOLS 1 Column 2 Ferrule 3 Nut 4 Detector block 5 Ferrule 6 Ferrule 7 Detector block 8 Detector gas introduction path 9 Small hole 10 Gas passage 11 Locking part 12 Conical concave part 13 Conical convex part 14 Sample vaporization chamber 15 Carrier gas Inlet 16 Detector 17 Conical concave portion 18 Conical concave portion 19 Conical convex portion 20 Small hole 21 Gas passage 22 Locking portion 23 Detector gas introduction passage A Support point B Adhering portion 7N Screw portion

Claims (4)

注入された試料を気化する試料気化室と、前記試料気化室に挿入されるとともに気化された前記試料が導入されるカラムと、前記カラムが挿入され前記カラムを通過した試料が溶出するとともに、前記試料の定量定性分析を行う検出器を取付ける検出器ブロックと、前記試料気化室および前記検出器ブロックと挿入された前記カラムを密封連結するためのフェルールを備えたガスクロマトグラフにおいて、前記試料気化室と前記検出器ブロックに対して挿入される前記カラムの先端位置を規制する係止部が前記試料気化室と前記検出器ブロックに内設されたことを特徴とするガスクロマトグラフ。   A sample vaporization chamber for vaporizing the injected sample, a column inserted into the sample vaporization chamber and into which the vaporized sample is introduced, a sample inserted through the column and passed through the column is eluted, and the In a gas chromatograph comprising a detector block for mounting a detector for quantitative qualitative analysis of a sample, and a ferrule for hermetically connecting the sample vaporization chamber and the detector block to the inserted column, the sample vaporization chamber and A gas chromatograph, wherein a locking portion for restricting a tip position of the column inserted into the detector block is provided in the sample vaporizing chamber and the detector block. カラム挿入口に向かって拡大する円錐状凹部を形成する前記試料気化室および前記検出器ブロックを備え、前記フェルールは、外周部は前記試料気化室および前記検出器ブロックの円錐状凹部に嵌合する端部に向かって縮小する円錐状凸部および内周部は前記端部に向かって拡大する円錐状凹部が形成されていることを特徴とする請求項1記載のガスクロマトグラフ。   The sample vaporization chamber and the detector block forming a conical recess that expands toward the column insertion port are provided, and the ferrule has an outer peripheral portion that fits into the sample vaporization chamber and the conical recess of the detector block. The gas chromatograph according to claim 1, wherein a conical convex portion and an inner peripheral portion that are reduced toward the end portion are formed with a conical concave portion that is enlarged toward the end portion. 前記係止部が、前記試料気化室および前記検出器ブロックに対する前記カラムの挿入長さを予め定められた値に規制する位置に内設されたことを特徴とする請求項1記載のガスクロマトグラフ。   The gas chromatograph according to claim 1, wherein the locking portion is provided at a position that regulates an insertion length of the column with respect to the sample vaporizing chamber and the detector block to a predetermined value. 前記係止部のカラム軸心上にカラム外径より小さな孔を有することを特徴とする請求項1または2または3記載のガスクロマトグラフ。   The gas chromatograph according to claim 1, 2 or 3, wherein a hole smaller than the outer diameter of the column is formed on a column axis of the locking portion.
JP2009009289U 2009-12-28 2009-12-28 Gas chromatograph Expired - Fee Related JP3158049U (en)

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