JPH11237340A - Flame photometric detector - Google Patents

Flame photometric detector

Info

Publication number
JPH11237340A
JPH11237340A JP5614598A JP5614598A JPH11237340A JP H11237340 A JPH11237340 A JP H11237340A JP 5614598 A JP5614598 A JP 5614598A JP 5614598 A JP5614598 A JP 5614598A JP H11237340 A JPH11237340 A JP H11237340A
Authority
JP
Japan
Prior art keywords
light
interference filter
convex lens
frame
concave mirror
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.)
Granted
Application number
JP5614598A
Other languages
Japanese (ja)
Other versions
JP3381611B2 (en
Inventor
Shigeaki Shibamoto
繁明 芝本
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP05614598A priority Critical patent/JP3381611B2/en
Publication of JPH11237340A publication Critical patent/JPH11237340A/en
Application granted granted Critical
Publication of JP3381611B2 publication Critical patent/JP3381611B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

PROBLEM TO BE SOLVED: To increase the quantity of light that reaches a photo detector. SOLUTION: A convex lens 23 is arranged between a hydrogen flame frame 21 and an interference filter 19, diffusion light being emitted from a combustion part 22 of a sample constituent in the frame 21 is collimated and is sent to the interference filter 19. Also, the frame 21 is put between the convex lens 23 and a concave mirror 24, and light being emitted in a direction opposite to a detection window 17 from the combustion part 22 is also reflected by the concave mirror 24 and is sent to the interference filter 19 via the convex lens 23, thus increasing the quantity of light being introduced to the interference filter 19, allowing the light to nearly vertically enter onto a filter surface, efficiently transmitting light with a desired wavelength for reaching a photomultiplier tube 20, and hence improving detection sensitivity.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、ガスクロマトグラ
フ装置等の検出器として利用される炎光光度形検出器
(以下「FPD(=Flame Photometric Detector)」と
呼ぶ)に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flame photometric detector (hereinafter referred to as "FPD (= Flame Photometric Detector)") used as a detector of a gas chromatograph or the like.

【0002】[0002]

【従来の技術】ガスクロマトグラフ装置の検出器として
は種々のものが実用化されているが、その中で、FPD
は硫黄化合物や燐化合物を選択的に検出する検出器であ
る。このため、硫化水素、メチルメルカプタン等の悪臭
成分の分析、薬品中の微量硫黄分の検出、残留農薬の分
析、生化学成分の分析等、幅広い用途に利用されてい
る。
2. Description of the Related Art Various types of gas chromatograph detectors have been put into practical use.
Is a detector for selectively detecting a sulfur compound or a phosphorus compound. Therefore, it is used for a wide range of applications such as analysis of malodorous components such as hydrogen sulfide and methyl mercaptan, detection of trace sulfur content in chemicals, analysis of residual agricultural chemicals, and analysis of biochemical components.

【0003】図2は、従来の一般的なFPDの検出セル
の構成図である。例えばガスクロマトグラフのカラム出
口に連結される試料ガス管10、水素供給管11及び空
気(又は酸素)供給管12は、上方にガス噴出口14を
有するノズル13に接続されている。ノズル13の周囲
には透明な石英筒15が配設されており、石英筒15全
体は金属製の保温ブロック16に覆われている。保温ブ
ロック16には図示しないヒータ及び温度センサが埋設
又は密着して設けられており、これにより保温ブロック
16が所定温度に維持されるようになっている。保温ブ
ロック16の所定箇所には検出窓17が開口しており、
その検出窓17の外側には冷却フィン18を介して干渉
フィルタ19と、更にその外側に検出手段として光電子
増倍管20が配設されている。
FIG. 2 is a configuration diagram of a detection cell of a conventional general FPD. For example, a sample gas pipe 10, a hydrogen supply pipe 11, and an air (or oxygen) supply pipe 12 connected to a column outlet of a gas chromatograph are connected to a nozzle 13 having a gas outlet 14 above. A transparent quartz tube 15 is provided around the nozzle 13, and the entire quartz tube 15 is covered with a heat insulating block 16 made of metal. A heater and a temperature sensor (not shown) are embedded or provided in close contact with the heat retaining block 16 so that the heat retaining block 16 is maintained at a predetermined temperature. A detection window 17 is opened at a predetermined position of the heat retaining block 16,
An interference filter 19 is provided outside the detection window 17 through a cooling fin 18, and a photomultiplier tube 20 is further provided outside the detection filter 17 as detection means.

【0004】上記FPDの動作原理は次の通りである。
試料ガス管10を通して供給される窒素等のキャリアガ
ス、水素供給管11を通して供給される水素ガス、及
び、空気供給管12を通して供給される空気をノズル1
3先端で混合し、これを燃焼して水素炎フレーム21を
形成する。例えばガスクロマトグラフのカラムから流出
した試料成分がその炎中に入ると、燃焼して成分に固有
の波長を有する光を発する。特に、過水素の還元炎で
は、硫黄化合物や燐化合物の燃焼によってそれぞれ39
4μm、526μmの波長の光を発する。水素炎フレー
ム21中の燃焼部22から発した光は透明な石英筒15
を透過し、干渉フィルタ19により上記特有の波長を有
する光のみが選択的に透過されて光電子増倍管20に到
達する。これにより、極めて選択性の高い成分検出を行
なうことができる。なお、石英筒15は、水素炎フレー
ム21から発生する水蒸気や煤等により干渉フィルタ1
9が曇らないようにするためのものである。
The operation principle of the above FPD is as follows.
The nozzle 1 supplies a carrier gas such as nitrogen supplied through a sample gas pipe 10, a hydrogen gas supplied through a hydrogen supply pipe 11, and air supplied through an air supply pipe 12.
The mixture is mixed at the three tips and burned to form a hydrogen flame frame 21. For example, when a sample component flowing out of a column of a gas chromatograph enters the flame, it burns and emits light having a wavelength unique to the component. In particular, in the reducing flame of perhydrogen, combustion of sulfur compounds and phosphorus compounds causes 39
It emits light with a wavelength of 4 μm, 526 μm. Light emitted from the combustion part 22 in the hydrogen flame frame 21 is a transparent quartz tube 15.
, And only light having the above specific wavelength is selectively transmitted by the interference filter 19 and reaches the photomultiplier tube 20. This makes it possible to detect components with extremely high selectivity. The quartz tube 15 is provided with an interference filter 1 made of water vapor or soot generated from the hydrogen flame frame 21.
9 is to prevent fogging.

【0005】[0005]

【発明が解決しようとする課題】干渉フィルタ19にお
ける目的波長光の透過率は、光が垂直に入射する場合に
最も効率がよくなる。水素炎フレーム21中の燃焼部2
2から発せられる光は拡散光(図2中に矢印で示す)で
あるから、干渉フィルタ19を水素炎フレーム21から
遠ざけるほど該干渉フィルタ19に垂直に近い角度で到
達する光(図2中の光軸cに平行な光)は減少する。上
記効率を上げるには干渉フィルタ19及び光電子増倍管
20を水素炎フレーム21に近付けることが望ましい
が、干渉フィルタ19、光電子増倍管20ともに耐熱温
度が低いため、高温の水素炎フレーム21から或る程度
離間し、しかも途中に冷却フィン18を配置する構成と
する必要があった。このため、燃焼部22からの発散光
のごく一部が光電子増倍管20に到達するのみであっ
て、検出感度が劣化する一因となっていた。
The transmittance of the interference filter 19 for the target wavelength light is most efficient when the light is incident vertically. Combustion part 2 in hydrogen flame frame 21
2 is diffused light (indicated by an arrow in FIG. 2), so that the farther the interference filter 19 is away from the hydrogen flame frame 21, the more light that reaches the interference filter 19 at an angle closer to the vertical (in FIG. 2). Light parallel to the optical axis c) decreases. To increase the efficiency, it is desirable to bring the interference filter 19 and the photomultiplier tube 20 close to the hydrogen flame frame 21. However, since both the interference filter 19 and the photomultiplier tube 20 have low heat-resistant temperatures, the interference filter 19 and the photomultiplier tube 20 must be close to each other. It is necessary to have a configuration in which the cooling fins 18 are arranged at a certain distance from each other and the cooling fins 18 are arranged on the way. For this reason, only a small part of the divergent light from the combustion section 22 reaches the photomultiplier tube 20, which is one of the causes of the deterioration of the detection sensitivity.

【0006】本発明は上記課題を解決するために成され
たものであり、その目的とするところは、光電子増倍管
に光を効率的に導入することにより感度を向上すること
ができる炎光光度形検出器を提供することにある。
SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and an object of the present invention is to provide a flame light capable of improving sensitivity by efficiently introducing light into a photomultiplier tube. It is to provide a photometric detector.

【0007】[0007]

【課題を解決するための手段】上記課題を解決するため
に成された本発明は、水素炎フレーム中に試料成分を導
入して燃焼させ、該燃焼部より発せられる光を特定の波
長を有する光を透過させる選択透過手段を介して光検出
手段へ導入する炎光光度形検出器において、前記水素炎
フレームと選択透過手段との間に集光手段を挿入するこ
とを特徴としている。
SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems. According to the present invention, a sample component is introduced into a hydrogen flame and burned, and light emitted from the burning portion has a specific wavelength. In a flame photometric detector to be introduced into the light detecting means via a selective transmitting means for transmitting light, a light condensing means is inserted between the hydrogen flame frame and the selective transmitting means.

【0008】[0008]

【発明の実施の形態】本発明に係る炎光光度検出器で
は、集光手段として例えば凸レンズを用いることができ
る。凸レンズを用いる場合、燃焼部が該凸レンズの焦点
位置になるように該凸レンズのおおよその位置が定めら
れる。これによれば、凸レンズは、水素炎フレーム中の
燃焼部から拡散して発せられる光をコリメートし、選択
透過手段の入射面に略垂直な光に変えて該選択透過手段
に導入する。これにより、該光の中の特定の波長を有す
る光のみが効率的に、つまり殆ど減衰することなく透過
し、光検出手段に到達する。
DESCRIPTION OF THE PREFERRED EMBODIMENTS In a flame photometric detector according to the present invention, for example, a convex lens can be used as a light collecting means. When a convex lens is used, the approximate position of the convex lens is determined so that the combustion section is located at the focal position of the convex lens. According to this, the convex lens collimates the light emitted from the combustion part in the hydrogen flame frame, converts the light into light substantially perpendicular to the incident surface of the selective transmission means, and introduces the light into the selective transmission means. As a result, only light having a specific wavelength in the light is transmitted efficiently, that is, almost without attenuation, and reaches the light detecting means.

【0009】また、より効率的に光を集めるには、水素
炎フレームを挟んで集光手段と反対側に凹面鏡を配設
し、該凹面鏡で反射した光を集光手段に送る構成とする
ことが好ましい。この構成によれば、水素炎フレームの
燃焼部から直接集光手段に送られる光のみならず、従来
は利用されていなかった、燃焼部から発して選択透過手
段と反対方向に進む光も凹面鏡で反射されて集光手段に
送られる。このため、選択透過手段に入射する光量が増
加する。なお、凹面鏡の凹面を球面とし、水素炎フレー
ムの燃焼部がその球面の中心となるように凹面鏡を配置
すると、凹面鏡で反射した光は燃焼部近傍を通過して集
光手段に到達するので、該反射光も集光手段により略平
行光に曲げられる。このため、光検出手段にに到達する
光はより多くなる。
In order to more efficiently collect light, a concave mirror is disposed on the opposite side of the hydrogen flame frame from the light collecting means, and the light reflected by the concave mirror is sent to the light collecting means. Is preferred. According to this configuration, not only the light directly sent from the combustion part of the hydrogen flame frame to the light collecting means, but also the light which has not been used conventionally and which is emitted from the combustion part and travels in the opposite direction to the selective transmission means is reflected by the concave mirror. The light is reflected and sent to the light collecting means. Therefore, the amount of light incident on the selective transmission unit increases. If the concave surface of the concave mirror is a spherical surface and the concave mirror is arranged so that the combustion part of the hydrogen flame frame is at the center of the spherical surface, the light reflected by the concave mirror passes through the vicinity of the combustion part and reaches the light collecting means. The reflected light is also bent into substantially parallel light by the condensing means. For this reason, more light reaches the light detecting means.

【0010】[0010]

【発明の効果】このように本発明の炎光光度形検出器に
よれば、干渉フィルタにより多くの光が、しかもフィル
タ面に略垂直に入射するので、該干渉フィルタにより定
まる特定の波長の光が効率よく透過して光検出手段に導
入される。このため、光検出手段の信号レベルが高くな
り、その結果、検出感度が向上する。
As described above, according to the flame photometric detector of the present invention, since more light is incident on the interference filter and almost perpendicularly to the filter surface, light of a specific wavelength determined by the interference filter is obtained. Is efficiently transmitted and introduced into the light detecting means. For this reason, the signal level of the light detecting means is increased, and as a result, the detection sensitivity is improved.

【0011】[0011]

【実施例】本発明に係る炎光光度形検出器の一実施例を
図1を参照して説明する。図1は本実施例によるFPD
の構成図であって、図2の従来のFPDと同一又は相当
する部分には同一の符号を付している。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of a flame photometric detector according to the present invention will be described with reference to FIG. FIG. 1 shows an FPD according to the present embodiment.
And the same or corresponding parts as those in the conventional FPD of FIG. 2 are denoted by the same reference numerals.

【0012】図1に示すように、本実施例のFPDで
は、水素炎フレーム21と干渉フィルタ19との間に、
燃焼部22が焦点となるように凸レンズ23を配設して
いる。この凸レンズ23は水素炎フレーム21に比較的
近い位置に置かれるので、耐熱性を持たせるために例え
ば石英等により形成するとよい。また、水素炎フレーム
21を挟んで凸レンズ23と反対側の保温ブロック16
内壁には、燃焼部22を中心とする球面状の凹面鏡24
が配設されている。凹面鏡24は、例えば、保温ブロッ
ク16の内壁面を球面状に窪んで形成し、該内壁面に反
射効果を有する金属等を蒸着等により付着させて鏡面を
形成するようにするとよい。
As shown in FIG. 1, in the FPD of the present embodiment, between the hydrogen flame frame 21 and the interference filter 19,
The convex lens 23 is provided so that the combustion part 22 becomes a focal point. Since the convex lens 23 is placed at a position relatively close to the hydrogen flame frame 21, it is preferable to form the convex lens 23 from, for example, quartz or the like in order to have heat resistance. Further, the heat retaining block 16 on the opposite side of the convex lens 23 with the hydrogen flame frame 21 interposed therebetween.
On the inner wall, a spherical concave mirror 24 centering on the combustion portion 22 is provided.
Are arranged. The concave mirror 24 may be formed, for example, by forming the inner wall surface of the heat retaining block 16 into a spherical shape and forming a mirror surface by depositing a metal or the like having a reflective effect on the inner wall surface by vapor deposition or the like.

【0013】本実施例のFPDでは、水素炎フレーム2
1中に試料成分が導入されると、燃焼部22近傍で該試
料成分が燃焼し、該成分に特有の波長の光が放出され
る。この光は該燃焼部22を中心として四方に拡散する
が、図1で右方向に進行して凸レンズ23に到達した光
は、該凸レンズ23によってコリメートされて光軸cに
平行な方向に変えられる。そして、干渉フィルタ19の
フィルタ面にほぼ垂直に入射し、該干渉フィルタ19の
特性に応じた特定の波長光のみが透過して光電子増倍管
20の受光面に到達する。
In the FPD of this embodiment, the hydrogen flame 2
When a sample component is introduced into the sample 1, the sample component is burned in the vicinity of the combustion section 22, and light having a wavelength specific to the component is emitted. This light is diffused in all directions around the combustion portion 22, but the light that travels rightward in FIG. 1 and reaches the convex lens 23 is collimated by the convex lens 23 and changed to a direction parallel to the optical axis c. . Then, the light enters the filter surface of the interference filter 19 almost perpendicularly, and only light having a specific wavelength according to the characteristics of the interference filter 19 is transmitted and reaches the light receiving surface of the photomultiplier tube 20.

【0014】一方、図1で左方向に進行して凹面鏡24
に到達した光は、凹面鏡24によってほぼ入射方向と反
対方向に反射される。従って、その反射光は燃焼部22
近傍を通過して凸レンズ23に到達する。このため、上
述のように燃焼部22から直接凸レンズ23に到達した
光に加えて、この反射光も凸レンズ23によりコリメー
トされ、光軸cに略平行な光となって干渉フィルタ19
に送られる。従って、凸レンズ23による集光の効果に
加えて、凹面鏡24による光量の増加の効果も得られ
る。
On the other hand, as shown in FIG.
Is reflected by the concave mirror 24 in a direction substantially opposite to the incident direction. Therefore, the reflected light is transmitted to the combustion section 22.
The light passes through the vicinity and reaches the convex lens 23. For this reason, in addition to the light that directly reaches the convex lens 23 from the combustion section 22 as described above, the reflected light is also collimated by the convex lens 23 and becomes light substantially parallel to the optical axis c, so that the interference filter 19
Sent to Therefore, in addition to the effect of condensing light by the convex lens 23, the effect of increasing the amount of light by the concave mirror 24 can be obtained.

【0015】このように、上記実施例のFPDでは、凸
レンズ23と凹面鏡24との両者により、従来のFPD
と比べて格段に多量の放出光が平行光として干渉フィル
タ19に到達し、該干渉フィルタ19により所望の波長
光のみが取り出されて光電子増倍管20に到達する。従
って、検出感度が向上し、より微量な試料成分が測定で
きるようになる。
As described above, in the FPD of the above embodiment, both the convex lens 23 and the concave mirror 24 make the conventional FPD
A much larger amount of emitted light reaches the interference filter 19 as parallel light, and only the light of a desired wavelength is extracted by the interference filter 19 and reaches the photomultiplier tube 20. Therefore, the detection sensitivity is improved, and a smaller amount of sample components can be measured.

【0016】なお、上記実施例は一例であって、本発明
の趣旨の範囲で適宜変更や修正を行なえることは明らか
である。
The above embodiment is merely an example, and it is apparent that changes and modifications can be made within the spirit of the present invention.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 本発明の炎光光度形検出器の一実施例の構成
図。
FIG. 1 is a configuration diagram of an embodiment of a flame photometric detector according to the present invention.

【図2】 従来の炎光光度形検出器の構成図。FIG. 2 is a configuration diagram of a conventional flame photometric detector.

【符号の説明】[Explanation of symbols]

10…試料ガス管 11…水素供給管 12…空気供給管 13…ノズル 14…ガス噴出口 15…石英筒 16…保温ブロック 17…検出窓 18…冷却フィン 19…干渉フィル
タ(選択透過手段) 20…光電子増倍管(光検出手段) 21…水素炎フレ
ーム 22…燃焼部 23…凸レンズ
(集光手段) 24…凹面鏡
DESCRIPTION OF SYMBOLS 10 ... Sample gas pipe 11 ... Hydrogen supply pipe 12 ... Air supply pipe 13 ... Nozzle 14 ... Gas ejection port 15 ... Quartz cylinder 16 ... Heat insulation block 17 ... Detection window 18 ... Cooling fin 19 ... Interference filter (selective transmission means) 20 ... Photomultiplier tube (light detecting means) 21 ... hydrogen flame frame 22 ... burning part 23 ... convex lens (light collecting means) 24 ... concave mirror

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 水素炎フレーム中に試料成分を導入して
燃焼させ、該燃焼部より発せられる光を特定の波長光を
透過させる選択透過手段を介して光検出手段へ導入する
炎光光度形検出器において、前記水素炎フレームと選択
透過手段との間に集光手段を挿入することを特徴とする
炎光光度形検出器。
1. A flame photometric type in which a sample component is introduced into a hydrogen flame and burned, and light emitted from the combustion section is introduced into light detection means via selective transmission means for transmitting light of a specific wavelength. A flame photometric detector, wherein a light collector is inserted between the hydrogen flame frame and the selective transmission means in the detector.
JP05614598A 1998-02-20 1998-02-20 Flame photometric detector Expired - Fee Related JP3381611B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP05614598A JP3381611B2 (en) 1998-02-20 1998-02-20 Flame photometric detector

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP05614598A JP3381611B2 (en) 1998-02-20 1998-02-20 Flame photometric detector

Publications (2)

Publication Number Publication Date
JPH11237340A true JPH11237340A (en) 1999-08-31
JP3381611B2 JP3381611B2 (en) 2003-03-04

Family

ID=13018926

Family Applications (1)

Application Number Title Priority Date Filing Date
JP05614598A Expired - Fee Related JP3381611B2 (en) 1998-02-20 1998-02-20 Flame photometric detector

Country Status (1)

Country Link
JP (1) JP3381611B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009288209A (en) * 2008-06-02 2009-12-10 Shimadzu Corp Flame photometric detector
CN103226101A (en) * 2012-01-31 2013-07-31 上海天美科学仪器有限公司 High sensitivity flame photometric detector

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009288209A (en) * 2008-06-02 2009-12-10 Shimadzu Corp Flame photometric detector
CN103226101A (en) * 2012-01-31 2013-07-31 上海天美科学仪器有限公司 High sensitivity flame photometric detector

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